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Materials, Volume 15, Issue 20 (October-2 2022) – 362 articles

Cover Story (view full-size image): Highly bioorthogonal and fast-swelling hydrogels, derived from norbornene functionalized hyaluronic acid and a water-soluble cross-linker possessing tetrazine functionalities on both ends of polyethylene glycol, were developed using IEDDA click reaction. The hydrogels formed rapidly, offering a possibility to use them as injectable drug carriers. The hydrogels were able to encapsulate a high amount of curcumin and released it in a temporal pattern. The resulting hydrogels showed no cytotoxicity in HEK-293 cells, demonstrating their promising application as an injectable drug delivery system. View this paper
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13 pages, 2570 KiB  
Article
The Influence of Plasma Treatment on the Corrosion and Biocompatibility of Magnesium
by Aleksandra Kocijan, Janez Kovač, Ita Junkar, Matic Resnik, Veno Kononenko and Marjetka Conradi
Materials 2022, 15(20), 7405; https://doi.org/10.3390/ma15207405 - 21 Oct 2022
Cited by 5 | Viewed by 1765
Abstract
In our study, plasma surface modification was employed to tailor the surface properties of magnesium in terms of surface chemistry, topography, and wettability. For two sets of samples, the plasma treatment involved two steps using two different gases (hydrogen and oxygen), while one [...] Read more.
In our study, plasma surface modification was employed to tailor the surface properties of magnesium in terms of surface chemistry, topography, and wettability. For two sets of samples, the plasma treatment involved two steps using two different gases (hydrogen and oxygen), while one set of samples was treated with one step only using oxygen. X-ray photoelectron spectroscopy (XPS) was applied to determine the surface composition, oxidation state of the elements, and the thickness of the surface oxide layer on the Mg samples after different plasma treatments. The surface morphology was characterised using atomic force microscopy (AFM) and scanning electron microscopy (SEM). The wettability was analysed by measuring the static water-contact angles and the corrosion was evaluated using potentiodynamic measurements. The interaction of the live cells with the differently modified Mg surfaces was evaluated in terms of biocompatibility using MG-63 cells (human bone osteosarcoma cells). We have shown that a plasma surface treatment significantly decreased the carbon content and the formation of a 15–20-nm-thick MgO layer was observed. This improves the corrosion resistance, while the biocompatibility was retained, compared to the untreated Mg. A plasma surface treatment is therefore an important step in the development of novel surfaces with improved corrosion resistance for magnesium in biomedical applications. Full article
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Figure 1

Figure 1
<p>Plasma treatment system: (1) quartz tube, (2) magnesium disc—sample, (3) copper coil, (4) gas inlet, (5) pressure gauge, (6) radio-frequency generator at 13.56 MHz with matching network, (7) vacuum pump.</p>
Full article ">Figure 2
<p>XPS spectra C 1s (<b>a</b>), O 1s (<b>b</b>) and Mg 1s (<b>c</b>) from untreated and treated magnesium samples.</p>
Full article ">Figure 3
<p>XPS depth profiles of (<b>a</b>) untreated Mg, (<b>b</b>) E-mode H<sub>2</sub>/O<sub>2</sub>, 200-W, and (<b>c</b>) H-mode H<sub>2</sub>/O<sub>2</sub>, 600-W samples.</p>
Full article ">Figure 4
<p>AFM images of 2 × 2 µm<sup>2</sup> areas and SEM images of (<b>a</b>,<b>b</b>) untreated Mg, (<b>c</b>,<b>d</b>) E-mode O<sub>2</sub>, 200-W Mg, (<b>e</b>,<b>f</b>) E-mode H<sub>2</sub>/O<sub>2</sub> 200-W and (<b>g</b>,<b>h</b>) H-mode H<sub>2</sub>/O<sub>2</sub>, 600-W Mg samples.</p>
Full article ">Figure 5
<p>Potentiodynamic curves for untreated and plasma-modified magnesium measured in simulated physiological Hank’s solution at pH = 7.8 and room temperature.</p>
Full article ">Figure 6
<p>Representative fluorescence images of MG-63 cells grown on (<b>A</b>) Mg, (<b>B</b>) E-mode O<sub>2</sub>, 200 W, (<b>C</b>) E-mode H<sub>2</sub>/O<sub>2</sub>, 200 W and (<b>D</b>) H-mode H<sub>2</sub>/O<sub>2</sub>, 600 W for 24 h. Blue fluorescence represents the cell nuclei of viable cells and red fluorescence represents the cell nuclei of cells with damaged plasmalemma. Scale bar = 100 µm.</p>
Full article ">Figure 7
<p>Adhesion of MG-63 cells to untreated and plasma-modified magnesium after 24 h incubation.</p>
Full article ">Figure 8
<p>SEM images of MG-63 cell distribution and shapes on (<b>A</b>,<b>B</b>) Mg, (<b>C</b>,<b>D</b>) E-mode O<sub>2</sub>, 200 W, (<b>E</b>,<b>F</b>) E-mode H<sub>2</sub>/O<sub>2</sub>, 200 W and (<b>G</b>,<b>H</b>) H-mode H<sub>2</sub>/O<sub>2</sub>, 600 W. Scale bar on the 100× images is 100 µm and on the 500× images it is 20 µm.</p>
Full article ">Figure 9
<p>(<b>A</b>) Relative distribution of different morphological cell types of MG-63 cells attached to the samples. Data are presented as the mean percentage of all cells (+SD). Asterisk indicates significant difference in comparison to unmodified Mg sample (* <span class="html-italic">p</span> &lt; 0.05; Student’s <span class="html-italic">t</span>-test). (<b>B</b>) SEM image showing different morphological cell types of MG-63 cells. Scale bar = 10 µm.</p>
Full article ">
23 pages, 13635 KiB  
Article
Research on the Behavior of Stiffening Walls in Single-Storey Buildings Made of Autoclaved Aerated Concrete (AAC) Masonry Units
by Krzysztof Grzyb and Radosław Jasiński
Materials 2022, 15(20), 7404; https://doi.org/10.3390/ma15207404 - 21 Oct 2022
Cited by 4 | Viewed by 2168
Abstract
Experimental identification of stiffening walls is often limited to studying single-wall models. However, these samples do not reflect many additional effects—torsion of the building and redistribution of internal forces. This paper presents the results of two full-scale buildings made of autoclaved aerated concrete [...] Read more.
Experimental identification of stiffening walls is often limited to studying single-wall models. However, these samples do not reflect many additional effects—torsion of the building and redistribution of internal forces. This paper presents the results of two full-scale buildings made of autoclaved aerated concrete (AAC) masonry elements. The primary purpose of the work was to determine the changes in the stiffness of the shear walls and to attempt the empirical distribution of loads on the stiffening walls. The intermediate goals were: a description of the crack morphology and the mechanism of failure, the designation of the stiffening walls’ behavior. It was shown that the first crack formed in the tensile corner of the door opening, and the subsequent cracks formed in the wall without a hole. Based on the changes in the value of the shear deformation angles, the phases of work of the stiffening walls were determined. The presented research results are only a part of an extensive study of stiffening walls in masonry buildings conducted at the Silesian University of Technology. Full article
(This article belongs to the Special Issue Masonry Structures and Reinforced Concrete Structures)
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Figure 1
<p>Behavior of stiffening masonry wall in simple and complex failure mode; <span class="html-italic">1</span>—straight crack (high compressive stress); <span class="html-italic">2</span>—stepped crack (low compressive stress); <span class="html-italic">3</span>—tensile corner; <span class="html-italic">s<sub>c</sub></span>—compressive stress; <span class="html-italic">s<sub>t</sub></span>—tensile stress; <span class="html-italic">H</span><sub>x</sub>—horizontal shear force; <span class="html-italic">F</span><sub>t</sub>—tensile force.</p>
Full article ">Figure 2
<p>Construction stages; (<b>a</b>) formwork of the lower perimeter beam; (<b>b</b>) erection of masonry walls made of autoclaved aerated concrete; (<b>c</b>) slab top reinforcement; (<b>d</b>) concreting the slab.</p>
Full article ">Figure 3
<p>Slab construction; (<b>a</b>) cross-section of panels; (<b>b</b>) longitudinal section of the panels; <span class="html-italic">1</span>—masonry wall made of autoclaved aerated concrete; <span class="html-italic">2</span>—precast L-shaped element made of lightweight concrete; <span class="html-italic">3</span>—reinforcement of the circumferential top beam; <span class="html-italic">4</span>—precast, pretensioned panel slab; <span class="html-italic">5</span>—lightweight filling–polystyrene; <span class="html-italic">6</span>—concrete overlay; <span class="html-italic">7</span>—the monolithic connection between panels.</p>
Full article ">Figure 4
<p>Research model in the test stand; <span class="html-italic">1</span>—slab; <span class="html-italic">2</span>—masonry wall made of autoclaved aerated concrete units; <span class="html-italic">3</span>—ring bottom beam; <span class="html-italic">4</span>—ring top beam; <span class="html-italic">5</span>—fixing the building model in the slab of great forces; <span class="html-italic">6</span>—hydraulic cylinder; <span class="html-italic">7</span>—force gauge; <span class="html-italic">8</span>—steel column.</p>
Full article ">Figure 5
<p>Loads of single-storey buildings; (<b>a</b>) horizontal load; (<b>b</b>) vertical load.</p>
Full article ">Figure 6
<p>Research model in the test stand; <span class="html-italic">1</span>—prestressed precast slab panel; <span class="html-italic">2</span>—reinforcement of the top ring beam; <span class="html-italic">3</span>—top reinforcement of the slab; <span class="html-italic">4</span>—steel C-profile; <span class="html-italic">5</span>—precast lintel; <span class="html-italic">6</span>—load suspension points; <span class="html-italic">7</span>—visible weights.</p>
Full article ">Figure 7
<p>Frame system mounted on each model’s walls to measure shear strain and deformation angle; <span class="html-italic">H</span>—horizontal shear force; <span class="html-italic">1</span>—rigid diaphragm; <span class="html-italic">2</span>—concrete foundation; <span class="html-italic">3</span>—masonry wall made of AAC; <span class="html-italic">4</span>—measuring base; <span class="html-italic">a</span><sub>0</sub>, <span class="html-italic">c</span><sub>0</sub>—horizontal part of the frame system; <span class="html-italic">b</span><sub>0</sub>, <span class="html-italic">d</span><sub>0</sub>—vertical part of the frame system; <span class="html-italic">e</span><sub>0</sub>, <span class="html-italic">f</span><sub>0</sub>—diagonal part of the frame system.</p>
Full article ">Figure 8
<p>Deformation of measuring base (frame system) due to the action of shear force; <span class="html-italic">H</span>—horizontal shear force; <span class="html-italic">1</span>—rigid diaphragm; <span class="html-italic">2</span>—concrete foundation; <span class="html-italic">3</span>—masonry wall made of AAC; <span class="html-italic">4</span>—measuring base before deformation; <span class="html-italic">5</span>—measuring base after deformation; <span class="html-italic">a</span><sub>d</sub>, <span class="html-italic">c</span><sub>d</sub>—deformed horizontal part of the frame system; <span class="html-italic">b</span><sub>d</sub>, <span class="html-italic">d</span><sub>d</sub>—deformed vertical part of the frame system; <span class="html-italic">e</span><sub>d</sub>, <span class="html-italic">f</span><sub>d</sub>—deformed diagonal part of the frame system.</p>
Full article ">Figure 9
<p>Deformation of measuring base resulting from flexural deformation; <span class="html-italic">V</span>—vertical force; <span class="html-italic">M</span>—in-plane bending moment; <span class="html-italic">1</span>—rigid diaphragm; <span class="html-italic">2</span>—concrete foundation; <span class="html-italic">3</span>—masonry wall made of AAC; <span class="html-italic">4</span>—measuring base before deformation; <span class="html-italic">a</span><sub>0</sub>, <span class="html-italic">c</span><sub>0</sub>—undeformed horizontal part of the frame system; <span class="html-italic">e</span><sub>1</sub>, <span class="html-italic">f</span><sub>1</sub>—deformed diagonal part of the frame system (result from flexural deformation).</p>
Full article ">Figure 10
<p>Deformation of measuring base resulting from shear deformation; <span class="html-italic">H</span>—horizontal shear force; <span class="html-italic">1</span>—rigid diaphragm; <span class="html-italic">2</span>—concrete foundation; <span class="html-italic">3</span>—masonry wall made of AAC; <span class="html-italic">4</span>—measuring base before deformation, <span class="html-italic">5</span>—measuring base after deformation; <span class="html-italic">a</span><sub>d</sub>, <span class="html-italic">c</span><sub>d</sub>—deformed horizontal part of the frame system; <span class="html-italic">b</span><sub>0</sub>, <span class="html-italic">d</span><sub>0</sub>—undeformed vertical part of the frame system; <span class="html-italic">e</span><sub>s</sub>, <span class="html-italic">f</span><sub>s</sub>—deformed diagonal part of the frame system (result from shear deformation); <math display="inline"><semantics> <mrow> <msub> <mi>θ</mi> <mrow> <mn>1</mn> <mi>s</mi> </mrow> </msub> <mo>,</mo> <msub> <mi>θ</mi> <mrow> <mn>2</mn> <mi>s</mi> </mrow> </msub> <mo>,</mo> <msub> <mi>θ</mi> <mrow> <mn>3</mn> <mi>s</mi> </mrow> </msub> <mo>,</mo> <msub> <mi>θ</mi> <mrow> <mn>4</mn> <mi>s</mi> </mrow> </msub> </mrow> </semantics></math>—values of partial strain deformation angles.</p>
Full article ">Figure 11
<p>The crack pattern of tested masonry buildings; (<b>a</b>) front view of MW-AAC-010/1 model; (<b>b</b>) back view of MW-AAC-010/1 model; (<b>c</b>) front view of MW-AAC-010/2 model; (<b>d</b>) back view of MW-AAC-010/2 model; the blue arrow marks the horizontal load.</p>
Full article ">Figure 12
<p>The crack propagation—MW-AAC-010/1 model; (<b>a</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 32.23 kN; (<b>b</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 46.39 kN; (<b>c</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 58.22 kN; (<b>d</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 42.40 kN (post-peak behavior).</p>
Full article ">Figure 13
<p>The crack propagation—MW-AAC-010/2 model; (<b>a</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 48.05 kN; (<b>b</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 48.60 kN; (<b>c</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 69.25 kN; (<b>d</b>) crack pattern—<span class="html-italic">H</span><sub>x</sub> = 42.77 kN (post-peak behavior).</p>
Full article ">Figure 14
<p>Post peak deformation analysis—MW-AAC-010/1 model—<span class="html-italic">H</span><sub>x</sub> = 42.40 kN; (<b>a</b>) displacement along the <span class="html-italic">X</span> axis; (<b>b</b>) displacement along the <span class="html-italic">Z</span> axis.</p>
Full article ">Figure 15
<p>Relationship between horizontal force and strain deformation angle for MW-AAC-010/1 model; (<b>a</b>) results for A and B wall (<b>b</b>) results for 1 and 2 wall.</p>
Full article ">Figure 16
<p>Relationship between horizontal force and strain deformation angle for MW-AAC-010/2 model; (<b>a</b>) results for A and B wall (<b>b</b>) results for 1 and 2 wall.</p>
Full article ">Figure 17
<p>Behavior phases of stiffening walls; (<b>a</b>) wall with door opening (<b>b</b>) wall without door opening.</p>
Full article ">Figure 18
<p>Relation between the <span class="html-italic">H</span><sub>x,i</sub>/<span class="html-italic">H</span><sub>u</sub> and <span class="html-italic">Θ</span><sub>A</sub>/<span class="html-italic">Θ</span><sub>B</sub> for the MB-AAC-010/2 model.</p>
Full article ">Figure 19
<p>Total wall stiffness method [<a href="#B6-materials-15-07404" class="html-bibr">6</a>]: (<b>a</b>) division of a wall with openings into component elements, (<b>b</b>) wall deformation caused by horizontal loads.</p>
Full article ">
17 pages, 6183 KiB  
Article
Waste Glass Valorization as Raw Material in the Production of Portland Clinker and Cement
by Alina Bădănoiu, Adriana Moanță, Ovidiu Dumitrescu, Adrian Ionuț Nicoară and Roxana Trușcă
Materials 2022, 15(20), 7403; https://doi.org/10.3390/ma15207403 - 21 Oct 2022
Cited by 3 | Viewed by 1824
Abstract
The paper presents experimental results regarding the synthesis of Portland clinker starting from raw mixes based on two types of clayey precursors, i.e., clay and marl (the most common types of raw materials used in the cement industry), with and without glass waste [...] Read more.
