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Search Results (385)

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Keywords = powder agglomeration

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17 pages, 4105 KiB  
Article
Experimental and Simulation Studies on Thermal Shock of Multilayer Thermal Barrier Coatings with an Intermediate Transition Layer at 1500 °C
by Pengpeng Liu, Shilong Yang, Kaibin Li, Weize Wang, Yangguang Liu and Ting Yang
Coatings 2024, 14(12), 1614; https://doi.org/10.3390/coatings14121614 - 23 Dec 2024
Abstract
Strain tolerance is a crucial factor affecting the thermal life of coatings, and a higher strain tolerance can effectively alleviate the thermal stresses on coatings during thermal shock. To improve the strain tolerance, the coating structure was optimized by introducing an intermediate transition [...] Read more.
Strain tolerance is a crucial factor affecting the thermal life of coatings, and a higher strain tolerance can effectively alleviate the thermal stresses on coatings during thermal shock. To improve the strain tolerance, the coating structure was optimized by introducing an intermediate transition layer in this study. The intermediate transition layer material was prepared using a 1:1 volume ratio mixture of 6–8 wt. % Yttria-stabilized zirconia (YSZ) and NiCrAlY powders in the experiments. The coating structure consisted of an Al2O3-GdAlO3 (AGAP) anti-erosion layer, a YSZ layer, an intermediate transition layer, and a bonding layer from top to bottom. After thermal shock experiments at 1500 °C, the coatings with the addition of the intermediate transition layer exhibited different failure modes, with the crack location shifting from between the YSZ and the bonding layer to within the intermediate transition layer, compared to the coatings without the intermediate transition layer. Finite element simulation analysis showed that the intermediate transition layer effectively increased the strain tolerance of the coating and significantly reduced the thermal stress. Furthermore, incorporating an embedded micron agglomerated particle-based (EMAP) thermal barrier coating structure into the intermediate transition layer effectively alleviated thermal stresses and enhanced the coating’s thermal insulation performance. Full article
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Figure 1
<p>Schematic of the Geometrical Model for Finite Element Simulation (the red arrow represents the path to the data extraction location).</p>
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<p>Cross-sectional morphologies of the as-sprayed (<b>a</b>,<b>d</b>) Group A, (<b>b</b>,<b>e</b>) Group B, and (<b>c</b>,<b>f</b>) Group C.</p>
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<p>Cross-sectional morphologies of coatings after thermal shock test (<b>a</b>) Group A, (<b>b</b>) Group B, (<b>c</b>) Group C.</p>
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<p>Temperature data plots of AYIB coatings with different intermediate transition layer thicknesses along the right boundary path at 1500 °C.</p>
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<p>Distribution of coating internal stresses along the right boundary path at 1500 °C for AYIB coatings with different intermediate transition layer thicknesses.</p>
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<p>Finite element model of AYI(E)B with different PEPC contents: (<b>a</b>) 3%; (<b>b</b>) 6%; (<b>c</b>) 9%.</p>
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<p>Temperature data plots of AYI(E)B coatings with different intermediate transition layer thicknesses along the right boundary path at 1500 °C.</p>
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<p>Stress distribution along the right boundary path at 1500 °C for coatings with different PEPC contents.</p>
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<p>AYI(E)B multilayer thermal barrier coating design solution.</p>
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31 pages, 15017 KiB  
Article
Green Synthesized Composite AB-Polybenzimidazole/TiO2 Membranes with Photocatalytic and Antibacterial Activity
by Hristo Penchev, Katerina Zaharieva, Silvia Dimova, Ivelina Tsacheva, Rumyana Eneva, Stephan Engibarov, Irina Lazarkevich, Tsvetelina Paunova-Krasteva, Maria Shipochka, Ralitsa Mladenova, Ognian Dimitrov, Daniela Stoyanova and Irina Stambolova
Crystals 2024, 14(12), 1081; https://doi.org/10.3390/cryst14121081 - 16 Dec 2024
Viewed by 608
Abstract
Novel AB-Polybenzimidazole (AB-PBI)/TiO2 nanocomposite membranes have been prepared using a synthetic green chemistry approach. Modified Eaton’s reagent (methansulfonic acid/P2O5) was used as both reaction media for microwave-assisted synthesis of AB-PBI and as an efficient dispersant of partially agglomerated [...] Read more.
Novel AB-Polybenzimidazole (AB-PBI)/TiO2 nanocomposite membranes have been prepared using a synthetic green chemistry approach. Modified Eaton’s reagent (methansulfonic acid/P2O5) was used as both reaction media for microwave-assisted synthesis of AB-PBI and as an efficient dispersant of partially agglomerated titanium dioxide powders. Composite membranes of 80 µm thickness have been prepared by a film casting approach involving subsequent anti-solvent inversion in order to obtain porous composite membranes possessing high sorption capacity. The maximal TiO2 filler content achieved was 20 wt.% TiO2 nanoparticles (NPs). Titania particles were green synthesized (using a different content of Mentha Spicata (MS) aqueous extract) by hydrothermal activation (150 °C), followed by thermal treatment at 400 °C. The various methods such as powder X-ray diffraction and Thermogravimetric analyses, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and Energy-dispersive X-ray spectroscopy, Electronic paramagnetic resonance, Scanning Electron Microscopy and Transmission Electron Microscopy have been used to study the phase and surface composition, structure, morphology, and thermal behavior of the synthesized nanocomposite membranes. The photocatalytic ability of the so-prepared AB-Polybenzimidazole/bio-TiO2 membranes was studied for decolorization of Reactive Black 5 (RB5) as a model azo dye pollutant under UV light illumination. The polymer membrane in basic form, containing TiO2 particles, was obtained with a 40 mL quantity of the MS extract, exhibiting the highest decolorization rate (96%) after 180 min of UV irradiation. The so-prepared AB-Polybenzimidazole/TiO2 samples have a powerful antibacterial effect on E. coli when irradiated by UV light. Full article
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<p>TEM micrographs and particle size distribution of M0 (<b>a</b>), M1 (<b>b</b>), and M2 (<b>c</b>) particles.</p>
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<p>TEM micrographs and particle size distribution of M0 (<b>a</b>), M1 (<b>b</b>), and M2 (<b>c</b>) particles.</p>
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<p>Diffuse-reflection spectra of green synthesized TiO<sub>2</sub> particles.</p>
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<p>Absorption spectra of the green synthesized TiO<sub>2</sub> particles with Kubelka–Munk conversion.</p>
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<p>Tauc’s plots of green synthesized TiO<sub>2</sub> particles.</p>
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<p>EPR spectra (right) of green synthesized TiO<sub>2</sub> particles.</p>
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<p>General preparation scheme for the synthesis of composite AB-PBI/TiO<sub>2</sub> membranes and reaction parameter comparison of the conventional (<b>left</b>) and microwave-assisted approaches (<b>right</b>).</p>
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<p>PXRD patterns of (<b>a</b>) green synthesized TiO<sub>2</sub> and (<b>b</b>) AB-PBI/bio-TiO<sub>2</sub> membranes and (<b>c</b>) pristine AB-PBI.</p>
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<p>Deconvolution of C1s, O1s, and N1s core level spectra of the AB-PBI-TiO<sub>2</sub>, M1 membranes (neutralized and acid-doped forms).</p>
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<p>EPR spectra of 1—polybenzimidazole; 2—PBI/bio-TiO<sub>2</sub>, M1 before UV irradiation; 3—PBI/bio-TiO<sub>2</sub>, M1 after UV irradiation recorded at room temperature; 4—PBI/bio-TiO<sub>2</sub>, M1 after UV irradiation recorded at 123 K.</p>
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<p>SEM images of (<b>A</b>) AB-PBI/bio-TiO<sub>2</sub>, M1 (basic form) and (<b>B</b>) AB-PBI/bio-TiO<sub>2</sub>, M1 (acid-doped form) membranes.</p>
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<p>EDS mapping of (<b>A</b>) AB-PBI/bio-TiO<sub>2</sub>, M1 (neutralized form) and (<b>B</b>) AB-PBI/bio-TiO<sub>2</sub>, M1 (acid-doped form) membranes.</p>
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<p>EDS mapping of (<b>A</b>) AB-PBI/bio-TiO<sub>2</sub>, M1 (neutralized form) and (<b>B</b>) AB-PBI/bio-TiO<sub>2</sub>, M1 (acid-doped form) membranes.</p>
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<p>FTIR spectra of green synthesized TiO<sub>2</sub> and AB-PBI/bio-TiO<sub>2</sub> membranes.</p>
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<p>Thermogravimetric curves of AB-PBI/TiO<sub>2</sub> membranes.</p>
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<p>Kinetic curves of UV decolorization of Reactive Black 5 dye using AB-PBI/bio-TiO<sub>2</sub> membranes as photocatalysts.</p>
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<p>Degree of decolorization of RB 5 dye during UV irradiation time period using (<b>a</b>,<b>b</b>) AB-PBI/bio-TiO<sub>2</sub>, M0 (neutralized and acid-doped forms); (<b>c</b>,<b>d</b>) AB-PBI/bio-TiO<sub>2</sub>, M1 (neutralized and acid-doped forms); (<b>e</b>,<b>f</b>) AB-PBI/bio-TiO<sub>2</sub>, M2 (neutralized and acid-doped forms) membranes as photocatalysts.</p>
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<p>UV–Vis absorption spectra of RB 5 dye during irradiation time period using AB-PBI/bio-TiO<sub>2</sub>, M1 (basic form) as the photocatalyst.</p>
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<p>The adsorption capacities (Q) (mg/g) of (1) and (2) AB-PBI/bio-TiO<sub>2</sub>, M2 (acid-doped and neutralized forms); (3) and (4) AB-PBI/bio-TiO<sub>2</sub>, M1 (neutralized and acid-doped forms); (5) and (6) AB-PBI/bio-TiO<sub>2</sub>, M0 (acid-doped and neutralized forms) membranes after a 30 min dark period.</p>
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<p>Degree of decolorization of RB 5 dye after 180 min under UV irradiation using basic form membranes in three photocatalytic runs. (<b>a</b>) AB-PBI/bio-TiO<sub>2</sub>, M0; (<b>b</b>) AB-PBI/bio-TiO<sub>2</sub>, M1; and (<b>c</b>) AB-PBI/bio-TiO<sub>2</sub>, M2.</p>
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<p>(<b>A</b>) Antimicrobial effect of the UV-irradiated (violet columns) suspensions of M0, M1, and M2 (0.5 mg/mL) with <span class="html-italic">E. coli</span> compared with their equivalents kept in the dark (gray columns) expressed as CFU/mL. (<b>B</b>) The decrease of CFU under UV light is well visible in the petri dishes.</p>
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<p>Antimicrobial effect of the composite membranes AB-PBI/bio-TiO<sub>2</sub>, M0, AB-PBI/bio-TiO<sub>2</sub>, M1, and AB-PBI/bio-TiO<sub>2</sub>, M2 on <span class="html-italic">E. coli</span> in the dark tested by the ASTM Standard Test Method E 2149–10. Control samples contain only bacterial suspension.</p>
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<p>Effect of AB-PBI-TiO<sub>2</sub> composites on standard <span class="html-italic">E. coli</span> suspension under UV irradiation for 10 min. Control samples contain only bacterial suspension.</p>
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<p>Representative SEM micrographs revealing the surface morphology and adhesion of <span class="html-italic">E. coli</span> 25922 during cultivation with composite membranes AB-PBI/bio-TiO<sub>2</sub>, M0 ((<b>a</b>)—treated with UV, 10 min. (<b>b</b>)—untreated), AB-PBI/bio-TiO<sub>2</sub>, M1 ((<b>c</b>)—treated with UV, 10 min. (<b>d</b>)—untreated) and AB-PBI/bio-TiO<sub>2</sub>, M2 ((<b>e</b>)—treated with UV, 10 min, (<b>f</b>)—untreated). Designations: White arrows—blebs or invaginations; white triangle—ruptured cells; white stars—amorphous substance. Zoom images highlight some of the damage in the bacterial cells. Bars = 5 μm.</p>
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19 pages, 21321 KiB  
Article
Mechanochemical Activation of Waste Clay Brick Powder with Addition of Waste Glass Powder and Its Influence on Pozzolanic Reactivity
by Csilla Őze, Nikolett Badacsonyi and Éva Makó
Molecules 2024, 29(23), 5740; https://doi.org/10.3390/molecules29235740 - 5 Dec 2024
Viewed by 385
Abstract
The availability of industrially used supplementary cementitious materials (SCMs, e.g., fly ash) decreases due to the rise in renewable energy sources and recycling technologies. Therefore, it is essential to find alternative SCMs (e.g., waste glass and clay brick powder) that are locally available. [...] Read more.
The availability of industrially used supplementary cementitious materials (SCMs, e.g., fly ash) decreases due to the rise in renewable energy sources and recycling technologies. Therefore, it is essential to find alternative SCMs (e.g., waste glass and clay brick powder) that are locally available. Accordingly, in this paper, the mechanochemical activation of clay brick waste (CBW) with abrasive glass powder (GP) and its pozzolanic reactivity are investigated. The mixtures of CBW and GP in mass ratios of 100:0, 75:25, 50:50, and 25:75 were mechanochemically activated for 15, 30, 45, and 60 min. The physical, chemical, and structural changes of the mixtures were examined by X-ray diffractometry, Fourier-transform infrared spectroscopy, scanning electron microscopy, and specific surface area measurements. The pozzolanic reactivity was characterized by the active silica content and the 28-day compressive strength of the binders (a mixture of ordinary Portland cement and activated material). The addition of GP favorably reduced the agglomeration and increased the active silica content of the activated mixtures (e.g., by 7–37% m/m at 15 min of mechanochemical activation). The 60 min of mechanochemical activation and the addition of 50% m/m of GP can increase the compressive strength by approximately 8%. Economically, the addition of 50% m/m of GP was found to be favorable, where only 30 min of mechanochemical activation resulted in a considerable increase in strength compared to that of the ordinary Portland cement. Full article
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<p>XRD patterns of the glass powder (GP) sample and the samples with 100, 75, 50, and 25% m/m of CBW (CBW, 75_CBW, 50_CBW, 25_CBW) ground for 0, 15, 30, and 60 min. (Mu: dehydroxylated muscovite PDF00-046-0741; An: anorthite PDF01-085-0878; Q: quartz PDF00-033-1161; D: diopside PDF00-011-0654, H: hematite PDF00-033-0664, M: Mullite PDF00-015-0776).</p>
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<p>Phase composition of the samples ground for 0, 15, 30, and 60 min. (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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<p>FT−IR spectra of the GP sample and the CBW, 75_CBW, 50_CBW, and 25_CBW samples ground for 0, 15, and 60 min. (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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<p>The amount of active SiO<sub>2</sub> of the samples ground for 0, 15, 30, and 60 min. (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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<p>SEM images of the samples measured at 250× and 25,000× magnification: CBW (1/A), CBW_15 (1/B), CBW_60 (1/C), 75_CBW (2/A), 75_CBW_15 (2/B), 75_CBW_60 (2/C), and GP (3/A). (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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<p>The secondary particle-size distribution (SPS) of the CBW, 75_CBW, 50_CBW, and 25_CBW samples after 15 and 60 min of mechanochemical activation and the primary particle-size distribution (PPS) of the GP sample. (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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<p>The primary particle-size distribution (PPS) of the CBW, 75_CBW, 50_CBW, and 25_CBW samples after 15 and 60 min of mechanochemical activation. (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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<p>The compressive strength of mortar specimens prepared with the OPC, the GP, the CBW, the 75_CBW, the 50_CBW, and the 25_CBW samples after 15 and 60 min of mechanochemical activation. (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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<p>The relative strength-difference index as a function of specific energy demand of mechanochemical activation. (The symbols of samples are given in <a href="#molecules-29-05740-f001" class="html-fig">Figure 1</a>).</p>
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17 pages, 11223 KiB  
Article
Structural Similarity-Induced Inter-Component Interaction in Silicone Polymer-Based Composite Sunscreen Film for Enhanced UV Protection
by Yuyan Chen, Hanwen Xu, Yuhang Liu, Qiuting Fu, Pingling Zhang, Jie Zhou, Hongyu Dong and Xiaodong Yan
Polymers 2024, 16(23), 3317; https://doi.org/10.3390/polym16233317 - 27 Nov 2024
Viewed by 452
Abstract
Film-forming agents are key ingredients in achieving long-lasting and effective sun protection by sunscreens. However, studies on the synergistic effects of film-forming agents with different properties as well as the interaction between film-forming agents and powders are scarce, restricting the development of sunscreens [...] Read more.
Film-forming agents are key ingredients in achieving long-lasting and effective sun protection by sunscreens. However, studies on the synergistic effects of film-forming agents with different properties as well as the interaction between film-forming agents and powders are scarce, restricting the development of sunscreens with strong ultraviolet (UV)-shielding effects. Herein, we innovatively adopt polysiloxane-15 as the soft film, trimethylsiloxysilicate as the hard film, and vinyl dimethicone/methicone silsesquioxane crosspolymer as the functional powder to construct a co-assembled sunscreen film, and we investigate the property-enhancing effects of the sunscreen film as well as the interaction between the silicone polymer-based film-forming agents and functional powder therein. The results show that structural similarity is essential to generating film-forming agent–powder interactions, which primarily enhance the Si−O bond binding energy, thereby enhancing the lasting protection effect of sunscreens. In addition, the inter-component interaction of the co-assembled sunscreen film inhibits the agglomeration of sunscreen paste to facilitate the formation of a homogeneous film, endowing the sunscreen with excellent UV protection abilities, with the sun protection factor (SPF) and protection factor of UVA (PFA) values increased by 61.58 and 43.84%, respectively. This work offers novel insights into the optimization of film-forming agent properties and the development of durable and efficient sunscreens. Full article
(This article belongs to the Special Issue Application and Characterization of Polymer Composites)
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Figure 1
<p>SEM images of (<b>A</b>) sample A, (<b>B</b>) sample B, (<b>C</b>) sample C, and (<b>D</b>) sample D after stretching.</p>
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<p>Film-forming conditions of sunscreen samples (<b>A</b>) CA, (<b>B</b>) BC, (<b>C</b>) NS, (<b>D</b>) NH, (<b>E</b>) NP, (<b>F</b>) RS, (<b>G</b>) RH, and (<b>H</b>) RP before and after stretching.</p>
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<p>SEM images of (<b>A</b>) VDSC and (<b>B</b>) talc. (<b>C</b>) Contact angles of pure VDSC and talc to film-forming agent solution.</p>
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<p>The migration conditions of coatings during drying of sunscreen samples (<b>A</b>) BC, (<b>B</b>) CA, and (<b>C</b>) NP. The time interval for each graph from left to right is 15 min.</p>
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<p>Film-forming conditions of sunscreen samples (<b>A</b>) CA, (<b>B</b>) BC, (<b>C</b>) NS, (<b>D</b>) NH, (<b>E</b>) NP, (<b>F</b>) RS, (<b>G</b>) RH, and (<b>H</b>) RP before and after rubbing.</p>
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<p>FTIR spectra of film-forming agent, (<b>A</b>) VDSC, and (<b>B</b>) talc before and after treatment. (<b>C</b>) Si 2p and (<b>D</b>) O 1s XPS spectra of VDSC before and after treatment.</p>
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<p>(<b>A</b>) UV absorption curves and (<b>B</b>) sun protection value test results of each sample.</p>
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<p>Three-dimensional contour images of pig skin (<b>A</b>) before and (<b>B</b>) after application of sunscreen CA, and contour curves of (<b>C</b>) X and (<b>D</b>) Y profiles. Three-dimensional contour images of pig skin (<b>E</b>) before and (<b>F</b>) after application of sunscreen BC, and contour curves of (<b>G</b>) X and (<b>H</b>) Y profiles.</p>
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<p>Comparison of initial and post-bath UV absorption curves of (<b>A</b>) CA, (<b>B</b>) BC, (<b>C</b>) NS, (<b>D</b>) NH, and (<b>E</b>) NP, and (<b>F</b>) sun protection value test results.</p>
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16 pages, 11772 KiB  
Article
Fabrication and Microstructure Analysis of Phosphate-Coated Mg Powder for Biomedical PLA/Mg Composites
by Ying-Ting Huang and Fei-Yi Hung
J. Compos. Sci. 2024, 8(12), 495; https://doi.org/10.3390/jcs8120495 - 26 Nov 2024
Viewed by 455
Abstract
Powdered magnesium has been widely applied in various fields. Magnesium is a highly reactive metal, with fine particles that are easy to agglomerate and have the risk of explosion. Furthermore, the storage of Mg particles is a challenge. Therefore, powdered magnesium is usually [...] Read more.