The paper presents experimental results regarding the synthesis of Portland clinker starting from raw mixes based on two types of clayey precursors, i.e., clay and marl (the most common types of raw materials used in the cement industry), with and without glass waste content. The soda-lime glass waste addition (5.36–5.59 wt %), used to control the silica ratio of the raw mix, improved the raw mix burnability and decreased the calcination temperature (by 20 °C), leading to a decrease in fuel consumption and contributing to the reduction in CO2 emissions associated with clinker and cement production. The clinkers obtained by the calcination of raw mixes with glass waste content at 1430 °C with a 30 min plateau had a similar mineralogical composition and microstructure to the clinkers obtained from the reference raw mixes and fulfilled the requirements of the specific standard EN 197-1. The obtained clinkers were used to produce two types of Portland cement, i.e., a unitary cement (CEM I) and a binary blended cement with slag (CEM II/B-S). The main characteristics of these cements, i.e., loss on ignition, insoluble residue, sulfate and chloride contents, as well as the setting time and soundness, meet the conditions stipulated in the EN 197-1 standard. The values of compressive strength, assessed on mortars after 2, 7 and 28 days of curing, allow the classification of all CEM I cements in the 42.5 R class. In the case of CEM II/B-S cements, those obtained from raw mixes with clay can be classified in the 42.5 N class, while those obtained from raw mixes with marl are classified in the 32.5 R class. Full article
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Figure 1

Figure 1
<p>XRD patterns of (<b>a</b>) limestone; (<b>b</b>) clay; (<b>c</b>) marl.</p>
Full article ">Figure 2
<p>Composition of raw mixes used for clinker and cement manufacture.</p>
Full article ">Figure 3
<p>Free lime assessed on the clinkers obtained by calcination at different temperatures and plateaus (red line = maximum free lime content recommended in clinkers).</p>
Full article ">Figure 4
<p>XRD patterns of clinkers obtained by calcination of raw mixes with/without WG content: (<b>a</b>) raw mix based on clay; (<b>b</b>) raw mix based on marl.</p>
Full article ">Figure 5
<p>Rietveld quantification of crystalline phases on clinkers obtained by calcination of raw mixes with/without WG content: Rc and Gc—raw mix based on clay; Rm and Gm—raw mix based on marl. Rc and Rm were obtained by thermal treatment at 1450 °C, 30 min; Gc and Gm were obtained by thermal treatment at 1430 °C, 30 min.</p>
Full article ">Figure 6
<p>SEM images of Rc and Rm clinkers at different magnifications; A—alite; B—belite; C—calcium ferrite aluminate; M—melt; pores are indicated by arrows.</p>
Full article ">Figure 7
<p>SEM image (<b>a</b>) and elemental mapping (<b>b</b>–<b>f</b>) of Rc clinker.</p>
Full article ">Figure 8
<p>SEM images (different magnifications) of Gc calcined at different temperatures and plateaus (1400 °C + 20 min and 1430 °C + 30 min).</p>
Full article ">Figure 9
<p>SEM image (<b>a</b>) and elemental mapping (<b>b</b>–<b>f</b>) of Gc clinker.</p>
Full article ">Figure 10
<p>SEM images (different magnifications) of Gm calcined at different temperatures and plateaus (1400 °C + 20 min and 1430 °C + 30 min).</p>
Full article ">Figure 11
<p>Compressive strengths vs. time for CEM I and CEM II B-S, with sand or WG and based on (<b>a</b>) clay; (<b>b</b>) marl.</p>
Full article ">
13 pages, 10296 KiB  
Article
Hot Deformation Behavior and Processing Maps of ZnSnO3/Cu Composites
by Wei-Jian Li, Zi-Yao Chen, Xiao-Peng Tang, Wen-Zhu Shao and Liang Zhen
Materials 2022, 15(20), 7402; https://doi.org/10.3390/ma15207402 - 21 Oct 2022
Cited by 2 | Viewed by 1414
Abstract
In this work, we designed ternary ZnSnO3 particle-reinforced Cu matrix composites and evaluated the hot deformation behavior of ZnSnO3/Cu composites. The hot deformation characteristics of typical dynamic recrystallization were probed by the resulting true stress–strain curves of ZnSnO3/Cu [...] Read more.
In this work, we designed ternary ZnSnO3 particle-reinforced Cu matrix composites and evaluated the hot deformation behavior of ZnSnO3/Cu composites. The hot deformation characteristics of typical dynamic recrystallization were probed by the resulting true stress–strain curves of ZnSnO3/Cu composites. The influences of deformation conditions, including temperatures (650–850 °C) and strain rates (0.01–5 s−1), on the flow stress of the designed composites were investigated. This revealed that the peak stress increased with the increasing of strain rate and decreasing of temperature. Additionally, the activation energy was calculated to be 237.05 kJ/mol and followed by yielding a constitutive equation for low-stress ZnSnO3/Cu composites. The processing maps established by dynamic materials model theory indicated that the designed composites possessed excellent hot workability, and then the processing parameters (790–850 °C and 0.01–0.04 s−1) of the ZnSnO3/Cu composites were determined for practical industrial production. Our work discloses the deformation behavior of ZnSnO3/Cu matrix composites and extends the rational process design for ternary ceramic/metal materials with excellent hot workability. Full article
(This article belongs to the Special Issue Manufacturing and Mechanical Properties of Metal Matrix Composites)
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Figure 1

Figure 1
<p>The morphology of electrolytic Cu powder (<b>a</b>), atomizing CuZr alloy powder (<b>b</b>), atomizing CuLa alloy powder (<b>c</b>), and ZnSnO<sub>3</sub> powder (<b>d</b>).</p>
Full article ">Figure 2
<p>(<b>a</b>,<b>b</b>) The morphology of the mixed powders. (<b>c</b>,<b>d</b>) Microscopic structure of the ZnSnO<sub>3</sub>/Cu composites.</p>
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<p>Relationship between the true stress and strain of the ZnSnO<sub>3</sub>/Cu composites at 650–850 °C and strain rates: (<b>a</b>) 0.01 s<sup>−1</sup>, (<b>b</b>) 0.1 s<sup>−1</sup>, (<b>c</b>) 1 s<sup>−1</sup>, and (<b>d</b>) 5 s<sup>−1</sup>.</p>
Full article ">Figure 4
<p>Microstructures of the ZnSnO<sub>3</sub>/Cu composites at 0.01 s<sup>−1</sup> strain rates with different temperatures: (<b>a</b>) 650 °C, (<b>b</b>) 700 °C, (<b>c</b>) 750 °C, and (<b>d</b>) 800 °C. CD presents the compression direction of the sample.</p>
Full article ">Figure 5
<p>Microstructures of the ZnSnO<sub>3</sub>/Cu composites at 1 s<sup>−1</sup> strain rates under different temperatures: (<b>a</b>) 650 °C, (<b>b</b>) 700 °C, (<b>c</b>) 750 °C, and (<b>d</b>) 800 °C. CD presents the compression direction of the sample.</p>
Full article ">Figure 6
<p>Relationships between (<b>a</b>) <math display="inline"><semantics> <mrow> <mrow> <mi>ln</mi> <mrow> <mover> <mi>ε</mi> <mo>.</mo> </mover> </mrow> </mrow> </mrow> </semantics></math> − <math display="inline"><semantics> <mi>σ</mi> </semantics></math>; (<b>b</b>) <math display="inline"><semantics> <mrow> <mrow> <mi>ln</mi> <mover> <mi>ε</mi> <mo>.</mo> </mover> </mrow> </mrow> </semantics></math> − <math display="inline"><semantics> <mrow> <mrow> <mi>ln</mi> <mi>σ</mi> </mrow> </mrow> </semantics></math>; (<b>c</b>) <math display="inline"><semantics> <mrow> <mrow> <mi>ln</mi> <mrow> <mtext> </mtext> <mover> <mi>ε</mi> <mo>.</mo> </mover> <mtext> </mtext> </mrow> </mrow> </mrow> </semantics></math> − <math display="inline"><semantics> <mrow> <mi>ln</mi> <mi>sin</mi> <mi mathvariant="normal">h</mi> <mfenced> <mrow> <mrow> <mi>α</mi> <mi>σ</mi> </mrow> </mrow> </mfenced> </mrow> </semantics></math>, and (<b>d</b>) <math display="inline"><semantics> <mrow> <mi>ln</mi> <mrow> <mtext> </mtext> <mover> <mi>ε</mi> <mo>.</mo> </mover> <mtext> </mtext> </mrow> </mrow> </semantics></math> − 1000/<span class="html-italic">T</span>.</p>
Full article ">Figure 7
<p>Relationship between <math display="inline"><semantics> <mrow> <mi>lnZ</mi> </mrow> </semantics></math> and <math display="inline"><semantics> <mrow> <mi>ln</mi> <mi>sin</mi> <mi mathvariant="normal">h</mi> <mfenced> <mrow> <mrow> <mi>α</mi> <mi>σ</mi> </mrow> </mrow> </mfenced> </mrow> </semantics></math> of ZnSnO<sub>3</sub>/Cu composites.</p>
Full article ">Figure 8
<p>Processing maps of ZnSnO<sub>3</sub>/Cu composites at a true strain of (<b>a</b>) 0.1, (<b>b</b>) 0.5, (<b>c</b>) 0.7, (<b>d</b>) 0.9, and (<b>e</b>) 0.95.</p>
Full article ">Figure 9
<p>Microstructures of the ZnSnO<sub>3</sub>/Cu composites at 800 °C with different strain rates: (<b>a</b>) 0.01 s<sup>−1</sup>, (<b>b</b>) 1 s<sup>−1</sup>. CD presents the compression direction of the sample. The red dotted circle in (<b>b</b>) indicates crack.</p>
Full article ">
20 pages, 8405 KiB  
Article
Thermo-Mechanical Coupling Model of Bond-Based Peridynamics for Quasi-Brittle Materials
by Haoran Zhang, Lisheng Liu, Xin Lai, Hai Mei and Xiang Liu
Materials 2022, 15(20), 7401; https://doi.org/10.3390/ma15207401 - 21 Oct 2022
Cited by 3 | Viewed by 1736
Abstract
The mechanical properties of quasi-brittle materials, which are widely used in engineering applications, are often affected by the thermal condition of their service environment. Moreover, the materials appear brittle when subjected to tensile loading and show plastic characteristics under high pressure. These two [...] Read more.
The mechanical properties of quasi-brittle materials, which are widely used in engineering applications, are often affected by the thermal condition of their service environment. Moreover, the materials appear brittle when subjected to tensile loading and show plastic characteristics under high pressure. These two phenomena manifest under different circumstances as completely different mechanical behaviors in the material. To accurately describe the mechanical response, the material behavior, and the failure mechanism of quasi-brittle materials with the thermo-mechanical coupling effect, the influence of the thermal condition is considered in calculating bond forces in the stretching and compression stages, based on a new bond-based Peridynamic (BB-PD) model. In this study, a novel bond-based Peridynamic, fully coupled, thermo-mechanical model is proposed for quasi-brittle materials, with a heat conduction component to account for the effect of the thermo-mechanical coupling. Numerical simulations are carried out to demonstrate the validity and capability of the proposed model. The results reveal that agreement could be found between our model and the experimental data, which show good reliability and promise in the proposed approach. Full article
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<p>Schematic diagram of the BB-PD model.</p>
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<p>Stress–strain diagram of tensile behavior.</p>
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<p>Stress-strain diagram of compression behavior.</p>
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<p>The two-dimensional flat plate subjected to heating loading.</p>
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<p>Comparison of calculation results of different methods. (<b>a</b>) Temperature; (<b>b</b>) Vertical displacement.</p>
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<p>The VBD specimen used in experiments.</p>
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<p>Splitting and destruction process of the VBD specimen. (<b>a</b>) 0 s; (<b>b</b>) 70 s; (<b>c</b>) 80 s; (<b>d</b>) 110 s; (<b>e</b>) 130 s; (<b>f</b>) 170 s.</p>
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<p>(<b>a</b>) Specimen before experiment; (<b>b</b>) Specimen after experiment; (<b>c</b>) The PD simulation result.</p>
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<p><span class="html-italic">m</span>-convergence with a fixed horizon size.</p>
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<p>(<b>a</b>) The vertical displacement of point A with a different non-locality parameter <span class="html-italic">m</span>; (<b>b</b>) an enlarged detail from (<b>a</b>).</p>
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<p><math display="inline"><semantics> <mi>δ</mi> </semantics></math>-convergence with a fixed parameter <span class="html-italic">m</span>.</p>
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<p>(<b>a</b>) The vertical displacement of point A with different horizon sizes <math display="inline"><semantics> <mi>δ</mi> </semantics></math>; (<b>b</b>) an enlarged detail from (<b>a</b>).</p>
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<p>Schematic diagram of the geometry and boundary condition of the ceramic subjected to cold shock.</p>
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<p>Comparison of ceramic plate thermal impact cracking results: (<b>a</b>) Specimens after thermal shock [<a href="#B36-materials-15-07401" class="html-bibr">36</a>]; (<b>b</b>) PD simulation results for the 1/2 model.</p>
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<p>(<b>a</b>) Granite samples containing prefabricated cracks; (<b>b</b>) PD model; (<b>c</b>) composition distribution of granite.</p>
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<p>PD simulation of damage in granite under uniaxial compression after thermal cycling. (<b>a</b>) Thermal cycle stage; (<b>b</b>) Uniaxial compression stage.</p>
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<p>Comparison of PD simulated cracks extension with experiment [<a href="#B37-materials-15-07401" class="html-bibr">37</a>,<a href="#B38-materials-15-07401" class="html-bibr">38</a>].</p>
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8 pages, 1414 KiB  
Article
Ionic Liquid Mixture Electrolyte Matching Porous Carbon Electrodes for Supercapacitors
by Yuhua Zhao, Yujuan Chen, Quanzhou Du, Kelei Zhuo, Lifang Yang, Dong Sun and Guangyue Bai
Materials 2022, 15(20), 7400; https://doi.org/10.3390/ma15207400 - 21 Oct 2022
Cited by 2 | Viewed by 1669
Abstract
Ionic liquids (ILs), with their wide electrochemical stable potential window, are promising electrolytes for supercapacitors (SCs). The suitable matching of the ion size and shape of the ILs to the pore size and structure of porous carbon (PC) electrode materials can realize the [...] Read more.
Ionic liquids (ILs), with their wide electrochemical stable potential window, are promising electrolytes for supercapacitors (SCs). The suitable matching of the ion size and shape of the ILs to the pore size and structure of porous carbon (PC) electrode materials can realize the enhanced capacitive performance of the SCs. Here we report an interesting result: The capacitance of PC-based SCs shows a quasi-sinusoidal relationship with the composition (mass fraction) of the binary IL mixture as the electrolyte. This relationship is also interpreted based on the matching between the pore sizes of the PC materials and the size/shape of various ions of the IL mixture electrolyte. This can provide a new strategy to improve the performance of SCs by formulating a suitable mixture of different ILs to match the carbon-based electrode materials with a special pore size distribution. Full article
(This article belongs to the Special Issue Nano and Advanced Material Engineering)
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<p>Pore size distribution of the activated carbon.</p>
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<p>Electrochemical performance of [Bmim][TFSI]<span class="html-italic"><sub>w</sub></span>[Emim][BF<sub>4</sub>]<sub>1<span class="html-italic">-w</span></sub> electrolyte at 30 °C: (<b>a</b>) CV curves at 50 mV S<sup>−1</sup> and (<b>b</b>) GCD curves at 1 A g<sup>−1</sup>. (<b>c</b>) CV and (<b>d</b>) GCD curves in [Bmim][TFSI]<sub>0.2</sub>[Emim][BF<sub>4</sub>]<sub>0.8</sub> electrolyte at 30 °C.</p>
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<p>Plots of (<b>a</b>) specific capacitance and (<b>b</b>) conductivity/viscosity vs. the mass fraction <span class="html-italic">w</span> of the binary IL mixtures ([Bmim][TFSI]<span class="html-italic"><sub>w</sub></span>[Emim][BF<sub>4</sub>]<sub>1-<span class="html-italic">w</span></sub>) at 30 °C.</p>
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20 pages, 3417 KiB  
Article
Fused Filament Fabrication of Alumina/Polymer Filaments for Obtaining Ceramic Parts after Debinding and Sintering Processes
by Claudio Tosto, Mario Bragaglia, Francesca Nanni, Giuseppe Recca and Gianluca Cicala
Materials 2022, 15(20), 7399; https://doi.org/10.3390/ma15207399 - 21 Oct 2022
Cited by 9 | Viewed by 3169
Abstract
In this paper, a hybrid commercially available alumina/polymer filament was 3D printed and thermally treated (debinding and sintering) to obtain ceramic parts. Microscopic and spectroscopic analysis was used to thoroughly characterize the green and sintered parts in terms of their mesostructured, as well [...] Read more.