Powdered magnesium has been widely applied in various fields. Magnesium is a highly reactive metal, with fine particles that are easy to agglomerate and have the risk of explosion. Furthermore, the storage of Mg particles is a challenge. Therefore, powdered magnesium is usually passivated by surface modification methods. In our research, an environmentally friendly phosphate solution was used to prepare conversion coating on magnesium particles. The results demonstrated that the phosphate coating layer attached on Mg particles surface successfully. From SEM images, the average particle size reduces slightly after the coating process. The composition of the coating layer is confirmed to be OCP and HAp by XRD and EPMA. The immersion test showed that the phosphate coating improved the corrosion resistance, and the ideal processing time is 20 min. Moreover, Mg and phosphate have good biocompatibility; therefore, the coated Mg powder can be a potential candidate for biomedical applications. Full article
(This article belongs to the Section Biocomposites)
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<p>(<b>a</b>) XRD patterns for Mg particles with different coating times. (<b>b</b>) Provides a detailed view of calcium phosphate peaks formed with extended treatment time. In the sample label MX, X represents the treatment time of the magnesium powder in minutes.</p>
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<p>SEM images of Mg particles with different coating times. In the sample label MX, X represents the treatment time of the magnesium powder in minutes.</p>
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<p>EPMA element mapping and EDS analysis of Mg particles. In the sample label MX, X represents the treatment time of the magnesium powder in minutes: (<b>a</b>) M0, (<b>b</b>) M20, and (<b>c</b>) M60.</p>
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<p>TEM bright field of M20 surface.</p>
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<p>EDS mapping of the M20 cross-section.</p>
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<p>TEM images of (<b>a</b>) coating surface, (<b>b</b>) interface, and (<b>c</b>) substrate.</p>
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<p>The polarization curve of each specimen label MX, and X represents the treatment time of the magnesium powder in minutes.</p>
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<p>Mass change ratio of Mg particles after immersion in 0.9 wt.% NaCl solution and the appearance of the surface. In the sample label MX, X represents the treatment time of the magnesium powder in minutes.</p>
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<p>SEM images and EDS after immersion for 48 h. In the sample label MX, X represents the treatment time of the magnesium powder in minutes.</p>
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<p>SEM images of the magnified surface. In the sample label MX, X represents the treatment time of the magnesium powder in minutes.</p>
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<p>Formation mechanism of phosphate coating.</p>
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<p>(<b>a</b>) Microstructure of PLA with coated Mg powder and (<b>b</b>) schematic diagram.</p>
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20 pages, 17899 KiB  
Article
Modification of Ceritinib Crystal Morphology via Spherical Crystallization
by Iva Zokić, Jasna Prlić Kardum, Lana Crnac, Mirta Sabol, Juraj Vuić and Valentina Travančić
Crystals 2024, 14(11), 975; https://doi.org/10.3390/cryst14110975 - 12 Nov 2024
Viewed by 726
Abstract
The formulation process for some drugs can be challenging, due to their unfavorable physical and mechanical properties and poor water solubility. Powder technology has made a significant impact in regard to the modification of the particles in active pharmaceutical ingredients (APIs) to produce [...] Read more.
The formulation process for some drugs can be challenging, due to their unfavorable physical and mechanical properties and poor water solubility. Powder technology has made a significant impact in regard to the modification of the particles in active pharmaceutical ingredients (APIs) to produce high-quality granules. Spherical particles are preferred over other shapes, due to their high tap and bulk density, reduced dustiness, better flowability, strong anti-caking properties, and better mechanical performance during tableting. The present study investigates the possibility of obtaining spherical crystals of ceritinib, a drug used for the treatment of anaplastic lymphoma kinase (ALK)-positive advanced non-small cell lung cancer, which belongs to BCS class IV drugs and has a platy crystal shape. Ceritinib spheres were prepared by spherical agglomeration, in a ternary system, and quasi-emulsion solvent diffusion, with the addition of polyvinylpyrrolidone, as well as a combination of these two methods. With the combined method of spherical crystallization, crystals with the most favorable morphology and the narrowest distribution of particle sizes were obtained, which was the reason for further optimization. The influence of different impeller geometries and mixing rates on the morphology of the obtained crystals was examined and the optimal conditions for the process were selected. Using empirical correlations and a visual criterion, the process was scaled up from a 0.1 L to a 1 L batch crystallizer. The obtained crystals were characterized by light and scanning electron microscopy. The addition of a bridging liquid and/or a polymer additive did not change the internal structure of the ceritinib crystals, which was confirmed by X-ray powder diffraction. Full article
(This article belongs to the Collection Feature Papers in Biomolecular Crystals)
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<p>Shape of the crystals obtained using the SA method and the tetrahydrofuran–water–heptane 1:7:1 system.</p>
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<p>Shape of crystals obtained by the QESD method with (<b>a</b>) 1 wt.%, (<b>b</b>) 3 wt.%, and (<b>c</b>) 5 wt.% PVP.</p>
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<p>SEM micrographs of dry spheres obtained from the tetrahydrofuran–water + 1 wt.% PVP–heptane system.</p>
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<p>Formation of spherical crystals recorded at (<b>a</b>) 5, (<b>b</b>) 20, and (<b>c</b>) 40 min.</p>
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<p>Visual determination of critical mixing rate for PROP impeller at mixing rates of (<b>a</b>) 300, (<b>b</b>) 500, and (<b>c</b>) 700 rpm.</p>
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<p>PSDs of spherical crystals obtained by the SA+QESD method, using all three impeller types at the respective minimum mixing rate.</p>
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<p>PSDs of spherical crystals obtained by the SA+QESD method, using the RT6-45 impeller at various mixing rates.</p>
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<p>PSDs of spherical crystals obtained by the SA+QESD method, using the PROP impeller at various mixing rates.</p>
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<p>PSDs of spherical crystals obtained by the SA+QESD method, using the RT6-90 impeller at various mixing rates.</p>
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<p>PSDs of spheres obtained by the SA+QESD method, using all three impellers, at a mixing rate of 800 rpm.</p>
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<p>Carr’s index of spherical crystals obtained using the SA+QESD method.</p>
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<p>The procedure for the determination of the minimum mixing rate: (<b>a</b>) 0 rpm, (<b>b</b>) 450 rpm, (<b>c</b>) 580 rpm, and (<b>d</b>) 747 rpm.</p>
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<p>PSDs of spheres obtained by scaling up the SA+QESD method at mixing rates of 580 and 747 rpm.</p>
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<p>SEM micrographs of (<b>a</b>) pure CRT form A and spherical crystals obtained using the SA+QESD method, (<b>b</b>) in the small vessel at 800 rpm, and in the large vessel at (<b>c</b>) 580 rpm and (<b>d</b>) 747 rpm.</p>
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<p>XRD spectra of PVP, pure CRT form A, and spherical crystals obtained using the SA, QESD, and SA+QESD methods.</p>
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<p>The mass loss curve was obtained by TGA for the PROP impeller, 800 rpm sample.</p>
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28 pages, 6631 KiB  
Review
Recent Advances in Hybrid Nanocomposites for Aerospace Applications
by Beatriz Monteiro and Sónia Simões
Metals 2024, 14(11), 1283; https://doi.org/10.3390/met14111283 - 12 Nov 2024
Viewed by 1184
Abstract
Hybrid nanocomposites have emerged as a groundbreaking class of materials in the aerospace industry, offering exceptional mechanical, thermal, and functional properties. These materials, composed of a combination of metallic matrices (based on aluminum, magnesium, or titanium) reinforced with a mixture of nanoscale particles, [...] Read more.