In this paper, a hybrid commercially available alumina/polymer filament was 3D printed and thermally treated (debinding and sintering) to obtain ceramic parts. Microscopic and spectroscopic analysis was used to thoroughly characterize the green and sintered parts in terms of their mesostructured, as well as their flexural properties. The sintered samples show an α alumina crystalline phase with a mean density of 3.80 g/cm3, a tensile strength of 232.6 ± 12.3 MPa, and a Vickers hardness of 21 ± 0.7 GPa. The mean thermal conductivity value at room temperature was equal to 21.52 ± 0.02 W/(mK). The values obtained through FFF production are lower than those obtained by conventional processes as the 3D-printed samples exhibited imperfect interlayer bonding and voids similar to those found in the structures of polymeric FFFs. Nonetheless, the highly filled ceramic filament is suitable for use in affordable and easy-to-operate FFF machines, as shown by the cost analysis of a real printed and sintered FFF part. Full article
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<p>FFF printer: (<b>a</b>) direct feeding system, (<b>b</b>) building area.</p>
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<p>Sample sketch with nominal dimensions in mm (<b>top</b>) and 3D-printed samples (<b>bottom</b>): (<b>a</b>) cubes; (<b>b</b>) flexural samples.</p>
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<p>SEM images of: filament at magnifications of (<b>a</b>) 50× and (<b>b</b>) 5k×; green parts at magnifications of 100× (<b>c</b>), and 500× (<b>d</b>).</p>
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<p>XRD pattern of 3D-printed sintered Al<sub>2</sub>O<sub>3.</sub></p>
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<p>Morphology of sintered 3D-printed alumina sample observed by SEM. (<b>a</b>) Low magnification, (<b>b</b>) detail of Vickers hardness imprint, (<b>c</b>) porosity (arrows) as a result of the FFF process, (<b>d</b>) detail of porosity.</p>
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<p>Representative flexural stress–strain curve of Al<sub>2</sub>O<sub>3</sub> 3D-printed sintered sample.</p>
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<p>SEM analysis of the sintered sample’s fracture surface: (<b>a</b>) initial crack point (red circle); (<b>b</b>) FFF-induced defects (red arrows) and bottom layers (red dashed ellipse).</p>
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<p>FFF alumina: (<b>a</b>) green part; (<b>b</b>) sintered part.</p>
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14 pages, 4225 KiB  
Article
Reducing Surface Roughness of 3D Printed Short-Carbon Fiber Reinforced Composites
by Raluca Maier, Sebastian-Gabriel Bucaciuc and Andrei Cristian Mandoc
Materials 2022, 15(20), 7398; https://doi.org/10.3390/ma15207398 - 21 Oct 2022
Cited by 9 | Viewed by 1959
Abstract
A 100 W fibre laser source was used to minimize the surface roughness of 3D-printed Onyx parts. Furthermore, this study aimed to determine the mechanism of surface finishing, the influence of the laser process parameters (laser power, pulse frequency, and laser scanning path) [...] Read more.
A 100 W fibre laser source was used to minimize the surface roughness of 3D-printed Onyx parts. Furthermore, this study aimed to determine the mechanism of surface finishing, the influence of the laser process parameters (laser power, pulse frequency, and laser scanning path) on the surface morphology, and the influence of the scanning path on the dimensional accuracy of the investigated Onyx 3D-printed specimens. A significant reduction in surface roughness of 91.15% was achieved on the S3 Onyx 3D-printed specimen following laser surface polishing treatment using a 50 W laser power and a frequency of 50 kHz. The laser scanning path had little influence on the surface roughness, but had a major impact on the geometrical deviation of the treated sample. Full article
(This article belongs to the Special Issue 3D Printing: Materials, Properties, and Applications)
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<p>The laser polishing process.</p>
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<p>Experimental methodology from design to manufacturing and post-processing.</p>
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<p>Onyx 3D-printed specimen sketch.</p>
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<p>Roughness measurement strategy.</p>
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<p>Experimental setup for the laser surface polishing treatment.</p>
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<p>Roughness measurements at 90° and 45° angles for the investigated specimens following laser polishing post-processing using different ED.</p>
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<p>Roughness reduction at 90° and 45° angle after laser polishing post-processing.</p>
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<p>Variation in surface roughness reduction (measured at 90°) with energy density.</p>
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<p>Three-dimensional (3D) topography of the specimen before and after the laser polishing: (<b>a</b>) unpolished; (<b>b</b>) S1: 60 W laser power, 90 kHz frequency.</p>
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<p>In-plane section view of S1; (<b>a</b>) before and (<b>b</b>) after laser polishing.</p>
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<p>Three-dimensional (3D) topography of the specimen before and after the laser polishing: (<b>a</b>) unpolished; (<b>b</b>) S5: 60 W laser power, 90 kHz frequency.</p>
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<p>In-plane section view of S5; (<b>a</b>) before and (<b>b</b>) after laser polishing.</p>
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<p>Three-dimensional (3D) topography of the specimen before and after the laser polishing: (<b>a</b>) unpolished; (<b>b</b>) S3: 50 W laser power, 50 kHz frequency.</p>
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<p>In-plane section view of S3; (<b>a</b>) before and (<b>b</b>) after laser polishing.</p>
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18 pages, 8384 KiB  
Article
Quick Curing Mechanisms for All-Season Paints and Renders
by Ivan Cabrera, Markus Rückel, Volodymyr Boyko, Roland Baumstark and Immanuel Willerich
Materials 2022, 15(20), 7397; https://doi.org/10.3390/ma15207397 - 21 Oct 2022
Cited by 1 | Viewed by 2289
Abstract
Paints and coatings are required to quickly cure under a broad variety of environmental conditions and deliver solid long-term performance. Achieving a balance during all seasons between quick curing of a coating film, i.e., early rain resistance, while maintaining sufficient workability and open [...] Read more.
Paints and coatings are required to quickly cure under a broad variety of environmental conditions and deliver solid long-term performance. Achieving a balance during all seasons between quick curing of a coating film, i.e., early rain resistance, while maintaining sufficient workability and open time for an optimized aesthetic appearance is a challenge for the architectural coatings industry. This article describes how the colloidal physics differs between the current standard mechanism to achieve early rain resistance by inhibited coagulants in winter paints and a new mechanism that provides all-season paints. A combination of advanced physical characterization methods, such as electrophoretic mobility, dynamic light scattering and confocal laser scanning microscopy, in combination with application tests, is used to provide a comprehensive mechanism of the early rain resistance achieved by such paints. In addition, it is shown that this new system can be transferred to wood coatings and organic renders. The key finding of this article is that all-season paints combining early rain resistance at cold and damp conditions with open time at high temperatures and dry conditions rely on fast paint film formation with high early integrity rather than coagulants triggered by base evaporation. Full article
(This article belongs to the Special Issue Recent Advances in Coatings, Adhesives and Construction Materials)
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<p>Criteria for all-season paints.</p>
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<p>Stages of film formation for latex particles. T is the temperature during the film formation. MFFT is the minimum film formation temperature of the latex.</p>
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<p>ERR rating of the paints with the reference binder A, the reference binder with inhibited coagulant (Binder B) and the new binder D (containing tertiary polyamine), formulated as shown in <a href="#materials-15-07397-t0A1" class="html-table">Table A1</a>. The tests were carried out according to <a href="#sec2dot2-materials-15-07397" class="html-sec">Section 2.2</a>. (<b>a</b>) The humidity at 5 °C was approximately 50%; (<b>b</b>) at 25 °C, the humidity was approximately 45%. It should be noted that a small difference in the humidity between 5 and 25 °C was accepted to avoid differences in air movement above the drying films by active ventilation, the latter having a far greater effect on the time to ERR than the former. This is not possible when using a humidity-controlled chamber due to the much lower absolute humidity at 5 °C vs. 25 °C, which requires faster ventilation to hold the relative humidity constant; thus, artificially accelerating the time to ERR at 5 °C.</p>
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<p>Comparison of the open time of paints with the reference binder A and the new binder D (<b>b</b>). The paint rollers were saturated with the same amount of the paint formulation from <a href="#app1-materials-15-07397" class="html-app">Appendix A</a> with both binders and rested for 40 min before applying them to a paper substrate (<b>a</b>).</p>
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<p>Electrophoretic mobility of the new binder D, binder C (without a tertiary polyamine) and binder B with an inhibited coagulant. The mobility curve for binder A is very similar to binder C.</p>
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<p>Evolution of pH during drying of the façade paint formulation from <a href="#materials-15-07397-t0A1" class="html-table">Table A1</a> each with binder D (green) and with the reference binder A (blue). The pH was measured on the coating surface using a surface pH electrode.</p>
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<p>Drying kinetics of the reference latex A and the new binder D. Each binder was studied twice (solid and dashed lines). The thickness decline over time is very similar for all of the curves shown.</p>
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<p>Rewetting kinetics of partially dried paints. If the paint with binder D is followed for a longer exposure time, the result does not change, i.e., no redissolution occurs. Circles mark the areas where constant or changing binder and TiO<sub>2</sub> particle positions can be observed best.</p>
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<p>ERR test of wood stains, formulated according to <a href="#materials-15-07397-t0A2" class="html-table">Table A2</a> and tested according to <a href="#sec2dot2-materials-15-07397" class="html-sec">Section 2.2</a>. The temperature during drying was 5 °C, and the humidity was approximately 75%.</p>
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<p>ERR test of white wood paints, formulated according to <a href="#materials-15-07397-t0A3" class="html-table">Table A3</a> and tested according to <a href="#sec2dot2-materials-15-07397" class="html-sec">Section 2.2</a>. The temperature during drying was 5 °C, and the humidity was approximately 75%.</p>
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<p>EIFS system with all components. The topic of this section is the topcoat render.</p>
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<p>ERR tests of white render topcoats, formulated according to <a href="#materials-15-07397-t0A4" class="html-table">Table A4</a> in <a href="#app1-materials-15-07397" class="html-app">Appendix A</a> and applied and tested according to <a href="#sec2dot2-materials-15-07397" class="html-sec">Section 2.2</a>. Red line marks the highest spot with water exposure.</p>
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<p>Setup for early rain resistance testing for façade paints.</p>
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<p>Setup for early rain resistance testing for wood paints.</p>
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<p>Gravimetric drying kinetics study recorded from films drawn on Leneta foil with a 400 µm doctor blade. The amount of paint applied for binder A was 11.85 g and 11.13 g for binder D. A denotes the paint with reference binder A; D denotes the paint with the new binder containing a tertiary polyamine. The green vertical bar is the latest point in the drying time when the paint behaves as a liquid (from touching with a glove); the red vertical bar is the touch dry point; whereas, in between, the irreversible marks remain on the touched paint surface.</p>
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13 pages, 3536 KiB  
Article
Investigating the Effect of PCL Concentrations on the Characterization of PLA Polymeric Blends for Biomaterial Applications
by Solechan Solechan, Agus Suprihanto, Susilo Adi Widyanto, Joko Triyono, Deni Fajar Fitriyana, Januar Parlaungan Siregar and Tezara Cionita
Materials 2022, 15(20), 7396; https://doi.org/10.3390/ma15207396 - 21 Oct 2022
Cited by 13 | Viewed by 2811
Abstract
Polylactic acid (PLA) and polycaprolactone (PCL) are synthetic polymers that are extensively used in biomedical applications. However, the PLA/PCL blend produced by ball milling, followed by pressure compaction and sintering, has not been extensively explored. The goal of this research is to investigate [...] Read more.
Polylactic acid (PLA) and polycaprolactone (PCL) are synthetic polymers that are extensively used in biomedical applications. However, the PLA/PCL blend produced by ball milling, followed by pressure compaction and sintering, has not been extensively explored. The goal of this research is to investigate the effect of the composition of biomaterials derived from PLA and PCL prepared by ball milling, followed by pressure compaction and sintering, on mechanical and physical properties. PCL and PLA with various concentrations were blended utilizing a ball milling machine for 2 h at an 80-rpm rotation speed. The obtained mixture was placed in a stainless steel 304 mold for the compacting process, which uses a pressure of 30 MPa to create a green body. The sintering procedure was carried out on the green body created at 150 °C for 2 h using a digital oven. The obtained PLA/PCL blend was tested using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Scanning electron microscopy (SEM), density, porosity, and three-point bending. Following the interaction between PCL and PLA in the PLA/PCL blend, the FTIR spectra and XRD diffractograms obtained in this work revealed a number of modifications in the functional groups and crystal phase. The 90PLA specimen had the best mechanical properties, with a maximum force and displacement of 51.13 N and 7.21 mm, respectively. The porosity of the PLA/PCL blend decreased with increasing PLA concentration so that the density and flexural properties of the PLA/PCL blend increased. The higher PCL content decreased the stiffness of the PLA molecular chain, consequently reducing its flexural properties. Full article
(This article belongs to the Special Issue Synthesis, Performance and Application of Polymers Materials)
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<p>The preparation process of PLA/PCL blend.</p>
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<p>FTIR spectra of samples.</p>
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<p>X-ray diffraction (XRD) patterns of samples.</p>
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<p>SEM images of surfaces (<b>a</b>) 90PLA, (<b>b</b>) 80PLA, (<b>c</b>) 70PLA, and (<b>d</b>) 60PLA at 5000× magnification.</p>
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<p>The density and porosity of PLA/PCL blends.</p>
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<p>The flexural test results on PLA/PCL blend.</p>
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22 pages, 3366 KiB  
Article
Prediction of Corrosion-Induced Longitudinal Cracking Time of Concrete Cover Surface of Reinforced Concrete Structures under Load
by Jian Wang, Yongyu Yuan, Qiang Xu and Hongtu Qin
Materials 2022, 15(20), 7395; https://doi.org/10.3390/ma15207395 - 21 Oct 2022
Cited by 8 | Viewed by 1625
Abstract
Reinforced concrete (RC) structures suffer from different types of loads during service life, and the corrosion characteristics of steel bars embedded in concrete under load are different from those under non-load. In this paper, when the interface between steel bars and concrete (IBSC) [...] Read more.
Reinforced concrete (RC) structures suffer from different types of loads during service life, and the corrosion characteristics of steel bars embedded in concrete under load are different from those under non-load. In this paper, when the interface between steel bars and concrete (IBSC) cracked and the concrete cover surface (CCS) cracked, the effects of load on the critical corrosion depth of steel bars were analysed based on the thick-walled cylinder model, and a prediction model for the corrosion-induced longitudinal cracking (CLC) time (i.e., initiation cracking time) of the CCS of RC structures under load was proposed. Finally, the influence of load on the CLC time of CCS was discussed on the basis of the proposed prediction model. The results showed that the load had a significant effect on the critical corrosion depth of steel bars when the IBSC cracked induced by corrosion, while the influence of load on the critical corrosion depth of steel bars when the CCS cracked induced by corrosion was not obvious. When the CCS cracks induced by corrosion under load, the influence of the rust-filling layer on the critical corrosion depth of steel bars was larger than that of the load. With the increase in load, the CLC time of CCS decreased. The calculated values of the proposed prediction model were in reasonable agreement with the experimental values, which can provide a reference for durability evaluation and service life prediction of RC structures and lay the foundation for the investigation of the corrosion depth of steel bars in concrete under load. Full article
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<p>Distribution of cracks near the transverse ribs of ribbed steel bars under load.</p>
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<p>Interaction between the ribbed steel bars and the surrounding concrete under load.</p>
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<p>Transformed cross-section before concrete cracking. (<b>a</b>) Original cross-section; (<b>b</b>) transformed cross-section.</p>
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<p>RC beams under the third-point concentrated load.</p>
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<p>Thick-walled cylinder model.</p>
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<p>Relationship between the average thickness of the rust-filling layer and the thickness of the rust layer.</p>
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<p>The rust-filling layer is converted to an equivalent rust layer.</p>
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<p>Radial deformations of concrete and rust layer at the IBSC under the total radial pressure in the non-cracking stage of the concrete cover.</p>
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<p>Critical corrosion depth of steel bars when the IBSC cracks.</p>
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<p>Radial deformations of concrete and rust layers at the IBSC under the total radial pressure in the partial cracking stage of the concrete cover.</p>
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<p>Partitions of the cracked part of the concrete cover.</p>
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<p>Critical corrosion depth of steel bars when the CCS cracks.</p>
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<p>Effects of load, <span class="html-italic">n</span>, and <span class="html-italic">n</span>/<span class="html-italic">n</span><sub>0</sub> on the CLC time of CCS. (<b>a</b>) <span class="html-italic">n</span> = 2; (<b>b</b>) <span class="html-italic">n</span> = 3; (<b>c</b>) <span class="html-italic">n</span> = 4.</p>
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<p>Effects of load, <span class="html-italic">n</span>, and <span class="html-italic">n</span>/<span class="html-italic">n</span><sub>0</sub> on the CLC time of CCS. (<b>a</b>) <span class="html-italic">n</span> = 2; (<b>b</b>) <span class="html-italic">n</span> = 3; (<b>c</b>) <span class="html-italic">n</span> = 4.</p>
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25 pages, 75269 KiB  
Article
Experimental Study on the Influence of Different Factors on the Mechanical Properties of a Soil–Rock Mixture Solidified by Micro-Organisms
by Yongshuai Sun, Jianguo Lv, Ya Tuo and Guihe Wang
Materials 2022, 15(20), 7394; https://doi.org/10.3390/ma15207394 - 21 Oct 2022
Cited by 1 | Viewed by 1844
Abstract
In this paper, we focus on the application of mechanical properties in a soil–rock mixture modified by microbial mineralization under the influence of different factors, including pH value, cementing solution concentration, and cementing time. Cementing fluids and samples with different pH values, calcium [...] Read more.
In this paper, we focus on the application of mechanical properties in a soil–rock mixture modified by microbial mineralization under the influence of different factors, including pH value, cementing solution concentration, and cementing time. Cementing fluids and samples with different pH values, calcium ion concentrations, and mineralization cementation were prepared. The process of urea hydrolysis MICP under different factors was studied. A solidified soil–rock mixture sample under triaxial compression was measured. Then, combined with scanning test methods, such as SEM and XRD, the influence of different factors on the mechanical strength and failure mode of the soil–rock mixture structure was analyzed from a microscopic point of view. The results show that a low concentration of cementing solution with a high concentration of bacteria liquid generated the highest calcium carbonate content and the strongest cementing ability. When the pH value of the cementation solution is six, the cementation effect between the pores is the best, and the deviatoric stress is stronger. When wet-curing samples, short or long curing time will adversely affect the strength of soil–rock mixture samples, the strongest curing and cementing ability is 5 days. The microscopic results show that the microbial mineralization technology fills the pores between the particles, and the interaction force between particles is enhanced to enhance the strength of the soil–rock mixture. Full article
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<p>LB liquid medium before and after inoculation.</p>
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<p>Relationship between shear strain and deviatoric stress of soil–rock mixture.</p>
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<p>Deviatoric stress at different pH values under different confining pressures.</p>
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<p>Samples after the triaxial shear test.</p>
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<p>The relationship between shear strain and deviatoric stress of the soil–rock mixture under different cementation solution concentrations.</p>
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<p>Deviatoric stress at different confining pressures with different cementation solutions.</p>
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<p>Specimen after the triaxial shear test.</p>
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<p>The relationship between shear strain and deviatoric stress of soil–rock mixture under different curing time.</p>
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<p>Deviatoric stress at 300 kPa confining pressure for different curing times.</p>
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<p>Deviatoric stress at 300 kPa confining pressure for different curing times.</p>
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<p>Specimens after triaxial shear test under different curing time.</p>
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<p>SEM micrographs of cement solution pH 6 under different magnifications.</p>
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<p>SEM micrographs of cement solution pH 8 under different magnifications.</p>
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<p>XRD patterns of samples at different pH.</p>
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<p>Element distribution map under different cementation pH.</p>
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<p>Element distribution map under different cementation pH.</p>
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<p>SEM micrographs of 0.5 mol/L cementation solution under different magnifications.</p>
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<p>SEM micrographs of 1.0 mol/L cementation solution under different magnifications.</p>
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<p>XRD patterns of samples at different concentrations.</p>
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<p>Elemental distribution of different cementitious liquid concentrations.</p>
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<p>SEM micrographs of curing for 5 days at different magnifications.</p>
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<p>SEM micrographs of curing for 7 days at different magnifications.</p>
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<p>XRD patterns of samples under different curing times.</p>
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<p>Element distribution diagram for different curing times.</p>
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14 pages, 3976 KiB  
Article
Mathematical Models and Experiments on the Acoustic Properties of Granular Packing Structures (Measurement of Tortuosity in Hexagonal Close-Packed and Face-Centered Cubic Lattices)
by Shuichi Sakamoto, Kyosuke Suzuki, Kentaro Toda and Shotaro Seino
Materials 2022, 15(20), 7393; https://doi.org/10.3390/ma15207393 - 21 Oct 2022
Cited by 3 | Viewed by 1658
Abstract
In this study, the sound absorption characteristics of hexagonal close-packed and face-centered cubic lattices were estimated by theoretical analysis. Propagation constants and characteristic impedances were obtained by dividing each structure into elements perpendicular to the incident direction of sound waves and by approximating [...] Read more.
In this study, the sound absorption characteristics of hexagonal close-packed and face-centered cubic lattices were estimated by theoretical analysis. Propagation constants and characteristic impedances were obtained by dividing each structure into elements perpendicular to the incident direction of sound waves and by approximating each element to a clearance between two parallel planes. Consequently, the propagation constant and the characteristic impedance were treated as a one-dimensional transfer matrix in the propagation of sound waves, and the normal incident sound absorption coefficient was calculated by the transfer matrix method. The theoretical value of the sound absorption coefficient was derived by using the effective density applied to the measured tortuosity. As a result, the theoretical value was becoming closer to the measured value. Therefore, the measured tortuosity is reasonable. Full article
(This article belongs to the Special Issue Advanced Materials Structures for Sound and Vibration Damping)
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<p>Test samples: (<b>a</b>) Hexagonal close-packed lattice (<span class="html-italic">d</span> = 4 mm); (<b>b</b>) Hexagonal close-packed lattice (<span class="html-italic">d</span> = 8 mm); (<b>c</b>) Face-centered cubic lattice (<span class="html-italic">d</span> = 4 mm); (<b>d</b>) Face-centered cubic lattice (<span class="html-italic">d</span> = 8 mm).</p>
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<p>Configuration diagram of a two-microphone impedance tube for the absorption coefficient measurement.</p>
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<p>Configuration diagram of the tortuosity measurement.</p>
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<p>Measurement results of the tortuosity.</p>
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<p>Analysis unit in each structure: (<b>a</b>) Hexagonal close-packed lattice; (<b>b</b>) Face-centered cubic lattice.</p>
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<p>Analysis unit at the top of the sample: (<b>a</b>) Hexagonal close-packed lattice; (<b>b</b>) Face-centered cubic lattice.</p>
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<p>Divided element approximated to the clearance between two planes: (<b>a</b>) Divided element (face-centered cubic); (<b>b</b>) Approximated clearance between two planes.</p>
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<p>Approximated clearance between two planes at the element in contact with the sample holder: (<b>a</b>) Divided element in contact with the sample holder on two sides; (<b>b</b>) Divided element in contact with the sample holder on one side.</p>
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<p>Cartesian coordinate system for the parallel clearance between the two planes.</p>
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<p>Sound incident area, incident plane, and transmission plane of approximated clearance between two planes in <a href="#materials-15-07393-f007" class="html-fig">Figure 7</a>b and <a href="#materials-15-07393-f009" class="html-fig">Figure 9</a>.</p>
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<p>Equivalent circuit in the analysis unit (cascade connecting the transfer matrix of each element).</p>
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<p>Equivalent circuit of the whole sample (parallel connection of the cascaded <span class="html-italic">T<sub>unit</sub></span>).</p>
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<p>Comparison between the experimental and calculated values (considering tortuosity in <a href="#sec3dot2-materials-15-07393" class="html-sec">Section 3.2</a> and tortuosity in Reference (Lee et al. 2009) [<a href="#B5-materials-15-07393" class="html-bibr">5</a>]) of the peak frequency and the sound absorption coefficient: (<b>a</b>) Hexagonal close-packed lattice (<span class="html-italic">d</span> = 4 mm); (<b>b</b>) Hexagonal close-packed lattice (<span class="html-italic">d</span> = 8 mm); (<b>c</b>) Face-centered cubic lattice (<span class="html-italic">d</span> = 4 mm); and (<b>d</b>) Face-centered cubic lattice (<span class="html-italic">d</span> = 8 mm).</p>
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<p>Comparison between the experimental and calculated values (considering tortuosity in <a href="#sec3dot2-materials-15-07393" class="html-sec">Section 3.2</a> and tortuosity in Reference (Lee et al. 2009) [<a href="#B5-materials-15-07393" class="html-bibr">5</a>]) of the peak frequency and the sound absorption coefficient: (<b>a</b>) Hexagonal close-packed lattice (<span class="html-italic">d</span> = 4 mm); (<b>b</b>) Hexagonal close-packed lattice (<span class="html-italic">d</span> = 8 mm); (<b>c</b>) Face-centered cubic lattice (<span class="html-italic">d</span> = 4 mm); and (<b>d</b>) Face-centered cubic lattice (<span class="html-italic">d</span> = 8 mm).</p>
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17 pages, 5175 KiB  
Article
Experimental Investigations and Effect of Nano-Powder-Mixed EDM Variables on Performance Measures of Nitinol SMA
by Rakesh Chaudhari, Yug Shah, Sakshum Khanna, Vivek K. Patel, Jay Vora, Danil Yurievich Pimenov and Khaled Giasin
Materials 2022, 15(20), 7392; https://doi.org/10.3390/ma15207392 - 21 Oct 2022
Cited by 13 | Viewed by 1959
Abstract
In the present study, the effect of alumina (Al2O3) nano-powder was investigated for the electrical discharge machining (EDM) of a Nitinol shape memory alloy (SMA). In addition to the nano-powder concentration, other parameters of pulse-on-time (Ton), pulse-off-time [...] Read more.
In the present study, the effect of alumina (Al2O3) nano-powder was investigated for the electrical discharge machining (EDM) of a Nitinol shape memory alloy (SMA). In addition to the nano-powder concentration, other parameters of pulse-on-time (Ton), pulse-off-time (Toff), and current were selected for the performance measures of the material removal rate (MRR), surface roughness (SR), and tool wear rate (TWR) of Nitinol SMA. The significance of the design variables on all the output measures was analyzed through an analysis of variance (ANOVA). The regression model term has significantly impacted the developed model terms for all the selected measures. In the case of individual variables, Al2O3 powder concentration (PC), Toff, and Ton had significantly impacted MRR, TWR, and SR measures, respectively. The influence of EDM variables were studied through main effect plots. The teaching–learning-based optimization (TLBO) technique was implemented to find an optimal parametric setting for attaining the desired levels of all the performance measures. Pursuant to this, the optimal parametric settings of current at 24 A, PC at 4 g/L, Toff at 10 µs, and Ton of 4 µs have shown optimal input parameters of 43.57 mg/min for MRR, 6.478 mg/min for TWR, and 3.73 µm for SR. These results from the TLBO technique were validated by performing the experiments at the optimal parametric settings of the EDM process. By considering the different user and application requirements, 40 Pareto points with unique solutions were generated. Lastly, scanning electron microscopy (SEM) performed the machined surface analysis. The authors consider this to be very beneficial in the nano-powder-mixed EDM process for appropriate manufacturing operations. Full article
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<p>Enlarged view of the EDM experimental.</p>
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<p>Nine Machined specimens as per the Taguch’s DOE.</p>
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<p>Analysis of alumina nano-powder: (<b>a</b>) X-ray Diffraction spectra, (<b>b</b>) Raman profile, and (<b>c</b>,<b>d</b>) FESEM with EDX analysis.</p>
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<p>Normal probability plot for (<b>a</b>) MRR, (<b>b</b>) TWR, and (<b>c</b>) SR.</p>
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<p>Impact of EDM variables on MRR.</p>
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<p>Impact of EDM variables on TWR.</p>
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<p>Impact of EDM variables on SR.</p>
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<p>3D Pareto curve.</p>
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<p>Machined surfaces for conventional EDM (without PC) for (<b>a</b>) top zone, (<b>b</b>) bottom zone.</p>
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<p>Machined surface for PMEDM (with Al<sub>2</sub>O<sub>3</sub> PC of 4 g/L) for (<b>a</b>) top zone, (<b>b</b>) bottom zone.</p>
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15 pages, 3497 KiB  
Review
3D Printing Technology for Smart Clothing: A Topic Review
by Shuangqing Wu, Taotao Zeng, Zhenhua Liu, Guozhi Ma, Zhengyu Xiong, Lin Zuo and Zeyan Zhou
Materials 2022, 15(20), 7391; https://doi.org/10.3390/ma15207391 - 21 Oct 2022
Cited by 12 | Viewed by 6752
Abstract
Clothing is considered to be an important element of human social activities. With the increasing maturity of 3D printing technology, functional 3D printing technology can realize the perfect combination of clothing and electronic devices while helping smart clothing to achieve specific functions. Furthermore, [...] Read more.
Clothing is considered to be an important element of human social activities. With the increasing maturity of 3D printing technology, functional 3D printing technology can realize the perfect combination of clothing and electronic devices while helping smart clothing to achieve specific functions. Furthermore, the application of functional 3D printing technology in clothing not only provides people with the most comfortable and convenient wearing experience, but also completely subverts consumers’ perception of traditional clothing. This paper introduced the progress of the application of 3D printing from the aspect of traditional clothing and smart clothing through two mature 3D printing technologies normally used in the field of clothing, and summarized the challenges and prospects of 3D printing technology in the field of smart clothing. Finally, according to the analysis of the gap between 3D-printed clothing and traditionally made clothing due to the material limitations, this paper predicted that the rise in intelligent materials will provide a new prospect for the development of 3D-printed clothing. This paper will provide some references for the application research of 3D printing in the field of smart clothing. Full article
(This article belongs to the Special Issue Photoelectric Functional Materials and Devices)
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<p>Iris van Herpen’s 3D-printed clothing from 2010 (<b>a</b>) and 2011 (<b>b</b>) in high-definition series [<a href="#B24-materials-15-07391" class="html-bibr">24</a>].</p>
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<p>The Radiate sports T-shirt with various colors [<a href="#B67-materials-15-07391" class="html-bibr">67</a>].</p>
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<p>(<b>a</b>) An integrated biosensor in the exercise shirt. (<b>b</b>) The smart T-shirt with a built-in sensor [<a href="#B68-materials-15-07391" class="html-bibr">68</a>,<a href="#B69-materials-15-07391" class="html-bibr">69</a>].</p>
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<p>(<b>a</b>) A mechanical glove, Robo-Glove, with pressure sensors and other sensors jointly developed by General Motors and NASA. (<b>b</b>) The back and details of the mechanical glove [<a href="#B69-materials-15-07391" class="html-bibr">69</a>].</p>
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<p>(<b>a</b>) The 3D printing of heat-adjusted textiles; (<b>b</b>) 3D printing of multifunctional, flexible phase-change nonwovens; (<b>c</b>) flexible grids which speed up finger recovery when clenching fists; (<b>d</b>) spaced hexagonal grids for fall-protective clothing [<a href="#B72-materials-15-07391" class="html-bibr">72</a>,<a href="#B73-materials-15-07391" class="html-bibr">73</a>,<a href="#B74-materials-15-07391" class="html-bibr">74</a>,<a href="#B75-materials-15-07391" class="html-bibr">75</a>,<a href="#B76-materials-15-07391" class="html-bibr">76</a>].</p>
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<p>(<b>a</b>) Application of the 3D-Printed E-Textile for Energy Management (<b>A</b>) Schematic illustration showing smart clothes for energy management and its performance. Inset (<b>i</b>) the output <span class="html-italic">I</span><sub>sc</sub> density of a smart gridline pattern printed on the underarm sleeve of a shirt generated by an arm moving. Inset (<b>ii</b>) the rectifying circuit diagram of the power system. Inset (<b>iii</b>) the rectified output <span class="html-italic">I</span><sub>sc</sub> density of the smart pattern; (<b>B</b>) Charging curves of a capacitor (3.3 μF) charged using the smart pattern displaced at different speeds; (<b>C</b>) Charging curves of different capacitances charged using the smart pattern with a displacement speed of 13 cm/s; (<b>D</b>) Photographs showing (<b>i</b>) LEDs and (<b>ii</b>) an electrical watch driven by the power generated by the 3D-printed E-textile. (<b>b</b>) stretchable elastic fibers for tactile sensor of electronic skin. Inset (<b>i</b>) original, (<b>ii</b>) Stretching. [<a href="#B84-materials-15-07391" class="html-bibr">84</a>,<a href="#B85-materials-15-07391" class="html-bibr">85</a>].</p>
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<p>Design and development of a wearable exoskeleton system for stroke rehabilitation. (<b>a</b>) and (<b>b</b>) are schematics of the exoskeleton; (<b>c</b>) schematic of simulated finger joint movement arc; (<b>d</b>) actual movements of each finger joint [<a href="#B93-materials-15-07391" class="html-bibr">93</a>].</p>
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<p>Hand rehabilitation exoskeleton. (<b>a</b>) Main concept of the hybrid model for wrist orthosis. (<b>b</b>) Combination of the upper cover and inner frame. (<b>c</b>) Wearing the new cast [<a href="#B94-materials-15-07391" class="html-bibr">94</a>].</p>
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<p>The process of designing and manufacturing gradient structure insole. (<b>a</b>) Different porous units to assembled (<b>b</b>) Porous substrate (<b>c</b>) Boolean intersection of the porous substrate and the original insole (<b>d</b>) The complete customized porous insole model (<b>e</b>) Manufactured porous customized flat insole and full contact insole (<b>f</b>) The printing machine and the 3D-printed testing samples [<a href="#B95-materials-15-07391" class="html-bibr">95</a>].</p>
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19 pages, 7560 KiB  
Article
Intermediate Crack Debonding of Externally Bonded FRP Reinforcement—Comparison of Methods
by Paweł Tworzewski, Jeffrey K. Alexy and Robert W. Barnes
Materials 2022, 15(20), 7390; https://doi.org/10.3390/ma15207390 - 21 Oct 2022
Cited by 4 | Viewed by 1616
Abstract
Many researchers around the world have made extensive efforts to study the phenomenon of fiber-reinforced polymer (FRP) debonding. Based on these efforts, code provisions and various models have been proposed for predicting intermediate crack (IC) debonding failure. The paper presents a comparison of [...] Read more.