Hybrid nanocomposites have emerged as a groundbreaking class of materials in the aerospace industry, offering exceptional mechanical, thermal, and functional properties. These materials, composed of a combination of metallic matrices (based on aluminum, magnesium, or titanium) reinforced with a mixture of nanoscale particles, such as carbon nanotubes (CNTs), graphene, and ceramic nanoparticles (SiC, Al2O3), provide a unique balance of high strength, low weight, and enhanced durability. Recent advances in developing these nanocomposites have focused on optimizing the dispersion and integration of nanoparticles within the matrix to achieve superior material performance. Innovative fabrication techniques have ensured uniform distribution and strong bonding between the matrix and the reinforcements, including advanced powder metallurgy, stir casting, in situ chemical vapor deposition (CVD), and additive manufacturing. These methods have enabled the production of hybrid nanocomposites with improved mechanical properties, such as increased tensile strength, fracture toughness, wear resistance, and enhanced thermal stability and electrical conductivity. Despite these advancements, challenges remain in preventing nanoparticle agglomeration due to the high surface energy and van der Walls forces and ensuring consistent quality and repeatability in large-scale production. Addressing these issues is critical for fully leveraging the potential of hybrid nanocomposites in aerospace applications, where materials are subjected to extreme conditions and rigorous performance standards. Ongoing research is focused on developing novel processing techniques and understanding the underlying mechanisms that govern the behavior of these materials under various operational conditions. This review highlights the recent progress in the design, fabrication, and application of hybrid nanocomposites for aerospace applications. It underscores their potential to revolutionize the industry by providing materials that meet the demanding requirements for lightweight, high-strength, and multifunctional components. Full article
(This article belongs to the Section Metal Matrix Composites)
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<p>Percentage of the materials used in some Boeing aircraft. Adapted from [<a href="#B1-metals-14-01283" class="html-bibr">1</a>].</p>
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<p>Representative diagram showing the parts of the aircraft constructions that required composite materials.</p>
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<p>Representation of the reinforcements that can be combined to produce hybrid nanocomposites.</p>
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<p>Schematic representation of the sequential steps of powder metallurgy route producing of Al hybrid nanocomposites.</p>
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<p>Unique color and Kernel average misorientation maps of (<b>a</b>,<b>b</b>) Al6061 matrix and (<b>c</b>,<b>d</b>) Al6061/CNTs/SiC hybrid nanocomposite produced by powder metallurgy and (<b>e</b>) hardness and tensile strength of the matrix and nanocomposite produced under the same conditions.</p>
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<p>SEM image of the nanocomposites produced by (<b>a</b>,<b>b</b>) conventional sintering reinforced with ZrC and B<sub>4</sub>C and (<b>c</b>) high magnification showing by arrows the ZrC agglomerates. Reprinted with permission from ref. [<a href="#B29-metals-14-01283" class="html-bibr">29</a>]. 2021 Elsevier.</p>
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<p>Scanning transmission electron microscopy (STEM) images of the Al hybrid nanocomposites: (<b>a</b>) bright-field, (<b>b</b>) dark-field images; (<b>c</b>,<b>d</b>) STEM images with the EDS regions marked; (<b>e</b>,<b>f</b>) TEM images showing regions with different grain size; and (<b>g</b>) STEM image with EDS mapping. Reprinted with permission from ref. [<a href="#B53-metals-14-01283" class="html-bibr">53</a>]. 2022 Elsevier.</p>
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<p>Schematic drawing of the conventional chemical vapor deposition (CVD).</p>
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<p>The schematic draw of the selective laser melting (SLM) process.</p>
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<p>Polarized images of (<b>a</b>) nanocomposites produced at 1200 rpm, (<b>b</b>) nanocomposites produced at 1300 rpm, (<b>c</b>) nanocomposites produced at 1400 rpm, (<b>d</b>) nanocomposites produced at 1500 rpm, and (<b>e</b>) matrix produced at 1200 rpm. Reprinted from Ref. [<a href="#B76-metals-14-01283" class="html-bibr">76</a>].</p>
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<p>Images of the nanocomposites produced using different processing conditions (<b>a</b>–<b>d</b>) 900 rpm; (<b>e</b>–<b>h</b>) 1250 rpm; (<b>i</b>–<b>l</b>) 1600 rpm and (<b>m</b>–<b>p</b>) consumable rod and AMDO NC900-12. Reprinted from Ref. [<a href="#B77-metals-14-01283" class="html-bibr">77</a>].</p>
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<p>Optical microscopy images of (<b>a</b>) AA5083-H321 consumed rod, (<b>b</b>) interface region between the AA5083 rod/substrate, (<b>c</b>) TMAZ of the deposited sample using 1600 rpm with 12 mm/min Reprinted from Ref. [<a href="#B78-metals-14-01283" class="html-bibr">78</a>].</p>
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<p>Schematic drawing of the conventional stir casting process.</p>
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<p>(<b>a</b>) Hardness and (<b>b</b>) wear rate of Al matrix and nanocomposites produced by stir casting. Reprinted from Ref. [<a href="#B80-metals-14-01283" class="html-bibr">80</a>].</p>
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<p>The yield strength (YS), elongation, and ultimate tensile strength (UTS) of the matrix of different nanocomposites. Reprinted from Ref. [<a href="#B85-metals-14-01283" class="html-bibr">85</a>].</p>
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<p>Comparison of mechanical properties and density between hybrid nanocomposites and metallic and ceramic materials: (<b>a</b>) relation between density and tensile strength and (<b>b</b>) relation between the fracture toughness with tensile strength. Graphs drawn based on data using Ansys Granta EduPack software R4.</p>
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13 pages, 7540 KiB  
Article
The Effect of Heat Treatment on the Sol–Gel Preparation of TiO2/ZnO Catalysts and Their Testing in the Photodegradation of Tartrazine
by Nina Kaneva and Albena Bachvarova-Nedelcheva
Appl. Sci. 2024, 14(21), 9872; https://doi.org/10.3390/app14219872 - 29 Oct 2024
Viewed by 630
Abstract
This study aims to synthesize TiO2/ZnO powders and to study the effect of heat treatment on their photocatalytic ability against the Tartrazine anionic dye. The as-obtained powders with the following compositions—90TiO2/10ZnO and 10TiO2/90ZnO (mol%)—were obtained by the [...] Read more.
This study aims to synthesize TiO2/ZnO powders and to study the effect of heat treatment on their photocatalytic ability against the Tartrazine anionic dye. The as-obtained powders with the following compositions—90TiO2/10ZnO and 10TiO2/90ZnO (mol%)—were obtained by the sol–gel technique. The prepared gels were annealed at 500 °C and 700 °C and subsequently characterized by XRD, UV–Vis, and SEM methods. The single crystalline phase of TiO2, which has been detected at up to 500 °C is anatase, while for ZnO, it is the hexagonal wurtzite structure. Further increases in the temperature (700 °C) led to the appearance of rutile in the samples. The SEM analysis demonstrated that the binary oxide materials had irregular shaped particles with a tendency to agglomerate. The UV–Vis spectra of the gels exhibited a red shift in the cut-off of the 90TiO2/10ZnO sample compared with pure Ti(IV) butoxide. Photocatalytic tests showed that the investigated samples possessed photocatalytic activity toward Tartrazine. Compared with TiO2, the prepared TiO2/ZnO photocatalysts showed superior properties in the photodegradation of a Tartrazine water solution. The target photocatalysts’ enhanced photocatalytic activities can be explained by their reduced band gap energy, improved surface physicochemical characteristics, separation of photo-induced electron–hole pairs, and lowered recombination rate. Higher photocatalytic activity was observed for powders annealed at 500 °C, with the 10TiO2/90ZnO (mol%) sample exhibiting the highest photocatalytic degradation of the used organic dye. Full article
(This article belongs to the Special Issue Environmental Catalysis and Green Chemistry)
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<p>X-ray phase analysis of the samples annealed at 500 °C (<b>a</b>) and 700 °C (<b>b</b>).</p>
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<p>SEM images of the samples annealed at 500 °C: TiO<sub>2</sub> (<b>a</b>), 90TiO<sub>2</sub>/10ZnO (<b>b</b>), and 10TiO<sub>2</sub>/90ZnO (<b>c</b>). SEM images of the samples annealed at 700 °C: TiO<sub>2</sub> (<b>d</b>), 90TiO<sub>2</sub>/10ZnO (<b>e</b>) and 10TiO<sub>2</sub>/90ZnO (<b>f</b>).</p>
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<p>EDS spectra of TiO<sub>2</sub> (<b>a</b>), 90TiO<sub>2</sub>/10ZnO (<b>b</b>), and 10TiO<sub>2</sub>/90ZnO (<b>c</b>) catalysts.</p>
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<p>UV–visible spectra of the investigated gels.</p>
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<p>Photocatalytic decomposition percent (<b>a</b>) and rate constants (<b>b</b>) of Tartrazine using pure TiO<sub>2</sub> and TiO<sub>2</sub>/ZnO powders annealed at 500 °C.</p>
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<p>A probable mechanism for the enhanced property of TiO<sub>2</sub>/ZnO catalysts to e Tartrazine. Mechanism adapted with permission from Ref. [<a href="#B36-applsci-14-09872" class="html-bibr">36</a>].</p>
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<p>Photocatalytic decomposition percent (<b>a</b>) and rate constants (<b>b</b>) of Tartrazine using pure TiO<sub>2</sub> and TiO<sub>2</sub>/ZnO powders annealed at 700 °C.</p>
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<p>Photocatalytic degradation rate of Tartrazine for three consecutive cycles using powders annealed at 500 °C (<b>a</b>) and 700 °C (<b>b</b>).</p>
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21 pages, 19685 KiB  
Article
Production and Characterization of Hybrid Al6061 Nanocomposites
by Beatriz Monteiro and Sónia Simões
Metals 2024, 14(11), 1206; https://doi.org/10.3390/met14111206 - 23 Oct 2024
Viewed by 2731
Abstract
Aluminum-based hybrid nanocomposites, namely the Al6061 alloy, have gained prominence in the scientific community due to their unique properties, such as high strength, low density, and good corrosion resistance. The production of these nanocomposites involves incorporating reinforcing nanoparticles into the matrix to improve [...] Read more.
Aluminum-based hybrid nanocomposites, namely the Al6061 alloy, have gained prominence in the scientific community due to their unique properties, such as high strength, low density, and good corrosion resistance. The production of these nanocomposites involves incorporating reinforcing nanoparticles into the matrix to improve its mechanical and thermal properties. The Al6061 hybrid nanocomposites were manufactured by conventional powder metallurgy (cold pressing and sintering). Ceramic silicon carbide (SiC) nanoparticles and carbon nanotubes (CNTs) were used as reinforcements. The nanocomposites were produced using different reinforcement amounts (0.50, 0.75, 1.00, and 1.50 wt.%) and sintered from 540 to 620 °C for 120 min. The characterization of the Al6061 hybrid nanocomposites involved the analysis of their mechanical properties, such as hardness and tensile strength, as well as their micro- and nanometric structures. Techniques such as optical microscopy (OM) and scanning electron microscopy (SEM) with electron backscatter diffraction (EBSD) were used to study the distribution of nanoparticles, the grain size of the microstructure, and the presence of defects in the matrix. The microstructural evaluation revealed significant grain refinement and greater homogeneity in the hybrid nanocomposites reinforced with 0.75 wt.% of SiC and CNTs, resulting in better mechanical performance. Tensile tests showed that the Al6061/CNT/SiC hybrid composite had the highest tensile strength of 104 MPa, compared to 63 MPa for the unreinforced Al6061 matrix. The results showed that adding 0.75% SiC nanoparticles and CNTs can significantly improve the properties of Al6061 (65% in the tensile strength). However, some nanoparticle agglomeration remains one of the challenges in manufacturing these nanocomposites; therefore, the expected increase in mechanical properties is not observed. Full article
(This article belongs to the Special Issue Design and Development of Metal Matrix Composites)
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<p>Schematic representation of the hybrid nanocomposite production process via powder metallurgy.</p>
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<p>Schematic representation of the hardness indentation on polished cross-sections of the nanocomposites.</p>
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<p>Scanning electron microscopy (SEM) image in secondary electron mode of the Al6061 as-received powders.</p>
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<p>EBSD results of an Al6061 powder particle (<b>a</b>) unique grain color map, (<b>b</b>) inverse pole figure map, (<b>c</b>) Kernel average misorientation map, and (<b>d</b>) image quality map with grain boundaries delimitated.</p>
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<p>A high-resolution (HRTEM) image of an MWCNT shows a magnification of a region of the layers where we can see the image and measure the number of walls.</p>
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<p>SEM image of the as-received SiC nanoparticles used as reinforcement material.</p>
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<p>Evolution of hardness (HV0.2) of the nanocomposites with the different amounts of the reinforcement. The hardness of the Al6061 matrix is also shown for comparison purposes.</p>
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<p>SEM images of the nanocomposites reinforced with SiC with (<b>a</b>) 0.50%, (<b>b</b>) 0.75%, and (<b>c</b>) 1.00% wt.</p>
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<p>SEM images of the nanocomposites of the SiC reinforced with (<b>a</b>) 0.50 wt.%, (<b>b</b>) 0.75 wt.%, (<b>c</b>) 1.00 wt.%, and (<b>d</b>) 1.50 wt.%.</p>
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<p>SEM image of Al6061 nanocomposites with the EDS analyzed regions marked and present in <a href="#metals-14-01206-t004" class="html-table">Table 4</a>.</p>
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<p>(<b>a</b>) SEM image of Al6061 matrix and EDS elemental distribution map of (<b>b</b>) Al, (<b>c</b>) Mg, (<b>d</b>) Si, and (<b>e</b>) Fe.</p>
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<p>The density of the Al6061 matrix and Al6061 reinforced with CNTs, SiC, and SiC/CNTs for the different sintered temperatures.</p>
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<p>(<b>a</b>) Low magnification SEM image of Al6061/SiC/CNTs produced at 580 °C, (<b>b</b>) higher magnification SEM images, and (<b>c</b>) EDS elemental distribution map of Al, Fe, Mg, C, O, Si, and Cu.</p>
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<p>Unique grain color map of (<b>a</b>) Al6061 matrix, (<b>b</b>) Al6061/CNTs, (<b>c</b>) Al6061/SiC, and (<b>d</b>) Al6061/SiC/CNTs.</p>
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<p>Inverse pole figures (IPF) maps and IPF figures of (<b>a</b>,<b>b</b>) Al6061 matrix, (<b>c</b>,<b>d</b>) Al6061/CNTs, (<b>e</b>,<b>f</b>) Al6061/SiC, and (<b>g</b>,<b>h</b>) Al6061/SiC/CNTs.</p>
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<p>KAM maps of (<b>a</b>) Al6061 matrix, (<b>b</b>) Al6061/CNTs, (<b>c</b>) Al6061/SiC, (<b>d</b>) Al6061/SiC/CNTs, and (<b>e</b>) distribution of KAM misorientation angle for all samples.</p>
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<p>The evolution of hardness of the Al6061 matrix and Al6061 reinforced with CNTs, SiC, and SiC/CNTs for the different sintered temperatures.</p>
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14 pages, 9406 KiB  
Article
Erosion Wear Behavior of HVAF-Sprayed WC/Cr3C2-Based Cermet and Martensitic Stainless Steel Coatings on AlSi7Mg0.3 Alloy: A Comparative Study
by Yury Korobov, Maksim Antonov, Vladimir Astafiev, Irina Brodova, Vladimir Kutaev, Svetlana Estemirova, Mikhail Devyatyarov and Artem Okulov
J. Manuf. Mater. Process. 2024, 8(5), 231; https://doi.org/10.3390/jmmp8050231 - 14 Oct 2024
Viewed by 1185
Abstract
The paper presents a comparative study of the erosion wear resistance of WC-10Co4Cr, Cr3C2-25NiCr and martensitic stainless steel (SS) coatings deposited onto an AlSi7Mg0.3 (Al) alloy substrate by high-velocity air‒fuel (HVAF) spraying. The influence of the abrasive type (quartz [...] Read more.
The paper presents a comparative study of the erosion wear resistance of WC-10Co4Cr, Cr3C2-25NiCr and martensitic stainless steel (SS) coatings deposited onto an AlSi7Mg0.3 (Al) alloy substrate by high-velocity air‒fuel (HVAF) spraying. The influence of the abrasive type (quartz sand or granite gravel), erodent attack angle, thickness, and microhardness of the coatings on their and Al substrate’s wear resistance was comprehensively investigated under dry erosion conditions typical for fan blades. The HVAF-spraying process did not affect the Al substrate’s structure, except for when the near-surface layer was 20‒40 μm thick. This was attributed to the formation of a modified Al-Si eutectic with enhanced microhardness and strength in the near-substrate area. Mechanical characterization revealed significantly higher microhardness values for the cermet WC-10Co4Cr (~12 GPa) and Cr3C2-25NiCr (~9 GPa) coatings, while for the SS coating, the value was ~5.7 GPa. Erosion wear tests established that while Cr3C2-25NiCr and SS coatings were more sensitive to abrasive type, the WC-10Co4Cr coating exhibited significantly higher wear resistance, outperforming the alternatives by 2‒17 times under high abrasive intensity. These findings highlight the potential of HVAF-sprayed WC-10Co4Cr coatings for extending the service life of AlSi7Mg0.3-based fan blades exposed to erosion wear at normal temperatures. Full article
(This article belongs to the Special Issue Deformation and Mechanical Behavior of Metals and Alloys)
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<p>Schematic illustration of the HVAF-spraying process and a general view of the feedstock powders: (<b>a</b>) WC-10Co4Cr, (<b>b</b>) Cr<sub>3</sub>C<sub>2</sub>-25NiCr, and (<b>c</b>) SS.</p>
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<p>(<b>a</b>) Schematic illustration of the erosion wear tester and (<b>b</b>) general view of the samples on a fixing mandrel (before and after wear tests (enlarged image)).</p>
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<p>Optical- and SEM-based microstructural features of the HVAF-sprayed (<b>a</b>–<b>c</b>) WC-10Co4Cr (splashing of the WC-10Co4Cr particles (<b>I</b>) on the coating surface and (<b>II</b>) inside the near-interface areas), (<b>d</b>–<b>f</b>) Cr<sub>3</sub>C<sub>2</sub>-25NiCr, and (<b>g</b>,<b>h</b>) SS coatings, and (<b>i</b>) their microhardness graph before erosion wear tests.</p>
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<p>X-ray diffraction patterns and bar diagrams of standards: (<b>a</b>) WC-10Co4Cr and (<b>b</b>) Cr<sub>3</sub>C<sub>2</sub>-25NiCr.</p>
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<p>SEM-based microstructure of the AlSi7Mg0.3, SS, Cr<sub>3</sub>C<sub>2</sub>-25NiCr, and WC-10Co4Cr coatings after wear tests with (<b>a</b>,<b>c</b>,<b>e</b>,<b>g</b>) quartz sand and (<b>b</b>,<b>d</b>,<b>f</b>,<b>h</b>) granite gravel, and (<b>i</b>) volumetric wear test graphs.</p>
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<p>Optical images of the WC-10Co4Cr coatings (top view) with various thicknesses: (<b>a</b>) 50 μm, (<b>b</b>) 100 μm, and (<b>c</b>) 200 μm; and (<b>d</b>) their relative wear resistance after wear tests with quartz sand.</p>
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20 pages, 9148 KiB  
Article
On the Role of Substrate in Hydroxyapatite Coating Formation by Cold Spray
by John Henao, Astrid Giraldo-Betancur, Carlos A. Poblano-Salas, Diego German Espinosa-Arbelaez, Jorge Corona-Castuera, Paola Andrea Forero-Sossa and Rene Diaz-Rebollar
Coatings 2024, 14(10), 1302; https://doi.org/10.3390/coatings14101302 - 12 Oct 2024
Cited by 1 | Viewed by 970
Abstract
The deposition of agglomerated hydroxyapatite (HAp) powders by low-pressure cold spray has been a topic of interest in recent years. Key parameters influencing the deposition of HAp powders include particle morphology and impact kinetic energy. This work examines the deposition of HAp powders [...] Read more.