Many researchers around the world have made extensive efforts to study the phenomenon of fiber-reinforced polymer (FRP) debonding. Based on these efforts, code provisions and various models have been proposed for predicting intermediate crack (IC) debonding failure. The paper presents a comparison of seven selected models: fib bulletin 14 approach, Teng et al. model, Lu model, Seracino et al. model, Said and Wu model, Elsanadedy et al. model and ACI 440. The accuracy of each model was evaluated based on the test results of 58 flexural specimens with IC debonding failures of externally bonded (EB), carbon FRP plates or sheets found in the existing literature. The experimental database was prepared to include a wide range of parameters affecting the issue under consideration. A comparison of the measured and predicted load capacity values was made to evaluate the prediction accuracy of the considered models. The analysis included the limitation of the load capacity estimated based on IC debonding models as well as concrete crushing and FRP rupture types of failure. The results indicate that the latest models proposed for direct implementation in design guidelines—the Said and Wu model and the Elsanadedy et al. model—offer the best accuracy in predicting the load capacity. In contrast, the fib bulletin 14 approach shows a wide dispersion of predictions and a large proportion of highly overestimated results. Full article
(This article belongs to the Special Issue Advanced Composite Materials: Theory, Design and Applications)
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<p>Intermediate crack (IC) [<a href="#B10-materials-15-07390" class="html-bibr">10</a>].</p>
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<p>Localized debonding of FRP reinforcement in maximum moment region [<a href="#B11-materials-15-07390" class="html-bibr">11</a>].</p>
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<p>Idealized failure plane [<a href="#B18-materials-15-07390" class="html-bibr">18</a>].</p>
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<p>Measured flexural strength versus <span class="html-italic">fib</span> bulletin 14 prediction.</p>
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<p>Measured flexural strength versus Teng et al. model prediction.</p>
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<p>Measured flexural strength versus Lu model prediction.</p>
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<p>Measured flexural strength versus Seracino et al. model prediction.</p>
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<p>Measured flexural strength versus Said and Wu model prediction.</p>
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<p>Measured flexural strength versus Elsanadedy et al. model prediction.</p>
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<p>Measured flexural strength versus ACI 440 prediction.</p>
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<p>Comparison of deviation of predicted results—box plots.</p>
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<p>Measured increase in flexural strength versus <span class="html-italic">fib</span> bulletin 14 prediction.</p>
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<p>Measured increase in flexural strength versus Teng et al. model prediction.</p>
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<p>Measured increase in flexural strength versus Lu model prediction.</p>
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<p>Measured increase in flexural strength versus Seracino et al. model prediction.</p>
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<p>Measured increase in flexural strength versus Said and Wu model prediction.</p>
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<p>Measured increase in flexural strength versus Elsanadedy et al. model prediction.</p>
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<p>Measured increase in flexural strength versus ACI 440 prediction.</p>
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<p>Comparison of predicted increase in flexural strength—box plots.</p>
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17 pages, 6110 KiB  
Article
Calorimetric Method for the Testing of Thermal Coefficients of the TIG Process
by Marek Mróz, Antoni Władysław Orłowicz, Magdalena Lenik, Andrzej Trytek and Mirosław Tupaj
Materials 2022, 15(20), 7389; https://doi.org/10.3390/ma15207389 - 21 Oct 2022
Viewed by 1306
Abstract
This paper presents an original design of a test apparatus for calorimetric measurements of arc efficiency η and melting efficiency ηm in welding processes. The construction and principle of operation of a new flow calorimeter are described, as well as the method [...] Read more.
This paper presents an original design of a test apparatus for calorimetric measurements of arc efficiency η and melting efficiency ηm in welding processes. The construction and principle of operation of a new flow calorimeter are described, as well as the method for determining the η and ηm values in the process of the surface melting of aluminium–silicon alloy casting surfaces with a concentrated heat flux generated by the TIG (Tungsten Inert Gas) method. The results obtained indicate the advisability of using calorimetric testing to assess the arc efficiency of welding processes. It was demonstrated that changing the welding current and arc scanning speed, as well as changing the chemical composition of the silumin, has an effect on the arc efficiency value η. This has the effect of introducing a different amount of heat into the area of the heated material. The consequence of this is a change in the value of the melting efficiency ηm, which results in a change in the width and depth of the surface melting areas, through this, the cooling conditions of the material. As is well known, this will affect the microstructure of the welds and the width and microstructure of the heat-affected zone, and thus the performance of the welded joints. Full article
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<p>Energy distribution in the TIG process: Q, total heat generated in the electric arc Q<sub>arc</sub> and on the electrode Q<sub>e</sub>; Q<sub>o</sub>, amount of heat transferred to the surrounding area; Q<sub>c</sub>, amount of heat required to heat and partially melt the material and then overheat the liquid metal; Q<sub>r</sub> + Q<sub>c</sub> is that part of the heat absorbed by the heated element; Q<sub>r</sub>, amount of heat transferred by conduction to the parent material.</p>
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<p>Havaldas’s calorimeter [<a href="#B18-materials-15-07389" class="html-bibr">18</a>].</p>
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<p>The Seebeck calorimeter [<a href="#B8-materials-15-07389" class="html-bibr">8</a>].</p>
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<p>Flow calorimeter diagram; 1, gasket; 2, thermocouple tip sliding contacts; 3, thermocouple; 4, flow meter [<a href="#B19-materials-15-07389" class="html-bibr">19</a>].</p>
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<p>Structural design of the flow calorimeter; 1, water; 2, flow chamber; 3, top edge of the chamber; 4, gasket; 5, superficially melted sample; 6, partitions; 7, water inlet pipe; 8, flow rotameter; 9, water drainage pipe; 10, 11, thermocouples; 12, tungsten electrode; 13, positive pole; 14, power source; 15, negative pole; 16, holder with protective gas; 17, temperature recording [<a href="#B23-materials-15-07389" class="html-bibr">23</a>].</p>
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<p>Diagram of the flow calorimeter test system.</p>
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<p>Calorimetric test bench; 1-TIG welding machine, 2—welding torch with tungsten electrode, 3—flow calorimeter with sample, 4—temperature recorder.</p>
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<p>Effect of welding current and scanning speed of TIG arc welding in an argon atmosphere on melting efficiency in calorimetric testing of AK 51 (<b>a</b>) and AK 20 (<b>b</b>) alloys samples.</p>
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<p>Effect of welding current and arc scanning speed values using the TIG method in an argon atmosphere on the volume of 200 mm long surface melting obtained from calorimetric measurements of AK 51 (<b>a</b>) and AK 20 (<b>b</b>) alloys samples.</p>
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<p>Microstructure of the AK 51 alloy in the surface melting area (top—area A) and in the native material area (bottom—area B). In the surface melting area, there is eutectic α(Al) + β(Si) and very fine dendrites of the α(Al) phase. Etch with Dix and Keith reagent.</p>
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<p>Microstructure of AK 51 alloy surface melting using the TIG method in an argon atmosphere at a welding current of I = 150 A and a scanning speed of vs. = 800 mm/min. A is the area in <a href="#materials-15-07389-f010" class="html-fig">Figure 10</a>. An eutectic characterised by a distance between lamellae and silica fibres λ<sub>E</sub> of less than 1 µm. Etch with Dix and Keith reagent.</p>
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<p>Microstructure of the AK 51 alloy in the native material area. B is the area in <a href="#materials-15-07389-f010" class="html-fig">Figure 10</a>. Visible lamellar and fibrous eutectics with the value of the parameter λ<sub>E</sub> on the order of a few micrometers and the dendrites of α(Al) phase. Etch with Dix and Keith reagent.</p>
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<p>Microstructure of the AK 20 alloy in the surface melting area (top—area A) and in the native material area (bottom—area B). In the surface melting area, there is a eutectic, undissolved primary silicon crystals and very fine dendrites of the α(Al) phase at the super-melting boundary and around the primary silicon crystals. Etch with Dix and Keith reagent.</p>
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<p>Microstructure of AK 20 alloy surface melting using the TIG method in an argon atmosphere at a welding current of I = 150 A and a scanning speed of vs. = 800 mm/min. A is the area in <a href="#materials-15-07389-f010" class="html-fig">Figure 10</a>. An eutectic characterised by a distance between lamellae and silica fibres λ<sub>E</sub> of less than 1 µm. Etch with Dix and Keith reagent.</p>
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<p>Microstructure of the AK 20 alloy in the native material area. B is the area in <a href="#materials-15-07389-f010" class="html-fig">Figure 10</a>. A visible lamellar and fibrous eutectic with an λ<sub>E</sub>-value of a few micrometres and a primary silicon crystal (top). Etch with Dix and Keith reagent.</p>
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27 pages, 6863 KiB  
Article
An Analytical and Experimental Study on Cutting Characteristics and Transient Cutting Force Modeling in Feed Directional Ultrasonic Vibration-Assisted Cutting of High Strength Alloys
by Xuelin Chen, Jinyuan Tang, Wen Shao, Bo Hu and Jinxiang Ye
Materials 2022, 15(20), 7388; https://doi.org/10.3390/ma15207388 - 21 Oct 2022
Cited by 5 | Viewed by 1978
Abstract
Ultrasonic vibration-assisted cutting (UVC) is progressively being used in machining as it can significantly promote the fabrication process. However, the ultrasonic vibration affecting the cutting process is still controversial. The full-transient cutting process is proposed in this study to analyze the affecting mechanism [...] Read more.
Ultrasonic vibration-assisted cutting (UVC) is progressively being used in machining as it can significantly promote the fabrication process. However, the ultrasonic vibration affecting the cutting process is still controversial. The full-transient cutting process is proposed in this study to analyze the affecting mechanism induced by ultrasonic vibration in the cutting process. This novel model is the first developed based on the fact that ultrasonic vibration would change mechanical behaviors and the cutting process. For example, the reduction of shear flowing stress in the primary shear zone and alteration of the shear angle in the UVC process. Then, considering those coupled effects, a novel model is proposed to determine the average and transient cutting forces. Here, insight and understanding into the physical phenomenon in UVC are provided. The effectiveness of the proposed model is verified by comparison with experimental results and analytical models available in the literature, with cutting parameters varying from macro to micro-scale. The results show that the ultrasonic vibration affects the cutting process in a complicated way, which is determined by transient characteristics, acoustic softening, thermal softening, plowing, and friction. Those effects on cutting performances in the UVC process under various cutting scenarios are investigated and discussed systematically. The average deviation of cutting forces between experiments and values predicted by the proposed model for Ti6Al4V, AISI 1045, and Al6063 is about 7%, 10.2%, and 11%, respectively. The deviation decreases with the increase of cutting speed in the machining of Ti6Al4V, which is different from the machining of other materials. This is contributed by the varied effect of ultrasonic vibration on the cutting process. Full article
(This article belongs to the Special Issue The Advanced Manufacturing Technologies of Metal Gears)
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<p>Illustration of the acoustic vibration-assisted turning.</p>
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<p>Principles of acoustic vibration-assisted cutting.</p>
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<p>Diagram of cutting speed in orthogonal UVC.</p>
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<p>The coordinate relationship between synthetic cutting speed and traditional cutting speed.</p>
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<p>The relationship of cutting force in two coordinate systems.</p>
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<p>The relationship of cutting in and out in UVA machining.</p>
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<p>The assembled apparatus (<b>a</b>) without protective shell, (<b>b</b>) with protective shell, and (<b>c</b>) its testing experiments.</p>
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<p>The testing origin data of ultrasonic vibration apparatus.</p>
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<p>The variation of ultrasonic amplitude with power for ultrasonic vibration apparatus.</p>
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<p>Presentation of the experiment by: (<b>a</b>) schematic and (<b>b</b>) experimental setup.</p>
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<p>The typical work-piece (<b>a</b>) and cutting forces (<b>b</b>) in cutting with and without ultrasonic vibration.</p>
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<p>Comparison between the predicted and experimental cutting forces with ultrasonic amplitude of 14.75 um and cutting depth of 0.3 mm: (<b>a</b>) Fx, (<b>b</b>) Fy, (<b>c</b>) Fz, and (<b>d</b>) Fc.</p>
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<p>Comparison between the predicted and experimental cutting forces with ultrasonic amplitude of 14.75 um and cutting depth of 0.3 mm: (<b>a</b>) Fx, (<b>b</b>) Fy, (<b>c</b>) Fz, and (<b>d</b>) Fc.</p>
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<p>The evolution of shear angle in chip formation process (h = 0.005 mm, hv = 8 um, n = 652 r/min, <math display="inline"><semantics> <mi>θ</mi> </semantics></math> = 36°, <span class="html-italic">D<sub>r</sub></span> = 12 mm).</p>
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<p>The shear is flowing stress in ultrasonic vibration-assisted orthogonal cutting.</p>
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<p>The shear is flowing stress with an increase of amplitude in UVC.</p>
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<p>The shear flowing stress with increase of feed rate in UVC.</p>
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<p>The predicted and experimental transient cutting force in the feed direction.</p>
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<p>The comparison of predicted and experimental averaged cutting forces with the increase of feed rate (cutting depth: 0.6 mm, Amplitude: 12 um, RPM: 1875).</p>
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<p>The comparison of predicted and experimental averaged cutting forces with the increased cutting depth (Feed rate: 50 mm/min, Amplitude: 12 um, RPM: 1875).</p>
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<p>The comparison of predicted and experimental averaged cutting forces with increased cutting velocity (Feed rate: 50 mm/min, Cutting depth: 0.6 mm, Amplitude: 12 um).</p>
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<p>The comparison of predicted and experimental averaged cutting force with the increase of ultrasonic vibration amplitude (Feed rate: 50 mm/min, Cutting depth: 0.6 mm, RPM: 1875).</p>
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15 pages, 5693 KiB  
Article
Numerical Study of the Mechanical Behaviour of Wedge-Shaped Defect Filling Materials
by Lyaysan Sakhabutdinova, Anna A. Kamenskikh, Alex G. Kuchumov, Yuriy Nosov and Inessa Baradina
Materials 2022, 15(20), 7387; https://doi.org/10.3390/ma15207387 - 21 Oct 2022
Cited by 2 | Viewed by 2095
Abstract
This paper deals with direct restorations of teeth with non-carious cervical lesions (NCCL). NCCL defects are capable of gradual growth and are accompanied by the degradation of the surrounding tissue. Direct restorative treatment, in which the cavity is filled with a cementing agent, [...] Read more.