The deposition of agglomerated hydroxyapatite (HAp) powders by low-pressure cold spray has been a topic of interest in recent years. Key parameters influencing the deposition of HAp powders include particle morphology and impact kinetic energy. This work examines the deposition of HAp powders on various metal surfaces to assess the impact of substrate properties on the formation of HAp deposits via cold spray. The substrates studied here encompass metals with varying hardness and thermal conductivities, including Al6061, Inconel alloy 625, AISI 316 stainless steel, H13 tool steel, Ti6Al4V, and AZ31 alloy. Single-track experiments offer insights into the initial interactions between HAp particles and different substrate surfaces. In this study, the results indicate that the ductility of the substrate may enhance HAp particle deposition only at the first deposition stages where substrate/particle interaction is the most critical factor for deposition. Features on the substrate associated with the first deposition sprayed layer include localized substrate deformation and the formation of clusters of HAp agglomerates, which aid in HAp deposition. Furthermore, after multiple spraying passes on the various metallic surfaces, deposition efficiency was significantly reduced when the build-up process of HAp coatings shifted from ceramic/metal to ceramic/ceramic interactions. Overall, this study achieved agglomerated HAp deposits with high deposition efficiencies (30–60%) through single-track experiments and resulted in the preparation of HAp coatings on various substrates with thickness values ranging from 24 to 53 µm. These coatings exhibited bioactive behavior in simulated body fluid. Full article
(This article belongs to the Special Issue Development of Hydroxyapatite Coatings)
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<p>SEM images from HAp powder used in this study.</p>
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<p>Properties of the metallic substrates in this study. (<b>a</b>) Experimental values of Vickers hardness taken with a 300 g load for 15 s. Insets at the bottom of bars display the prints obtained from each substrate. (<b>b</b>) Thermal conductivity of the substrates obtained from [<a href="#B38-coatings-14-01302" class="html-bibr">38</a>].</p>
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<p>Percentage area of deposited HAp particles versus deposition efficiency for spraying conditions M1 to M7 on the different substrates. Each substrate is represented with a different color, whereas each condition is identified with a different symbol. The dashed lines in the graph serve as a visual guide for the two linear regions.</p>
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<p>Optical micrographs from the top view of the HAp tracks related to the spraying conditions of HAp listed in <a href="#coatings-14-01302-t001" class="html-table">Table 1</a>, 40× magnification. The dashed line in the graph serves as a visual guide to separate samples M1 to M3, which were fabricated under the same spraying conditions but with different preheating temperatures (25 °C, 100 °C, and 200 °C).</p>
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<p>SEM images of tracks prepared with the M1 spraying condition: (<b>a</b>) Ti64, (<b>b</b>) SS316, (<b>c</b>) H13, (<b>d</b>) Inc625, (<b>e</b>) AZ31, and (<b>f</b>) Al6061. The blue arrows in the images serve as a visual guide to highlight the areas of plastic deformation in the substrates caused by the impact and rebound of the HAp particles.</p>
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<p>SEM images of tracks prepared with the M4 spraying condition: (<b>a</b>) Ti64, (<b>b</b>) SS316, (<b>c</b>) H13, and (<b>d</b>) Inc625. Dashed lines in Figure (<b>a</b>) illustrate the cone-like morphology of deposited HAp particles.</p>
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<p>SEM images of tracks prepared with the M4 spraying condition: (<b>a</b>,<b>b</b>) AZ31; (<b>c</b>,<b>d</b>) Al6061.</p>
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<p>Deposition efficiency of deposited HAp particles under single-track experiments versus (<b>a</b>) substrate hardness, (<b>b</b>) yield stress ratio of the substrates(Ystress at 200 °C/Ystress at 25 °C). Dashed lines are used as visual guides to show tendencies.</p>
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<p>Energy-based deposition window for the cold-sprayed HAp powder in this study. (<b>a</b>) Energy ratio as a function of velocity and particle diameter, including the hardness values of the substrates represented by the dashed lines. (<b>b</b>) Energy ratio as a function of velocity and particle diameter, highlighting in the gray area the effect of the substrate temperature on the deposition efficiency values.</p>
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<p>Images of cold-sprayed HAp coatings prepared using the M4 spraying condition with preheating at 200 °C: (<b>a</b>) evidence of delamination; (<b>b</b>) temperature history of the substrates during spraying.</p>
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<p>(<b>a</b>) Deposition efficiency and (<b>b</b>) average thickness of HAp coatings as a function of the number of spraying passes. Data correspond to the spraying conditions outlined in <a href="#coatings-14-01302-t002" class="html-table">Table 2</a>.</p>
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<p>Optical micrographs of the top surface of cold-sprayed hydroxyapatite (HAp) coatings deposited on the metallic substrates under the conditions specified in <a href="#coatings-14-01302-t002" class="html-table">Table 2</a>. The R1, R4, and R5 designations correspond to 5, 24, and 36 spraying passes, respectively.</p>
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<p>SEM images of the cross-section of cold-sprayed HAp coatings after 36 spraying passes under condition R5, deposited on: (<b>a</b>) AZ31, (<b>b</b>) Al6061, (<b>c</b>) Ti64, (<b>d</b>) SS316, (<b>e</b>) H13, and (<b>f</b>) Inc625; (<b>g</b>) HAp coatings thickness.</p>
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<p>XRD analysis results: (<b>a</b>) Characteristic diffraction patterns of cold-sprayed HAp coatings on the metallic substrates compared to the feedstock powder; (<b>b</b>) diffraction patterns of the HAp coatings after 14 days of immersion in Kokubo’s solution at 37 °C (* represents the substrate contribution in each sample after SBF soaking time. The vertical dashed lines at the bottom represent the reference patterns that indicate the positions of the HAp peaks).</p>
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<p>SEM images of the top surface of cold-sprayed HAp coatings on various metallic substrates after 14 days of immersion in Kokubo’s solution at 37 °C: (<b>a</b>) AZ31, (<b>b</b>) Al6061, (<b>c</b>) Ti64, (<b>d</b>) SS316, (<b>e</b>) H13, and (<b>f</b>) Inc625. The inset in (<b>b</b>) provides a closer view of the surface, while the inset in (<b>e</b>) shows a region where the apatite layer was not formed.</p>
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28 pages, 6905 KiB  
Article
Corrosion Behaviour of Heat-Treated Cold Spray Nickel Chromium/Chromium Carbides
by Cedric Tan, Kannoorpatti Krishnan and Naveen Kumar Elumalai
Metals 2024, 14(10), 1153; https://doi.org/10.3390/met14101153 - 10 Oct 2024
Viewed by 714
Abstract
Chromium carbide powder agglomerated with nickel/chrome was deposited using a cold spray process onto a mild steel substrate. The deposits were heat-treated at 650 °C and 950 °C in ambient conditions to reduce porosity and improve adhesion between powder particles. The corrosion behaviour [...] Read more.
Chromium carbide powder agglomerated with nickel/chrome was deposited using a cold spray process onto a mild steel substrate. The deposits were heat-treated at 650 °C and 950 °C in ambient conditions to reduce porosity and improve adhesion between powder particles. The corrosion behaviour of these cold-sprayed materials was studied in artificial seawater conditions using electrochemical techniques. Heat treatment at 650 °C was found to best improve corrosion resistance, while the 950 °C treatment performed better than the as-sprayed condition but lower than the 650 °C sample. Microstructural analysis revealed complex phase transformations and structural refinements with increasing heat treatment temperature. The crystallite size of both Cr3C2 and NiCr phases decreased, while microstrain and dislocation density increased due to heat treatment. The formation of and subsequent reduction in Cr23C6 content indicated a complex sequence of carbide dissolution, transformation, and precipitation processes. The 650 °C heat-treated sample demonstrated superior corrosion resistance, evidenced by the highest corrosion potential, lowest passive current, and largest charge transfer resistance. This enhanced performance was attributed to the formation of a more stable and protective passive film, optimal carbide dissolution, and a homogeneous microstructure. Meanwhile, the 950 °C treatment led to excessive carbide dissolution and formed increased interfaces between the carbide and matrix. Mechanical property changes were also observed, with carbide hardness significantly decreasing after corrosion testing. These findings highlight the critical role of controlled heat treatment in optimising the performance of cold-sprayed Cr3C2-NiCr coatings, demonstrating that achieving superior corrosion resistance requires a delicate balance between microstructural refinement, phase transformations, and preservation of coating integrity. Full article
(This article belongs to the Special Issue Recent Advances in Corrosion and Protection of Metallic Materials)
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<p>Microstructure of Sample A (non-heat-treated) showing primary carbides surrounded by NiCr matrix as well as voids for (<b>a</b>) SEM at lower magnification, (<b>b</b>) SEM at higher magnification, and (<b>c</b>) optical microscopy.</p>
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<p>Microstructure of Sample B heat-treated at 650 °C for (<b>a</b>) SEM at lower magnification, (<b>b</b>) SEM at higher magnification, and (<b>c</b>) optical microscopy.</p>
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<p>Microstructure of Sample C heat-treated at 950 °C for (<b>a</b>) SEM at lower magnification, (<b>b</b>) SEM at higher magnification, and (<b>c</b>) optical microscopy.</p>
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<p>SEM-EDS surface indicating locations of matrix and carbide analysis, with example at 950 °C.</p>
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<p>XRD for 2θ = 40–90°: (<b>a</b>) noHT Sample A, (<b>b</b>) 650HT Sample B, and (<b>c</b>) 950HT Sample C.</p>
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<p>XRD for 2θ = 35–55°: (<b>a</b>) noHT Sample A, (<b>b</b>) 650HT Sample B, and (<b>c</b>) 950HT Sample C.</p>
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<p>Crystallite sizes of Cr<sub>3</sub>C<sub>2</sub> and NiCr.</p>
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<p>Microstrain values of Cr<sub>3</sub>C<sub>2</sub> and NiCr.</p>
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<p>Dislocation densities of Cr<sub>3</sub>C<sub>2</sub> and NiCr.</p>
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<p>EIS Nyquist plot for Samples A, B, and C.</p>
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<p>Bode plots: (<b>a</b>) phase vs. freq and (<b>b</b>) Mod Z vs. freq.</p>
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<p>Equivalent circuit model for the coating system.</p>
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<p>Potentiodynamic curves for Samples A, B, and C.</p>
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<p>Optical microscopy for the noHT Sample A’s potentiostatic point at 45 mV.</p>
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<p>Optical microscopy for the noHT Sample A’s potentiostatic point at 2000 mV.</p>
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<p>Optical microscopy for the 650HT Sample B’s potentiostatic point at 2000 mV.</p>
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<p>Optical microscopy for the 950HT Sample C’s potentiostatic point at 2000 mV.</p>
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<p>Hardness tests for 950HT Sample C (<b>a</b>) before indentation and (<b>b</b>) after indentation. Also note the following features: 1. carbides, 2. collapse of carbide around the indentation, and 3. the square indentation itself.</p>
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<p>Complete removal of carbide post-indentation, as shown surrounded by green box.</p>
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<p>Illustrated microstructural changes with heat treatment.</p>
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24 pages, 17126 KiB  
Article
Characteristics of a Spray-Dried Porcine Blood Meal for Aedes aegypti Mosquitoes
by Alexander R. Weaver, Nagarajan R. Rajagopal, Roberto M. Pereira, Philip G. Koehler, Andrew J. MacIntosh, Rebecca W. Baldwin and Christopher D. Batich
Insects 2024, 15(9), 716; https://doi.org/10.3390/insects15090716 - 19 Sep 2024
Viewed by 906
Abstract
Research into mosquito-borne illnesses faces hurdles because feeding fresh animal blood to rear female mosquitoes presents logistical, economic, and safety challenges. In this study, a shelf-stable additive (spray-dried porcine blood; SDPB) hypothesized to supply accessible hemoglobin was evaluated within an alternative meal (AM) [...] Read more.
Research into mosquito-borne illnesses faces hurdles because feeding fresh animal blood to rear female mosquitoes presents logistical, economic, and safety challenges. In this study, a shelf-stable additive (spray-dried porcine blood; SDPB) hypothesized to supply accessible hemoglobin was evaluated within an alternative meal (AM) containing whey powder and PBS for rearing the yellow fever mosquito Aedes aegypti. LC–MS/MS proteomics, microbial assays, and particle reduction techniques confirmed and characterized the functionality of hemoglobin in SDPB, while engorgement, fecundity, egg viability, and meal stability bioassays assessed AM performance. Chemical assays supported hemoglobin as the phagostimulant in SDPB with aggregates partially solubilized in the AM that can be more accessible via particle reduction. Unpaired two-tailed t-tests indicate that the AM stimulates oogenesis (t11 = 13.6, p = 0.003) and is stable under ambient (1+ y; t12 = 0.576, p = 0.575) and aqueous (14 d; t12 = 0.515, p = 0.639) conditions without decreasing fecundity. Egg hatch rates for the ninth generation of AM-reared Ae. aegypti were 50–70+%. With further development, this meal may serve as a platform for mass rearing or studying effects of nutritional additives on mosquito fitness due to its low cost and stability. Future work may examine tuning spray drying parameters and resulting impacts on hemoglobin agglomeration and feeding. Full article
(This article belongs to the Section Insect Pest and Vector Management)
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<p>Aqueous preparations of (<b>a</b>) the simple AM with unground SDPB after complete segregation, (<b>b</b>) the simple AM after complete segregation, and (<b>c</b>) espresso-ground SDPB (<b>left</b>) and unground SDPB (<b>right</b>) upon sitting for several minutes.</p>
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<p>Light microscopy of unground SDPB visualized on Neubauer hemocytometer slides at scale lengths of (<b>a</b>) 0.1 mm and (<b>b</b>) 0.05 mm.</p>
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<p>Preparations of SDPB imaged via 5 kV SEM. Subfigures represent SDPB (<b>a</b>) unground, (<b>b</b>) coffee-ground, (<b>c</b>) espresso-ground, and (<b>d</b>) espresso-ground and sieved through a 63 µm wire mesh. Green lines in subfigures (<b>a</b>–<b>c</b>) represent digitally generated particle diameters. Scale lengths of 500 µm or 100 µm are represented by a red bar in each subfigure.</p>
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<p>Preparation of whey powder (<b>a</b>) imaged via 5 kV SEM and (<b>b</b>) box-and-whisker plots of measured particle diameters of SDPB in <a href="#insects-15-00716-f003" class="html-fig">Figure 3</a>a–c and the whey preparation. Green lines in subfigure (<b>a</b>) represent digitally generated particle diameters. A minimum of ten particle diameters were estimated at random for each condition. Error bars represent standard deviation.</p>
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<p>Cumulative particle distribution measurements gathered for (<b>A</b>) whey powder, (<b>B</b>) coffee-ground SDPB, and (<b>C</b>) unground SDPB via laser diffraction.</p>
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<p>Graphs of LC–MS/MS SDPB and whey protein spectral matches (<b>a</b>) by sequence molecular weight and (<b>b</b>) for ten proteins of high alignment between all conditions. Proteins included within this subset were (A) filamin A, (B) albumin (bovine or porcine), (C) protease 1, (D) ubiquitin C, (E) apolipoprotein A-1, (F) β-lactoglobulin, (G) α-lactoglobulin, (H) hemoglobin subunit beta, (I) hemoglobin fetal subunit beta, and (J) hemoglobin subunit alpha.</p>
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<p>Contamination assay of (A) boiled water and aqueous preparations of (B) autoclaved SDPB, (C) “raw” SDPB, and (D) EC-1118 <span class="html-italic">S. cerevisiae</span>, showing (<b>a</b>) ATP luminescence measurements and (<b>b</b>) agar culture plates. Asterisks indicate significant differences in engorgement between the denoted meals (UTT; ** for <span class="html-italic">p</span> &lt; 0.01). Error bars represent standard deviation.</p>
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<p>Aqueous culture and feeding of the simple AM after (A) 0 h and (B) 2 h, autoclaved SDPB after (C) 0 h and (D) 2 h, and the simple AM with autoclaved SDPB after (E) 0 h and (F) 2 h. Subfigures show (<b>a</b>) ATP luminescence measurements and (<b>b</b>) fecundity of the simple AM and the AM containing SDPB autoclaved at 121 °C for 1 h. Asterisks indicate significant differences in engorgement between the denoted meals (UTT; * for <span class="html-italic">p</span> &lt; 0.05, ** for <span class="html-italic">p</span> &lt; 0.01, **** for <span class="html-italic">p</span> &lt; 0.0001). Error bars represent standard deviation in (<b>a</b>) and standard error in (<b>b</b>).</p>
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<p>Feeding of AMs containing ball-milled SDPB with fecundity of the simple AM (A/C) and AMs containing SDPB ball-milled for 72 h (B) and 96 h (D). Asterisks indicate significant differences in engorgement between the denoted meals (UTT; ** for <span class="html-italic">p</span> &lt; 0.01). Error bars represent standard error.</p>
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<p>Engorgement of individual mosquitos with (<b>a</b>) mass measurements of engorgement on fresh bovine blood, the simple AM, 20% SDPB (<span class="html-italic">w</span>/<span class="html-italic">v</span>) in PBS, and 10% whey (<span class="html-italic">w</span>/<span class="html-italic">v</span>) in PBS and (<b>b</b>) female <span class="html-italic">Ae. aegypti</span> fully engorged on SDPB. Asterisks indicate significant differences in engorgement between the denoted meals (ANOVA; * for <span class="html-italic">p</span> &lt; 0.05). Error bars represent standard error.</p>
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<p>Fecundity of fresh bovine blood, the simple AM, and 10% whey in PBS meals. Asterisks indicate significant differences in engorgement between the denoted meals (UTT; ** for <span class="html-italic">p</span> &lt; 0.01). Error bars represent standard error.</p>
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<p>Fecundity and egg viability evaluations of <span class="html-italic">Ae. aegypti</span> reared exclusively on the AM. Subfigure (<b>a</b>) shows ratios of six generations of an <span class="html-italic">Ae. aegypti</span> colony exclusively fed the simple AM. The ratio represents AM-colony egg fecundity relative to the fecundity of a fresh-blood-fed sister colony. Subfigure (<b>b</b>) shows larval and pupal hatch ratios relative to the number of eggs aliquoted for hatching. Data from clutches (A) and (B) are grouped by day post-hatch. Error bars represent standard error.</p>
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<p>Fecundity of fresh blood and simple AM meals when fed immediately (0 d) and 14 d post-collection for fresh blood or post-preparation for the AM. Error bars represent standard error.</p>
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<p>Fecundity data obtained from feeding the simple AM with the dry and sealed formulation not aged, aged, or aged with an N<sub>2</sub> blanket. Error bars represent standard error.</p>
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16 pages, 22326 KiB  
Article
An Advanced Surface Treatment Technique for Coating Three-Dimensional-Printed Polyamide 12 by Hydroxyapatite
by Abdulaziz Alhotan, Saleh Alhijji, Sahar Ahmed Abdalbary, Rania E. Bayoumi, Jukka P. Matinlinna, Tamer M. Hamdy and Rasha M. Abdelraouf
Coatings 2024, 14(9), 1181; https://doi.org/10.3390/coatings14091181 - 12 Sep 2024
Cited by 1 | Viewed by 1050
Abstract
Polymer 3D printing has is used in a wide range of applications in the medical field. Polyamide 12 (PA12) is a versatile synthetic polymer that has been used to reconstruct bony defects. Coating its surface with calcium phosphate compounds, such as hydroxyapatite (HA), [...] Read more.