This paper deals with direct restorations of teeth with non-carious cervical lesions (NCCL). NCCL defects are capable of gradual growth and are accompanied by the degradation of the surrounding tissue. Direct restorative treatment, in which the cavity is filled with a cementing agent, is considered to be an accessible and common treatment option. The study included simulations of the teeth without lesions, the teeth with V and U lesions and the tooth-restorative system. Parameterised numerical tooth models were constructed. Two cases with defect depths of 0.8 mm and ~1.7 mm and three variants with fillet radii of the defect end of 0.1, 0.2 and 0.3 mm were considered. The effect of two biomaterials for restorations was studied, namely Herculite XRV (Kerr Corp, Orange, CA, USA) and Charisma (Heraeus Kulzer GmbH, Hanau, Germany). The models were deformed with a vertical load of 100 to 1000 N from the antagonist tooth. The tooth-restorative system was considered, taking into consideration the contact interaction in the interface areas with the tooth tissues. Within the limits of the research, the character of the distribution of the deformation characteristics and their dependence on the level of loading, the depth of the defect and the radius of the curvature of the “wedge” were established. Full article
(This article belongs to the Special Issue Applications of Dental Biomaterials)
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<p>Mid-section of a tooth with a wedge-shaped defect.</p>
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<p>FE model: (<b>a</b>) 3D cross-section, and the (<b>b</b>) section with boundary conditions.</p>
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<p>Dependence of maximum stress intensity values of the biomechanical unit on load: (<b>a</b>) enamel; (<b>b</b>) dentin; black—model without defect; red—model with 0.1 mm defect fillet; blue—model with 0.2 mm defect fillet; green—model with 0.3 mm defect fillet.</p>
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<p>Dependence of maximum strain intensity values of the biomechanical unit on load: (<b>a</b>) enamel; (<b>b</b>) dentin; black—model without defect; red—model with 0.1 mm defect fillet; blue—model with 0.2 mm defect fillet; green—model with 0.3 mm defect fillet.</p>
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<p>Maximum stress intensity of a biomechanical unit as a function of load: (<b>a</b>) enamel; (<b>b</b>) dentine; dashed line—model with filling material 1; solid line—model with filling material 2; blue—model with 0.1 mm fillet; red—model with 0.2 mm fillet; black—model with 0.3 mm fillet.</p>
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<p>Maximum strain intensity of a biomechanical unit as a function of load: (<b>a</b>) enamel; (<b>b</b>) dentine; dashed line—model with filling material 1; solid line—model with filling material 2; blue—model with 0.1 mm fillet; red—model with 0.2 mm fillet; black—model with 0.3 mm fillet.</p>
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<p>Dependence of the maximum stress intensity of the biomechanical unit on the fillet radius of a shallow wedge-shaped defect: (<b>a</b>) enamel; (<b>b</b>) dentin.</p>
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<p>Dependence of the maximum strain intensity of the biomechanical unit on the fillet radius of a shallow wedge-shaped defect: (<b>a</b>) enamel; (<b>b</b>) dentin.</p>
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<p>Comparison of biomechanical stress intensities of a shallow and deep wedge defect: (<b>a</b>) enamel; (<b>b</b>) dentin; solid line—model with filling material 1; dotted line—model with filling material 2; black—model with 0.1 mm rounded defect, blue—model with 0.2 mm rounded defect, brown—model with 0.3 mm rounded defect.</p>
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<p>Comparison of the deformation intensities of the biomechanical unit of a deep versus shallow wedge defect: (<b>a</b>) enamel; (<b>b</b>) dentin; solid line—model with filling material 1, dashed line—model with filling material 2; black—model with 0.1 mm fillet, blue—model with 0.2 mm fillet, brown—model with 0.3 mm fillet.</p>
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32 pages, 15559 KiB  
Article
High-Temperature Mechanical Properties of Stress-Relieved AlSi10Mg Produced via Laser Powder Bed Fusion Additive Manufacturing
by Dirk Lehmhus, Thomas Rahn, Adrian Struss, Phillip Gromzig, Tim Wischeropp and Holger Becker
Materials 2022, 15(20), 7386; https://doi.org/10.3390/ma15207386 - 21 Oct 2022
Cited by 11 | Viewed by 3143
Abstract
The present study is dedicated to the evaluation of the mechanical properties of an additively manufactured (AM) aluminum alloy and their dependence on temperature and build orientation. Tensile test samples were produced from a standard AlSi10Mg alloy by means of the Laser Powder [...] Read more.
The present study is dedicated to the evaluation of the mechanical properties of an additively manufactured (AM) aluminum alloy and their dependence on temperature and build orientation. Tensile test samples were produced from a standard AlSi10Mg alloy by means of the Laser Powder Bed Fusion (LPBF) or Laser Beam Melting (LBM) process at polar angles of 0°, 45° and 90°. Prior to testing, samples were stress-relieved on the build platform for 2 h at 350 °C. Tensile tests were performed at four temperature levels (room temperature (RT), 125, 250 and 450 °C). Results are compared to previously published data on AM materials with and without comparable heat treatment. To foster a deeper understanding of the obtained results, fracture surfaces were analyzed, and metallographic sections were prepared for microstructural evaluation and for additional hardness measurements. The study confirms the expected significant reduction of strength at elevated temperatures and specifically above 250 °C: Ultimate tensile strength (UTS) was found to be 280.2 MPa at RT, 162.8 MPa at 250 °C and 34.4 MPa at 450 °C for a polar angle of 0°. In parallel, elongation at failure increased from 6.4% via 15.6% to 26.5%. The influence of building orientation is clearly dominated by the temperature effect, with UTS values at RT for polar angles of 0° (vertical), 45° and 90° (horizontal) reaching 280.2, 272.0 and 265.9 MPa, respectively, which corresponds to a 5.1% deviation. The comparatively low room temperature strength of roughly 280 MPa is associated with stress relieving and agrees well with data from the literature. However, the complete breakdown of the cellular microstructure reported in other studies for treatments at similar or slightly lower temperatures is not fully confirmed by the metallographic investigations. The data provide a basis for the prediction of AM component response under the thermal and mechanical loads associated with high-pressure die casting (HPDC) and thus facilitate optimizing HPDC-based compound casting processes involving AM inserts. Full article
(This article belongs to the Special Issue Additive Manufacturing Methods and Modeling Approaches (Volume II))
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<p>Overview of room temperature properties of AlSi10Mg produced via the LPBF process as reported in the scientific literature [<a href="#B16-materials-15-07386" class="html-bibr">16</a>,<a href="#B18-materials-15-07386" class="html-bibr">18</a>,<a href="#B21-materials-15-07386" class="html-bibr">21</a>,<a href="#B22-materials-15-07386" class="html-bibr">22</a>,<a href="#B26-materials-15-07386" class="html-bibr">26</a>,<a href="#B27-materials-15-07386" class="html-bibr">27</a>,<a href="#B28-materials-15-07386" class="html-bibr">28</a>,<a href="#B29-materials-15-07386" class="html-bibr">29</a>,<a href="#B30-materials-15-07386" class="html-bibr">30</a>,<a href="#B31-materials-15-07386" class="html-bibr">31</a>,<a href="#B32-materials-15-07386" class="html-bibr">32</a>,<a href="#B33-materials-15-07386" class="html-bibr">33</a>,<a href="#B34-materials-15-07386" class="html-bibr">34</a>,<a href="#B35-materials-15-07386" class="html-bibr">35</a>,<a href="#B36-materials-15-07386" class="html-bibr">36</a>,<a href="#B37-materials-15-07386" class="html-bibr">37</a>,<a href="#B38-materials-15-07386" class="html-bibr">38</a>,<a href="#B39-materials-15-07386" class="html-bibr">39</a>]: (<b>a</b>) ultimate tensile strength (UTS) plotted vs. yield strength (YS), and (<b>b</b>) elongation at failure plotted vs. UTS. The data cover different printing directions, process parameters and heat treatment states, namely as-built (AB), stress-relieved (SR), solution heat-treated (SHT) and warm-aged (WA), plus combinations of these. The individual values are presented in <a href="#materials-15-07386-t0A1" class="html-table">Table A1</a> in <a href="#app1-materials-15-07386" class="html-app">Appendix A</a> together with a brief explanation of the respective boundary conditions.</p>
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<p>Samples’ dimensions according to DIN 50125:2016-12 and explanation of the build orientation [<a href="#B44-materials-15-07386" class="html-bibr">44</a>]. Note that in the sketches to the left, the <span class="html-italic">z</span>-axis is the vertical direction, while the <span class="html-italic">x</span>-axis is the re-coating direction in the present experiment and the plane of the build platform is spanned by the <span class="html-italic">x</span>- and <span class="html-italic">y</span>-axes together. Θ is the polar and φ is the azimuth angle.</p>
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<p>Test setup for high-temperature tensile tests showing sample position and furnace as well as the extensometer used for the experiments. (<b>Left</b>) Overview including part of the Zwick Roell Z250 test device, and (<b>right</b>) detailed view of the extensometer and sample.</p>
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<p>Representative engineering stress vs. strain curves for different build orientations and test temperatures: (<b>a</b>) room temperature data, (<b>b</b>) test temperature 125 °C, (<b>c</b>) test temperature 250 °C and (<b>d</b>) test temperature 450 °C. Note that <span class="html-italic">x</span>- and <span class="html-italic">y</span>-axis scaling are identical in all cases to allow for direct comparison of the diagrams.</p>
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<p>Overview of results of tensile tests performed at room temperature (RT), 125, 250 and 450 °C for three different build orientations, namely polar angles of 0°, 45° and 90°: (<b>a</b>) yield strength, (<b>b</b>) ultimate tensile strength and (<b>c</b>) elongation at failure.</p>
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<p>Macroscopic images of unetched metallographic sections of tensile test samples of polar angle 0° tested at increasing temperatures: (<b>a</b>) RT, (<b>b</b>) 125, (<b>c</b>) 250 and (<b>d</b>) 450 °C. The images provide an impression of the level of porosity as well as highlighting the necking, which increases with the increasing test temperature from (<b>a</b>–<b>d</b>). The sample tested at 450 °C also showed evidence of pore growth in the plastic region adjacent to the fracture location.</p>
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<p>Macroscopic images of metallographic sections of tensile test samples produced at a polar angle of 0° and tested at increasing temperatures, after grain boundary etching using MIL etchant: (<b>a</b>) RT, (<b>b</b>) 125, (<b>c</b>) 250 and (<b>d</b>) 450 °C. Figures show increasing levels of necking parallel to the increasing test temperature. Etching highlights the orientation of the individual layers, perpendicular to the direction of force in this case, as well as the boundary layer.</p>
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<p>Region of fracture of a sample of polar angle 0° tested at room temperature: (<b>a</b>,<b>b</b>) metallographic section of etched samples at different magnifications, (<b>c</b>,<b>d</b>) back-scattered electron (BSE) images of the fracture surface at different magnifications and (<b>e</b>,<b>f</b>) secondary electron (SE) images of the fracture surface, overview and detailed view. Note that the red box in the image on the left highlights the area depicted in the magnified view on the right.</p>
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<p>Region of fracture of a sample of polar angle 0° tested at 125 °C: (<b>a</b>,<b>b</b>) metallographic section of etched samples at different magnifications, (<b>c</b>,<b>d</b>) back-scattered electron (BSE) images of the fracture surface at different magnifications and (<b>e</b>,<b>f</b>) secondary electron (SE) images of the fracture surface, overview and detailed view. Note that the red box in the image on the left highlights the area depicted in the magnified view on the right.</p>
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<p>Region of fracture of a sample of polar angle 0° tested at 250 °C: (<b>a</b>,<b>b</b>) metallographic section of etched samples at different magnifications, (<b>c</b>,<b>d</b>) back-scattered electron (BSE) images of the fracture surface at different magnifications and (<b>e</b>,<b>f</b>) secondary electron (SE) images of the fracture surface, overview and detailed view. Note that the red box in the image on the left highlights the area depicted in the magnified view on the right.</p>
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<p>Region of fracture of a sample of polar angle 0° tested at 450 °C: (<b>a</b>,<b>b</b>) metallographic section of etched samples at different magnifications, (<b>c</b>,<b>d</b>) back-scattered electron (BSE) images of the fracture surface at different magnifications and (<b>e</b>,<b>f</b>) secondary electron (SE) images of the fracture surface, overview and detailed view. Note that the red box in the image on the left highlights the area depicted in the magnified view on the right.</p>
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<p>Metallographic sections of etched samples produced at varied polar angles after tensile testing at 250 °C. Left, general overview, right, detailed view of the fracture zone: (<b>a</b>,<b>b</b>) polar angle 0°, (<b>c</b>,<b>d</b>) polar angle 45 ° and (<b>e</b>,<b>f</b>) polar angle 90°.</p>
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<p>Fracture surfaces of samples produced at varied polar angles after tensile testing at 250 °C. Left column, low magnification overview, right, increased magnification: (<b>a</b>,<b>b</b>) polar angle 0°, (<b>c</b>,<b>d</b>) polar angle 45 ° and (<b>e</b>,<b>f</b>) polar angle 90°. Readers should note that the images in <a href="#materials-15-07386-f011" class="html-fig">Figure 11</a>a,b have already been shown as <a href="#materials-15-07386-f008" class="html-fig">Figure 8</a>c,d and are repeated here for direct comparison with their counterparts with polar angles 45° and 90°. Figures highlight the differences in failure locations relative to melt pool features also visible in the metallographic sections in <a href="#materials-15-07386-f012" class="html-fig">Figure 12</a>, specifically when comparing <a href="#materials-15-07386-f013" class="html-fig">Figure 13</a>a,b to <a href="#materials-15-07386-f013" class="html-fig">Figure 13</a>c–f. Note that the red box in the image on the left highlights the area depicted in the magnified view on the right.</p>
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<p>Microstructure of: (<b>a</b>,<b>b</b>) microstructure (<b>a</b>) and EDX area scan (<b>b</b>) for a sample produced at a 0° polar angle and tested at room temperature, and (<b>c</b>,<b>d</b>) microstructure (<b>c</b>) and EDX area scan (<b>d</b>) for a sample produced at a 0° polar angle and tested at 450 °C. Image is contrast-enhanced by 30% using the MS Word image formatting feature to increase material contrast in (<b>a</b>,<b>c</b>). Identification of bright-grey phases with silicon is confirmed. Images (<b>c</b>,<b>d</b>) confirm dissolution of the cellular structure as well as growth of the silicon phase.</p>
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<p>Microhardness measured near the fracture surface and in the sample core for specimens of polar angle 0° tested at room temperature (RT), 125, 250 and 450 °C. Note that the hardness measurements themselves were performed at room temperature.</p>
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<p>Microstructure of a sample printed at a 0° polar angle and cut in the <span class="html-italic">xz</span> plane assuming laser scanning in <span class="html-italic">y</span>-direction. The difference in comparison to the micrograph is due to the fact that for one thing the schematic representation does not account for the 60° layer-to-layer shift of the scanning direction, and besides the orientation of the micrograph is at an arbitrary angle to the scanning direction(s). The sketch to the left depicts the main microstructural zones based on the designation by Santos Macias et al. [<a href="#B43-materials-15-07386" class="html-bibr">43</a>].</p>
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12 pages, 2369 KiB  
Article
Using Physical Modeling to Optimize the Aluminium Refining Process
by Tomáš Prášil, Ladislav Socha, Karel Gryc, Jana Svizelová, Mariola Saternus, Tomasz Merder, Jacek Pieprzyca and Martin Gráf
Materials 2022, 15(20), 7385; https://doi.org/10.3390/ma15207385 - 21 Oct 2022
Cited by 4 | Viewed by 1574
Abstract
Concern for the environment and rational management of resources requires the development of recoverable methods of obtaining metallic materials. This also applies to the production of aluminium and its alloys. The quality requirements of the market drive aluminium producers to use effective refining [...] Read more.
Concern for the environment and rational management of resources requires the development of recoverable methods of obtaining metallic materials. This also applies to the production of aluminium and its alloys. The quality requirements of the market drive aluminium producers to use effective refining methods, and one of the most commonly used is blowing an inert gas into liquid aluminium via a rotating impeller. The efficiency and cost of this treatment depends largely on the application of the correct ratios between the basic parameters of the process, which are the flow rate of the inert gas, the speed of the rotor and the duration of the process. Determining these ratios in production conditions is expensive and difficult. This article presents the results of research aimed at determining the optimal ratio of the inert gas flow rate to the rotary impeller speed, using physical modeling techniques for the rotor as used in industrial conditions. The tests were carried out for rotary impeller speeds from 150 to 550 rpm and gas flow rates of 12, 17 and 22 dm3/min. The research was carried out on a 1:1 scale physical model, and the results, in the form of visualization of the degree of gas-bubble dispersion, were assessed on the basis of the five typical dispersion patterns. The removal of oxygen from water was carried out analogously to the process of removing hydrogen from aluminium. The curves of the rate of oxygen removal from the model liquid were determined, showing the course of oxygen reduction during refining with the same inert gas flows and rotor speeds mentioned above. Full article
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<p>Schematic diagram of the FDU physical (water) model.</p>
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<p>Basic dimensional data (m) of the physical model and individual components: (<b>a</b>) front view, (<b>b</b>) side view.</p>
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<p>A 3D view of the rotor (impeller).</p>
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<p>Demonstration of the nature of internal flow, behavior and distribution of emerging bubbles of blown argon.</p>
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<p>Typical types of inert gas dispersion in liquid aluminium formed during the refining operation: (<b>a</b>) no dispersion (geyser and single bubbles creation), (<b>b</b>) minimal dispersion, (<b>c</b>) fine dispersion, (<b>d</b>) uniform dispersion, (<b>e</b>) excessive dispersion (chain flow and swirls).</p>
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<p>Characteristic features of excessive dispersion (creation of swirls in yellow and dead zones–no dispersion in green) for different variants of experiments: (<b>a</b>) 550 rpm, 12 dm<sup>3</sup>·min<sup>−1</sup> (<b>b</b>) 550 rpm, 17 dm<sup>3</sup>·min<sup>−1</sup>.</p>
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<p>Demonstration of concentration curves measured on a physical model. Gas flow rate: (<b>a</b>) 12 dm<sup>3</sup>·min<sup>−1</sup>, (<b>b</b>) 17 dm<sup>3</sup>·min<sup>−1</sup>, (<b>c</b>) 22 dm<sup>3</sup>·min<sup>−1</sup>.</p>
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<p>The minimum times of oxygen removal from the model liquid to the content of 1 ppm.</p>
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17 pages, 3760 KiB  
Article
Preparation and Application of Foaming Agent Based on the Compound System of Short-Chain Fluorocarbon and Soybean Residue Protein
by Ning Song, Zhihe Li, Shaoqing Wang and Yuanliang Xiong
Materials 2022, 15(20), 7384; https://doi.org/10.3390/ma15207384 - 21 Oct 2022
Cited by 5 | Viewed by 1880
Abstract
This study provides a new idea for the design of an advanced foaming agent with soybean residue protein (SRP) as a potential protein source. In order to achieve the most effective foaming performance, we employed the novel approach of response surface methodology (RSM) [...] Read more.
This study provides a new idea for the design of an advanced foaming agent with soybean residue protein (SRP) as a potential protein source. In order to achieve the most effective foaming performance, we employed the novel approach of response surface methodology (RSM) to improve important process parameters in a hot-alkali experiment. The experimental results showed that the optimum reaction parameters of pH and temperature were pH 10.2 and 50.5 °C, respectively, which, when continued for 3 h, led to the highest foaming property of the SRP foaming agent (486 mL). Based on the scheme, we also designed an experiment whereby we incorporated 1.0g/L FS-50 into the SRP foaming agent (SRP-50) to achieve higher foaming capacity compared with the commercial foaming agent. This foaming agent was cheaper than commercial vegetable protein foaming agents (12 USD/L) at 0.258 USD/L. Meanwhile, the properties of foam concrete prepared using SRP-50 were studied in comparison with a commercial vegetable protein foaming agent (PS). The results demonstrated that the foam prepared using SRP-50 had better stability, and the displacement of the foam decreased by 10% after 10 min. During the curing period, the foam concrete possesseda compressive strength of 5.72 MPa after 28 days, which was an increase from 2.95 MPa before. The aperture of the foam ranged from 100 to 500 μm with the percentage increasing up to 71.5%, which indicated narrower pore-size distribution and finer pore size. In addition, the shrinkage of the foam concrete was also improved. These findings not only achieve the utilization of waste but also provide a new source for protein foaming agents. Full article
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<p>Effect of pH value on foaming ability.</p>
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<p>Effect of hydrolysis temperature on foaming ability.</p>
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<p>Effect of hydrolysis time on foaming ability.</p>
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<p>Response surface curves (<b>left</b>) and contour plots (<b>right</b>): (<b>a</b>) fixed X<sub>3</sub> at 3 h; (<b>b</b>) fixed X<sub>2</sub> at 50 °C; (<b>c</b>) fixed X<sub>1</sub> at 10.</p>
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<p>Effects of FS-50 and FS-3100 on foaming ability.</p>
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<p>Drainage of foams.</p>
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<p>Morphology of foams: (<b>a</b>) PS—20 times; (<b>b</b>) SRP—20 times.</p>
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<p>Compressive strength of foam concretes.</p>
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<p>Drying shrinkage of foam concretes.</p>
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<p>Microstructure of the control group (<b>a</b>) and experimental group (<b>b</b>).</p>
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<p>Aperture distributions of foam concrete group.</p>
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19 pages, 5356 KiB  
Article
Development and Application of Carbonate Dissolution Test Equipment under Thermal–Hydraulic–Chemical Coupling Condition
by Jinzhu Meng, Sili Chen, Junxiang Wang, Zhi Chen and Jingyu Zhang
Materials 2022, 15(20), 7383; https://doi.org/10.3390/ma15207383 - 21 Oct 2022
Cited by 7 | Viewed by 1882
Abstract
The latest continuous flow micro reaction technology was adopted to independently develop carbonate rock dissolution test equipment. Carbonate rock dissolution tests were conducted under different temperatures, flow rates, and dynamic water pressure conditions to study the dissolution process of carbonate rocks under the [...] Read more.
The latest continuous flow micro reaction technology was adopted to independently develop carbonate rock dissolution test equipment. Carbonate rock dissolution tests were conducted under different temperatures, flow rates, and dynamic water pressure conditions to study the dissolution process of carbonate rocks under the coupling of heat-water-chemistry. The dissolution effect and development law of carbonate rocks were explored by quantitatively studying carbonate rock dissolution rate and chemical composition of karst water. The results showed that the self-designed dissolution test equipment has obvious advantages. After dissolution, carbonate rock specimens were damaged to varying degrees. The dissolution rate was proportional to water velocity and hydrodynamic pressure, with the velocity effect being greater than the hydrodynamic pressure effect. The pH value, conductivity, and Ca2+ ion content of the reaction solution gradually increased after dissolution. The development and application of the equipment have proved that, at low dynamic water pressures (2 MPa), the water flow velocity effect on the dissolution velocity was 1.5 times that when the dynamic water pressure was high (6 MPa); at a low water flow velocity of 15 mL/min, the dynamic water pressure effect on the dissolution velocity was three times that when the water flow velocity was high (75 mL/min). The development process is gradually becoming strong and stable. Its research has important theoretical significance and engineering application value to provide technical means and guarantee for the early identification, karst development, and safety evaluation of karst geological disasters. Full article
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<p>Self-made YDYR-2 rock hydrodynamic pressure dissolution test equipment.</p>
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<p>Schematic diagram of the composition of the dissolution test equipment.</p>
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<p>Thin sections of carbonate rocks observed under optical microscopy.</p>
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<p>A supplementary figure of the X-ray diffraction whole-rock mineral analysis.</p>
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<p>Graphic of rock samples.</p>
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<p>Flow chart of the dissolution test.</p>
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<p>Comparison diagram of rock samples before and after dissolution: (<b>a</b>) Original sample; (<b>b</b>) Test condition 1; (<b>c</b>) Test condition 2; (<b>d</b>) Test condition 3; (<b>e</b>) Test condition 4.</p>
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<p>The dissolution rate of 16 carbonate rock specimens.</p>
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<p>Comparison of the dissolution rate at a water flow velocity of 15 mL/min.</p>
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<p>Comparison of the dissolution rate at a water flow velocity of 75 mL/min.</p>
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<p>Comparison of the dissolution rate at a pressure of 2 MPa.</p>
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<p>Comparison of the dissolution rate at a pressure of 6 MPa.</p>
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<p>The curve of change of pH value during the test.</p>
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<p>The trend of pH value before and after dissolution.</p>
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<p>The trend of electrical conductivity value before and after dissolution.</p>
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11 pages, 1312 KiB  
Article
Birch Tar Introduced into Polylactide and Its Influence on the Barrier, Thermal, Functional and Biological Properties of the Film Obtained by Industrial Extrusion
by Agnieszka Richert, Rafał Malinowski, Magda Ringwelska and Grażyna B. Dąbrowska
Materials 2022, 15(20), 7382; https://doi.org/10.3390/ma15207382 - 21 Oct 2022
Cited by 4 | Viewed by 1432
Abstract
The aim of the study was to evaluate possibility of producing a polylactide film with birch tar by the industrial extrusion method and whether the addition of 10% birch tar can ensure adequate biocidal properties of PLA against pathogenic microorganisms (E. coli [...] Read more.
The aim of the study was to evaluate possibility of producing a polylactide film with birch tar by the industrial extrusion method and whether the addition of 10% birch tar can ensure adequate biocidal properties of PLA against pathogenic microorganisms (E. coli, S. aureus, P. aeruginosa, A. tumefaciens, X. campestris, P. brassicacearum, P. corrugate and P. syringae) and fungi (A. niger, A. flavus and A. versicolor) while ensuring beneficial functional properties, such as water vapor, nitrogen, oxygen and carbon dioxide permeability, which are of considerable importance in the packaging industry. The main test methods used were ISO 22196, ISO 846, ISO 2556, ASTM F 1927 and ASTM F 2476-20. The obtained results prove the possibility of extruding polymer films with a biocidal additive, i.e., birch tar, and obtaining favorable properties that qualify the produced film for applications in the packaging industry. Full article
(This article belongs to the Special Issue Structure Property Relationship of Polymeric Materials)
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<p>DSC results of plasticizer PLA (L) and plasticizer PLA with birch tar (Lt5) analysis. (<b>A</b>) First-run analysis (first heating), (<b>B</b>) second-gear analysis (second heating), (<b>C</b>) cooling analysis.</p>
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<p>DSC results of plasticizer PLA (L) and plasticizer PLA with birch tar (Lt5) analysis. (<b>A</b>) First-run analysis (first heating), (<b>B</b>) second-gear analysis (second heating), (<b>C</b>) cooling analysis.</p>
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8 pages, 2708 KiB  
Article
Crystal Structures and Electronic Properties of BaAu Compound under High Pressure
by Bingtan Li, Jianyun Wang, Shuai Sun and Hanyu Liu
Materials 2022, 15(20), 7381; https://doi.org/10.3390/ma15207381 - 21 Oct 2022
Viewed by 1395
Abstract
The investigations of Au-bearing alloy materials have been of broad research interest as their relevant features exhibit significant advantages compared with pure Au. Here, we extensively investigate the compression behaviors of BaAu compounds via first-principles calculations and find that a high-pressure cubic phase [...] Read more.
The investigations of Au-bearing alloy materials have been of broad research interest as their relevant features exhibit significant advantages compared with pure Au. Here, we extensively investigate the compression behaviors of BaAu compounds via first-principles calculations and find that a high-pressure cubic phase is calculated to be stable above 12 GPa. Further electronic calculations indicate that despite the low electronegativity of Ba, Fd-3m-structured BaAu exhibits metallic characteristics, which is different from those of semiconducting alkali metal aurides that possess slight characteristics of an ionic compound. These findings provide a step toward a further understanding of the electronic properties of BaAu compounds and provide key insight for exploring the other Au-bearing alloy materials under extreme conditions. Full article
(This article belongs to the Special Issue Quantum Materials and Emergent Phenomena under Extreme Conditions)
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<p>The schematic figure of this manuscript.</p>
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<p>(<b>a</b>) Enthalpy as a function of external pressure for selected structures of BaAu in different symmetries. (<b>b</b>) The crystal structure of the <span class="html-italic">Fd</span>-3<span class="html-italic">m</span> BaAu under high pressure. Yellow and red spheres represent Ba and Au atoms, respectively. Phonon dispersions of BaAu with (<b>c</b>) <span class="html-italic">Pnma</span> symmetry at 10 GPa and (<b>d</b>) <span class="html-italic">Fd</span>-3<span class="html-italic">m</span> symmetry at 25 GPa.</p>
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<p>(<b>a</b>) PDOS calculated using the Perdew–Burke–Ernzerhof functional for BaAu in the <span class="html-italic">Pnma</span> structure at 10 GPa. PDOS calculated for BaAu in the <span class="html-italic">Fd</span>-3<span class="html-italic">m</span> structure at (<b>b</b>) 25 GPa, (<b>c</b>) 100 GPa, and (<b>d</b>) hypothetical Ba<sub>0</sub>Au at 25 GPa. The dashed line at zero indicates the Fermi energy.</p>
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<p>(<b>a</b>) Calculated electron localization function (ELF) for <span class="html-italic">Fd</span>-3<span class="html-italic">m</span>-BaAu compounds on the (101) plane at 25 GPa. (<b>b</b>) Pressure dependence of the Bader charges on Au in <span class="html-italic">Fd</span>-3<span class="html-italic">m-</span>structured BaAu from 25 to 100 GPa.</p>
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<p>PDOS calculated for CsAu (<b>a</b>) and BaAu (<b>b</b>) with the CsCl-type structure at 0 GPa.</p>
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16 pages, 11197 KiB  
Article
The Tribological Properties of 30CrMnSiA Bearing Steels Treated by the Strengthening Grinding Process under Lubrication Wear
by Xiaochu Liu, Xiujie Chen, Zhongwei Liang, Tao Zou, Zhaoyang Liu, Jinrui Xiao, Dongwei Li and Diaodiao Yu
Materials 2022, 15(20), 7380; https://doi.org/10.3390/ma15207380 - 21 Oct 2022
Cited by 7 | Viewed by 1543
Abstract
This study used the strengthening grinding process (SGP) to treat the surface of 30CrMnSiA bearing steels. The effect of the jet angle of SGP on the tribological properties of 30CrMnSiA bearing steels under lubrication was investigated. The principle of enhancing wear resistance of [...] Read more.
This study used the strengthening grinding process (SGP) to treat the surface of 30CrMnSiA bearing steels. The effect of the jet angle of SGP on the tribological properties of 30CrMnSiA bearing steels under lubrication was investigated. The principle of enhancing wear resistance of 30CrMnSiA bearing steel ascribed to SGP was discussed in detail. The results showed that the lubrication properties and surface hardness of the 30CrMnSiA steels were enhanced due to the formation of numerous microscale microscope oil pockets on the surface layer and the grain refinement of the surface microstructures, resulting in a significant improvement in wear resistance. With the jet angle of SGP increased from 0° to 90°, the friction coefficient, the wear volume, and the specific wear rate were exhibited to reduce rapidly first, then reduce slowly, and then rise slowly. With the optimal parameters at the jet angle of 60°, compared with the control sample, the average friction coefficient was reduced from 0.2235 to 0.1609, and the wear volume and specific wear rate were reduced from 9.04 × 10−3 mm3 to 3.82 × 10−3 mm3 and from 15.13 × 10−3 mm2/N to 6.36 × 10−3 mm2/N, respectively. When the jet angle was 90°, the reduced wear resistance was mainly attributed to the excessive roughness that caused the oil coating on the surface to be severely damaged. Full article
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<p>SEM microstructure of 30CrMnSiA.</p>
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<p>Parameter setting and treatment process of SGP.</p>
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<p>Principle diagram of sliding wear.</p>
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<p>(<b>a</b>) SEM maps of surface microstructure versus jet angle; (<b>b</b>) three-dimensional morphology at different jet angles; (<b>c</b>) two-dimensional profile at different jet angles.</p>
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<p>(<b>a</b>) Two-dimensional profile pits at different jet angles; (<b>b</b>) width and depth of pits versus jet angle; (<b>c</b>) surface roughness at different jet angles; (<b>d</b>) hardness profiles in the cross-sectional at different jet angles.</p>
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<p>(<b>a</b>) The X-ray diffraction pattern characteristics on the tested sample surface; (<b>b</b>) the average grain size and lattice deformation at different jet angles.</p>
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<p>(<b>a</b>) Friction coefficients at functions of time at different jet angles; (<b>b</b>) friction coefficients during the running-in stage.</p>
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<p>Average friction coefficients at different jet angles.</p>
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<p>Three-dimensional wear morphology at different jet angles of SGP.</p>
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<p>Two-dimensional morphology of wear masks: (<b>a</b>) wear mark section profile versus jet angle; (<b>b</b>) average wear depth and width versus jet angle.</p>
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<p>(<b>a</b>) The wear volume versus jet angle of SGP; (<b>b</b>) specific wear rates at different jet angles of SGP.</p>
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<p>SEM images of worn surface morphology under different jet angles.</p>
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<p>Two-dimensional illustration of the microscope oil pocket.</p>
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<p>Microscope morphology of the oil pocket.</p>
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22 pages, 19176 KiB  
Article
Fracture Behavior of Basalt Fiber-Reinforced Airport Pavement Concrete at Different Strain Rates
by Yifan Mu, Haiting Xia, Yong Yan, Zhenhui Wang and Rongxin Guo
Materials 2022, 15(20), 7379; https://doi.org/10.3390/ma15207379 - 21 Oct 2022
Cited by 10 | Viewed by 1849
Abstract
As a commonly used surface structure for airport runways, concrete slabs are subjected to various complex and random loads for a long time, and it is necessary to investigate their fracture performance at different strain rates. In this study, three-point bending fracture tests [...] Read more.