Polymer 3D printing has is used in a wide range of applications in the medical field. Polyamide 12 (PA12) is a versatile synthetic polymer that has been used to reconstruct bony defects. Coating its surface with calcium phosphate compounds, such as hydroxyapatite (HA), could enhance its bonding with bone. The aim of this study was to coat 3D-printed polyamide 12 specimens with hydroxyapatite by a simple innovative surface treatment using light-cured resin cement. Polyamide 12 powder was printed by selective laser sintering to produce 80 disc-shaped specimens (15 mm diameter × 1.5 mm thickness). The specimens were divided randomly into two main groups: (1) control group (untreated), where the surface of the specimens was left without any modifications; (2) treated group, where the surface of the specimens was coated with hydroxyapatite by a new method using a light-cured dental cement. The coated specimens were characterised by both Fourier transform infrared spectroscopy (FTIR) and Transmission Electron Microscopy (TEM), (n = 10/test). The control and treated groups were further randomly subdivided into two subgroups according to the immersion in phosphate-buffered saline (PBS). The first subgroup was not immersed in PBS and was left as 3D-printed, while the second subgroup was immersed in PBS for 15 days (n = 10/subgroup). The surfaces of the control and treated specimens were examined using an environmental scanning electron microscope (SEM) and energy dispersive X-ray analysis (EDXA) before and after immersion in PBS. Following the standard American Society for Testing and Materials (ASTM D3359), a cross-cut adhesion test was performed. The results of the FTIR spectroscopy of the coated specimens were confirmed the HA bands. The TEM micrograph revealed agglomerated particles in the coat. The SEM micrographs of the control 3D-printed polyamide 12 specimens illustrated the sintered 3D-printed particles with minimal porosity. Their EDXA revealed the presence of carbon, nitrogen, and oxygen as atomic%: 52.1, 23.8, 24.1 respectively. After immersion in PBS, there were no major changes in the control specimens as detected by SEM and EDXA. The microstructure of the coated specimens showed deposited clusters of calcium and phosphorus on the surface, in addition to carbon, nitrogen, and oxygen, with atomic%: 9.5, 5.9, 7.2, 30.9, and 46.5, respectively. This coat was stable after immersion, as observed by SEM and EDXA. The coat adhesion test demonstrated a stable coat with just a few loose coating flakes (area removed <5%) on the surface of the HA-coated specimens. It could be concluded that the 3D-printed polyamide 12 could be coated with hydroxyapatite using light-cured resin cement. Full article
(This article belongs to the Special Issue Advanced Biomaterials and Coatings)
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<p>Diagram representing the surface treatment steps.</p>
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<p>Stereomicroscopic image illustrating the steps a–c of coating. Magnification: 12.5×.</p>
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<p>Stereomicroscopic image showing coated and uncoated surfaces (before immersion in PBS). Magnification: 12.5×.</p>
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<p>Stereomicroscopic image after immersion in PBS for coated and uncoated surfaces). Magnification: 12.5×.</p>
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<p>Diagram showing adhesion-scale according to ASTM D3359 standard.</p>
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<p>FTIR Spectra of the coated specimen.</p>
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<p>TEM micrographs of the coated specimen.</p>
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<p>SEM micrograph of control specimens before immersion in phosphate-buffered saline.</p>
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<p>EDXA of control specimens before immersion in phosphate-buffered saline.</p>
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<p>SEM micrograph of treated specimens before immersion in phosphate-buffered saline (magnification: 200×).</p>
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<p>EDXA spectrum of treated specimens before immersion in phosphate-buffered saline.</p>
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<p>SEM micrograph of control specimens after immersion in phosphate-buffered saline.</p>
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<p>EDXA spectrum of control specimens after immersion in phosphate-buffered saline.</p>
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<p>SEM micrograph of treated specimens after immersion in phosphate-buffered saline.</p>
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<p>EDXA spectrum of treated specimens after immersion in phosphate-buffered saline.</p>
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<p>SEM micrograph of lateral view of the coated specimens (magnification: 500×).</p>
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19 pages, 5359 KiB  
Article
Cellulose Nanofibrils Dewatered with Poly(Lactic Acid) for Improved Bio-Polymer Nanocomposite Processing
by Alexander Collins and Mehdi Tajvidi
Nanomaterials 2024, 14(17), 1419; https://doi.org/10.3390/nano14171419 - 30 Aug 2024
Viewed by 1141
Abstract
Cellulose nanofibrils (CNFs) have theoretically ideal properties for bio-based composite applications; however, the incorporation of these materials into polymers is made challenging by the strong binding of water to CNFs and the irreversible agglomeration of CNFs during drying. Previous methods used “contact dewatering”, [...] Read more.
Cellulose nanofibrils (CNFs) have theoretically ideal properties for bio-based composite applications; however, the incorporation of these materials into polymers is made challenging by the strong binding of water to CNFs and the irreversible agglomeration of CNFs during drying. Previous methods used “contact dewatering”, wherein the addition of wood flour (WF) to CNFs facilitated the mechanical removal of water from the system via cold pressing, which showed potential in producing dried CNF fibrils attached to wood fibers for biocomposite applications. In this work, the viability of contact dewatering with poly(lactic) acid (PLA) powder for PLA/CNF composites was evaluated. The energy efficiency of dewatering, preservation of nanoscale CNF morphology, and mechanical properties were examined by mixing wet CNFs with pulverized PLA at various loading levels, pressing water out of the system, and compression molding and shear mixing composites for testing. The most impressive results from this dewatering method were the preservation of micron-to-nanoscale fibers with high aspect ratios in PLA-CNF composites; increased strength and modulus of 1.7% and 4.2%, respectively, compared to neat PLA; equivalent or better properties than spray-dried nanocellulose at similar loading levels; and an 11-194x reduction in drying energy compared to spray-drying CNFs. Full article
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<p>Outline for PLA-CNF dewatering and manufacture of composites.</p>
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<p>PLM image processing for particle analysis of CNF in PLA-CNF films. (<b>A</b>–<b>C</b>) show the steps used to pre-process images so that particles can be analyzed by Image J. (<b>A</b>) Image of PLA-0.5% SDCNF, cropped to 8 × 8 mm<sup>2</sup> with scale bar removed. CNF particles are yellow-blue-green, PLA background is magenta-purple. (<b>B</b>) “Green” channel from R/G/B channel split. (<b>C</b>) Final binary image used in particle size analysis. Scale bar size = 50 μm.</p>
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<p>Dried and milled PLA-CNF mixtures under SEM.</p>
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<p>Results for tensile testing of masterbatched PLA-CNF composites and the PLA control. (<b>A</b>) Tensile strength. (<b>B</b>) Tensile modulus. Common letters on data points indicate statistically insignificant differences at 95% confidence level Error bars represent standard deviation.</p>
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<p>Tensile test results for compression molded PLA-CNF films with respect to CNF loading level. Common letters on data points indicate statistically insignificant differences at 95% confidence level. Error bars represent standard deviation.</p>
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<p>Results for tensile strength (<b>A</b>) and tensile modulus (<b>B</b>) of shear-mixed dewatered PLA-CNF composites at low loading levels. Common letters on data points indicate statistically insignificant differences at 95% confidence level. Error bars represent standard deviation.</p>
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<p>(<b>A</b>) Total estimated surface area in 1 g PLA particles over particle diameter. (<b>B</b>) Estimated threshold wt.% CNFs in PLA required to form a monolayer over each PLA particle based on PLA particle diameter.</p>
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<p>PLA-CNF composite films made from masterbatched PLA-50% CNF visualized with PLM. Letters correspond to CNF loading level, numbers denote microscopy type. (<b>A</b>–<b>C</b>) 10, 20, 30 wt.% CNF. 1, 2: PLM between crossed polarizers without a retardation filter and PLM between crossed polarizers with a retardation filter, respectively.</p>
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<p>Polarized light microscopy images of PLA-CNF composites made at lower CNF loading levels. Letters correspond to CNF loading level; numbers denote microscopy type. (<b>A</b>–<b>C</b>) 0.5, 2, 6 wt.% CNF. (<b>1</b>,<b>2</b>): PLM between crossed polarizers without a retardation filter and PLM between crossed polarizers with a retardation filter, respectively.</p>
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<p>PLM images of PLA-CNF films at lower loading levels of CNF. Letters correspond to CNF loading level, numbers correspond to processing/CNF type. (<b>A</b>–<b>C</b>) 0.5, 1, 2 wt.% CNF. 1, 2, 3: compression molded PLA-dCNF films, shear-mixed PLA-dCNF, and shear-mixed PLA-SDCNF. Objective lens: 10×.</p>
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<p>Aspect ratio histograms from analysis of PLA-dCNF and PLA-SDCNF PLM images. Bin size = 0.333 μm/μm. Bandwidth for kernel density overlay= 1.507 × 10<sup>−1</sup>. Median aspect ratios are listed above each distribution.</p>
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<p>(<b>A</b>) Percent solids of PLA-CNF mixtures after multiple dewatering passes, compared to WF-10% CNF. (<b>B</b>) HR water contents of PLA-CNF and WF-CNF furnishes (CNFs at ~3% solids, mixtures at ~5% solids).</p>
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<p>(<b>A</b>) Percent solids of low CNF mixtures after multiple dewatering passes. (<b>B</b>) Theoretical specific drying energy per gram of CNFs calculated for PLA-2%dCNF (20 wt.% starting solids) and PLA-50% dCNF (5 wt.% starting solids) after 1× dewatering passes compared to 1× pressed CNFs.</p>
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