As a commonly used surface structure for airport runways, concrete slabs are subjected to various complex and random loads for a long time, and it is necessary to investigate their fracture performance at different strain rates. In this study, three-point bending fracture tests were conducted using ordinary performance concrete (OPC) and basalt fiber-reinforced airport pavement concrete (BFAPC) with fiber volume contents of 0.2, 0.4, and 0.6%, at five strain rates (10−6 s−1, 10−5 s−1, 10−4 s−1, 10−3 s−1, and 10−2 s−1). Considering parameters such as the peak load, initial cracking load, double K fracture toughness, fracture energy, and critical crack expansion rate, the effects of the fiber volume content and strain rate on the fracture performance of concrete were systematically studied. The results indicate that these fracture parameters of OPC and BFAPC have an obvious strain rate dependence; in particular, the strain rate has a positive linear relationship with peak load and fracture energy, and a positive exponential relationship with the critical crack growth rate. Compared with OPC, the addition of basalt fiber (BF) can improve the fracture performance of airport pavement concrete, to a certain extent, where 0.4% and 0.6% fiber content were the most effective in enhancing the fracture properties of concrete under strain rates of 10−6–10−5 s−1 and 10−4–10−2 s−1, respectively. From the point of view of the critical crack growth rate, it is shown that the addition of BF can inhibit the crack growth of concrete. In this study, the fracture properties of BFAPC were evaluated at different strain rates, providing an important basis for the application of BFAPC in airport pavement. Full article
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<p>(<b>a</b>) Macro and (<b>b</b>) micro morphologies of BF.</p>
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<p>Regimes of strain rates.</p>
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<p>Diagram of the test device.</p>
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<p>The failure sections of concrete at different loading rates: (<b>a</b>) 10<sup>−6</sup> s<sup>−1</sup>; (<b>b</b>) 10<sup>−4</sup> s<sup>−1</sup>; and (<b>c</b>) 10<sup>−2</sup> s<sup>−1</sup>.</p>
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<p>The <span class="html-italic">P–CMOD</span> curves under different loading rates: (<b>a</b>) OPC; (<b>b</b>) B-0.2; (<b>c</b>) B-0.4; and (<b>d</b>) B-0.6.</p>
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<p>The relationship between the peak load and strain rate: (<b>a</b>) OPC; (<b>b</b>) B-0.2; (<b>c</b>) B-0.4; and (<b>d</b>) B-0.6.</p>
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<p>Peak loads under different fiber content.</p>
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<p>Comparison of the <span class="html-italic">P</span><sub>ini</sub> value obtained by the test curve method and the strain gauge method.</p>
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<p>Relationship between the initial cracking load and strain rate.</p>
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<p>The relationship between the double K fracture toughness and strain rate: (<b>a</b>) OPC; (<b>b</b>) B-0.2; (<b>c</b>) B-0.4; and (<b>d</b>) B-0.6.</p>
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<p>The relationship between the fracture energy and strain rate: (<b>a</b>) OPC; (<b>b</b>) B-0.2; (<b>c</b>) B-0.4; and (<b>d</b>) B-0.6.</p>
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<p>(<b>a</b>) The fracture energy and (<b>b</b>) ductility index of BFAPC with different fiber contents.</p>
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<p>The BFAPC with 0.6% fiber content at strain rate of 10<sup>−6</sup> s<sup>−1</sup> at peak load: (<b>a</b>) COD contour; (<b>b</b>) COD pattern at y = 40 mm; (<b>c</b>) COD pattern at y = 66.85 mm; and (<b>d</b>) strain contour.</p>
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<p>The strain contours of 0.6% BFAPC at strain rate of 10<sup>−6</sup> s<sup>−1</sup> and 10<sup>−4</sup> s<sup>−1</sup>: (<b>a</b>) Pre-60%<span class="html-italic">P</span><sub>max</sub>; (<b>b</b>) pre-80%<span class="html-italic">P</span><sub>max</sub>; (<b>c</b>) <span class="html-italic">P</span><sub>max</sub>; (<b>d</b>) post-80%<span class="html-italic">P</span><sub>max</sub>; and (<b>e</b>) post-20%<span class="html-italic">P</span><sub>max</sub>.</p>
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<p>Variation diagram of strain and load with time: (<b>a</b>) schematic; and (<b>b</b>) experimental result.</p>
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<p>Critical crack propagation velocities at various loading rates: (<b>a</b>) OPC; (<b>b</b>) B-0.2; (<b>c</b>) B-0.4; and (<b>d</b>) B-0.6.</p>
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<p>Effect of fiber content on critical crack propagation velocities.</p>
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18 pages, 4237 KiB  
Article
Chemical State of Potassium on the Surface of Iron Oxides: Effects of Potassium Precursor Concentration and Calcination Temperature
by Md. Ariful Hoque, Marcelo I. Guzman, John P. Selegue and Muthu Kumaran Gnanamani
Materials 2022, 15(20), 7378; https://doi.org/10.3390/ma15207378 - 21 Oct 2022
Cited by 1 | Viewed by 4305
Abstract
Potassium is used extensively as a promoter with iron catalysts in Fisher–Tropsch synthesis, water–gas shift reactions, steam reforming, and alcohol synthesis. In this paper, the identification of potassium chemical states on the surface of iron catalysts is studied to improve our understanding of [...] Read more.
Potassium is used extensively as a promoter with iron catalysts in Fisher–Tropsch synthesis, water–gas shift reactions, steam reforming, and alcohol synthesis. In this paper, the identification of potassium chemical states on the surface of iron catalysts is studied to improve our understanding of the catalytic system. Herein, potassium-doped iron oxide (α-Fe2O3) nanomaterials are synthesized under variable calcination temperatures (400–800 °C) using an incipient wetness impregnation method. The synthesis also varies the content of potassium nitrate deposited on superfine iron oxide with a diameter of 3 nm (Nanocat®) to reach atomic ratios of 100 Fe:x K (x = 0–5). The structure, composition, and properties of the synthesized materials are investigated by X-ray diffraction, differential scanning calorimetry, thermogravimetric analysis, Fourier-transform infrared, Raman spectroscopy, inductively coupled plasma-atomic emission spectroscopy, and X-ray photoelectron spectroscopy, as well as transmission electron microscopy, with energy-dispersive X-ray spectroscopy and selected area electron diffraction. The hematite phase of iron oxide retains its structure up to 700 °C without forming any new mixed phase. For compositions as high as 100 Fe:5 K, potassium nitrate remains stable up to 400 °C, but at 500 °C, it starts to decompose into nitrites and, at only 800 °C, it completely decomposes to potassium oxide (K2O) and a mixed phase, K2Fe22O34. The doping of potassium nitrate on the surface of α-Fe2O3 provides a new material with potential applications in Fisher–Tropsch catalysis, photocatalysis, and photoelectrochemical processes. Full article
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<p>X-ray diffraction (XRD) patterns of 100 Fe:<span class="html-italic">x</span> K materials, with the atomic ratio of potassium (<span class="html-italic">x</span>) indicated in each panel. The assigned Miller indices match the hematite phase of iron oxide.</p>
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<p>XRD patterns of the 100 Fe:5 K material calcined at the temperature indicated in each panel. The assigned Miller indices match the hematite phase of iron oxide. The peaks are marked as black asterisks (*) for K<sub>2</sub>O and as red crosses (×) for K<sub>2</sub>Fe<sub>22</sub>O<sub>34</sub>.</p>
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<p>Thermogravimetric analysis (TGA, dashed line with the left vertical axis) and the first derivative of the thermogram (solid line with the right vertical axis) curves for 100 Fe:5 K material, at the calcination temperatures indicated in each panel. Peaks A and B correspond to the conversion of KNO<sub>2</sub> to K<sub>2</sub>O, and of KNO<sub>3</sub> to KNO<sub>2</sub>, respectively.</p>
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<p>Raman spectra of 100 Fe:<span class="html-italic">x</span> K materials, with the atomic ratio of potassium (<span class="html-italic">x</span>) indicated in each panel. The numbers 1 to 8 correspond to modes of the hematite phase, while peak 9 relates to a mode of <math display="inline"><semantics> <mrow> <msubsup> <mrow> <mi>NO</mi> </mrow> <mn>3</mn> <mo>−</mo> </msubsup> </mrow> </semantics></math> in the range of 980–1150 cm<sup>–1</sup>.</p>
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<p>X-ray photoelectron (XPS) survey spectra for 100 Fe:<span class="html-italic">x</span> K materials with <span class="html-italic">x</span> = 0, 1, and 5, as indicated by the red, green, and blue traces, respectively. The peak assignment is based on the binding energy of photoelectron and Auger electron lines.</p>
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<p>(Black trace) High-resolution XPS spectra of (<b>left panel</b>) O 1<span class="html-italic">s</span> and (<b>right panel</b>) Fe(III) 2<span class="html-italic">p</span> for 100 Fe:<span class="html-italic">x</span> K materials, calcined at 400 °C, with the atomic ratio of potassium (<span class="html-italic">x</span>) indicated in each panel. Dashed blue lines show the fitted peaks, numbered as follows: (1) O 1<span class="html-italic">s</span> for lattice oxides, (2) lattice hydroxyl, (3) surface hydroxyl, (4) Fe(III) 2<span class="html-italic">p</span><sub>3/2</sub>, (5) Fe 2<span class="html-italic">p</span><sub>3/2</sub> satellite, (6) Fe(III) 2<span class="html-italic">p</span><sub>1/2</sub>, and (7) Fe(III) 2<span class="html-italic">p</span><sub>1/2</sub> satellite. Solid green lines show the fitted background.</p>
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<p>(Black trace) High-resolution XPS spectra of (<b>left panel</b>) K 2<span class="html-italic">p</span> and (<b>right panel</b>) N 1<span class="html-italic">s</span> for 100 Fe:<span class="html-italic">x</span> K materials, calcined at 400 °C, with the atomic ratio of potassium (<span class="html-italic">x</span>) indicated in each panel. (Dashed blue) Fitted peaks numbered (8) K 2<span class="html-italic">p</span><sub>3/2</sub>, (9) K 2<span class="html-italic">p</span><sub>1/2</sub>, and (10) nitrate. (Solid green) Fitted background.</p>
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<p>(Black trace) High-resolution XPS spectra of (<b>left panel</b>) K 2<span class="html-italic">p</span> and (<b>right panel</b>) N 1<span class="html-italic">s</span> for 100 Fe:5 K material, calcined at the indicated temperatures. (Dashed blue) Fitted peaks numbered (8) K 2<span class="html-italic">p</span><sub>3/2</sub>, (9) K 2<span class="html-italic">p</span><sub>1/2</sub>, (10) nitrate, and (11) nitrite. (Solid green) Fitted background.</p>
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<p>(Black trace) High-resolution XPS spectra of O 1<span class="html-italic">s</span> for 100 Fe:5 K material, calcined at the temperature specified in each panel. (Dashed blue) Fitted peaks numbered (1) O 1<span class="html-italic">s</span> for lattice iron oxides, (2) lattice hydroxyl, (3) surface hydroxyl, and (12) K–O bonded species. (Solid green) Fitted background.</p>
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<p>(From left to right) Transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and selected area electron diffraction (SAED) patterns of (from top to bottom) 100 Fe:2 K, 100 Fe:½ K, and 100 Fe:0 K materials, calcined at 400 °C.</p>
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<p>Energy-dispersive X-ray spectroscopy (EDS) spectra of 100 Fe:<span class="html-italic">x</span> K materials for potassium contents (<span class="html-italic">x</span>) of (green) 0 K, (red) ½ K, and (blue) 5 K for the K (Kα) emission line.</p>
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<p>(From left to right) TEM, HRTEM, and SAED patterns of 100 Fe:5 K calcined at (from top to bottom), 800, 600, and 400 °C.</p>
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11 pages, 7593 KiB  
Article
Competitive Formation Zones in Carbon Nanotube Float-Catalysis Synthesis: Growth in Length vs. Growth Suppression
by Vladimir Z. Mordkovich, Aida R. Karaeva, Nikita V. Kazennov, Eduard B. Mitberg, Mariem Nasraoui, Boris A. Kulnitskiy and Vladimir D. Blank
Materials 2022, 15(20), 7377; https://doi.org/10.3390/ma15207377 - 21 Oct 2022
Cited by 1 | Viewed by 1837
Abstract
Catalytic synthesis of carbon nanotubes (CNT) produces numerous various byproducts such as soot, graphite platelets, catalyst nanoparticles, etc. Identification of the byproduct formation mechanisms would help develop routes to more selective synthesis of better carbon-based materials. This work reports on the identification of [...] Read more.
Catalytic synthesis of carbon nanotubes (CNT) produces numerous various byproducts such as soot, graphite platelets, catalyst nanoparticles, etc. Identification of the byproduct formation mechanisms would help develop routes to more selective synthesis of better carbon-based materials. This work reports on the identification of the formation zone and conditions for rather unusual closed multishell carbon nanocapsules in a reactor for float-catalysis synthesis of longer CNT. Structural investigation of the formed nanocapsule material along with computational fluid dynamics (CFD) simulations of the reactor suggested a nanocapsule formation mechanism, in which CNT embryos are suppressed in growth by the in-reactor turbulence. By means of TEM and FFT investigation, it is found that differently oriented single crystals of γ–Fe2O3, which do not have clear connections with each other, determine a spherical surface. The carbon atoms that seep through these joints do not form crystalline graphite layers. The resulting additional product in the form of graphene-coated (γ–Fe/Fe3C)/γ–Fe2O3 nanoparticles can be a lightweight and effective microwave absorber. Full article
(This article belongs to the Special Issue Current and Future Trends in Carbon-Based Materials)
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<p>Schematic representation of the proprietary float-catalysis synthesis reactor rig.</p>
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<p>CFD simulation of the flow trajectory of a feed gas in the turbulence zone after exiting the FIT at two different feed gas flowrates: (<b>a</b>) hydrogen flowrate 2.8 L/min; (<b>b</b>) hydrogen flowrate 1.4 L/min.</p>
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<p>TEM images of a short single CNT as a co-product obtained in the turbulence zone of the CNT-cotton synthesis reactor.</p>
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<p>Fe- containing carbon nanocapsules: (<b>a</b>) general TEM view manifesting mean particle size 15–30 nm; (<b>b</b>) detailed structure of a nanocapsule by TEM (arrows indicate two encapsulating shells: inner Fe<sub>2</sub>O<sub>3</sub> shell and outer carbon shell); (<b>c</b>) EDS spectra from view (<b>a</b>).</p>
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<p>Fe- containing carbon nanocapsules: (<b>a</b>) general TEM view manifesting mean particle size 15–30 nm; (<b>b</b>) detailed structure of a nanocapsule by TEM (arrows indicate two encapsulating shells: inner Fe<sub>2</sub>O<sub>3</sub> shell and outer carbon shell); (<b>c</b>) EDS spectra from view (<b>a</b>).</p>
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<p>Fragments of nanocapsules, the inner part of which contains Fe<sub>3</sub>C carbide (<b>a</b>) and γ– Fe (<b>b</b>). The tabs show the corresponding FFT.</p>
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<p>Carbon-encapsulated nanoparticles containing iron: (<b>a</b>) two fragments b and c are marked with white ellipses in the surface layer; (<b>b</b>,<b>c</b>) are the corresponding FFT, both fragments correspond to the cubic phase of γ– Fe<sub>2</sub>O<sub>3</sub> (maghemite), the axes of zones [11-2] and [-111], respectively.</p>
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<p>Carbon-encapsulated nanoparticles containing iron; a white ellipse marks a fragment with a γ– Fe<sub>2</sub>O<sub>3</sub> lattice. The tab shows the FFT from the selected area. The presence of reflex (0–11) is characteristic of the maghemite lattice.</p>
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<p>The particle through which the deformation bands pass (<b>a</b>). One of the bands is indicated by a white arrow; in the left part is the α– Fe (<b>b</b>), in the right part of the particle is the γ– Fe phase (<b>c</b>); (<b>d</b>) is the inverse FFT image of the deformation band (indicated by an arrow) with a structure close to amorphous.</p>
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11 pages, 3660 KiB  
Article
Evaluation of the Sublimation Process of Some Purine Derivatives: Sublimation Rate, Activation Energy, Mass Transfer Coefficients and Phenomenological Models
by Cerasela-Ionela Cleminte, Daniela Ionita, Cătălin Lisa, Mariana Cristea, Ioan Mamaligă and Gabriela Lisa
Materials 2022, 15(20), 7376; https://doi.org/10.3390/ma15207376 - 21 Oct 2022
Cited by 2 | Viewed by 1802
Abstract
Caffeine and theophylline are compounds with important applications in the pharmaceutical industry and other fields of the chemical industry. These purine derivatives have simple chemical structures, therefore, the evaluation of their sublimation process contributes to the development of mass transfer analysis methods that [...] Read more.
Caffeine and theophylline are compounds with important applications in the pharmaceutical industry and other fields of the chemical industry. These purine derivatives have simple chemical structures, therefore, the evaluation of their sublimation process contributes to the development of mass transfer analysis methods that can later be applied to other compounds with more complex structures. With the help of thermogravimetric analysis in isothermal conditions, the kinetic study of the sublimation of caffeine and theophylline, along with the evaluation of kinetic parameters (activation energy and the pre-exponential factor), was carried out. Global mass transfer coefficients were determined, which vary for caffeine between 53 × 10−8 and 631 × 10−8 mol/s·m2·Pa, and for theophylline between 68 × 10−8 and 441 × 10−8 mol/s·m2·Pa. The dimensionless equations of the form: Sh=a+b·Rec·Scd have been proposed, which allow the determination of individual mass transfer coefficients at temperatures between 130 and 160 °C for caffeine and between 170 and 200 °C for theophylline. Full article
(This article belongs to the Section Materials Chemistry)
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<p>TG (<b>a</b>) and DTG (<b>b</b>) curves.</p>
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<p>Optimized geometry representing ball shape for 12 caffeine molecules (<b>a</b>) and 12 theophylline molecules (<b>b</b>).</p>
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<p>Percentage loss of mass over time for the sublimation of caffeine at various temperatures: 130, 140, 150 and 160 °C.</p>
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<p>Percentage loss of mass over time for the sublimation of theophylline at various temperatures: 170, 180, 190 and 200 °C.</p>
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<p>The variation of the sublimation rate depending on the temperature for caffeine (<b>a</b>) and theophylline (<b>b</b>).</p>
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<p>Calculation of the parameters of the Arrhenius equation for caffeine (<b>a</b>) and theophylline (<b>b</b>).</p>
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<p>Influence of temperature on the mass transfer process for caffeine (<b>a</b>) and theophylline (<b>b</b>).</p>
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<p>Influence of temperature on the mass flow of sublimated caffeine (<b>a</b>) and theophylline (<b>b</b>).</p>
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