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Search Results (1,073)

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17 pages, 1438 KiB  
Article
Fabrication and Electrical Characterization of Low-Temperature Polysilicon Films for Sensor Applications
by Filipa C. Mota, Inês S. Garcia, Aritz Retolaza, Dimitri E. Santos, Patrícia C. Sousa, Diogo E. Aguiam, Rosana A. Dias, Carlos Calaza, Alexandre F. Silva and Filipe S. Alves
Micromachines 2025, 16(1), 57; https://doi.org/10.3390/mi16010057 - 31 Dec 2024
Viewed by 213
Abstract
The development of low-temperature piezoresistive materials provides compatibility with standard silicon-based MEMS fabrication processes. Additionally, it enables the use of such material in flexible substrates, thereby expanding the potential for various device applications. This work demonstrates, for the first time, the fabrication of [...] Read more.
The development of low-temperature piezoresistive materials provides compatibility with standard silicon-based MEMS fabrication processes. Additionally, it enables the use of such material in flexible substrates, thereby expanding the potential for various device applications. This work demonstrates, for the first time, the fabrication of a 200 nm polycrystalline silicon thin film through a metal-induced crystallization process mediated by an AlSiCu alloy at temperatures as low as 450 °C on top of silicon and polyimide (PI) substrates. The resulting polycrystalline film structure exhibits crystallites with a size of approximately 58 nm, forming polysilicon (poly-Si) grains with diameters between 1–3 µm for Si substrates and 3–7 µm for flexible PI substrates. The mechanical and electrical properties of the poly-Si were experimentally conducted using microfabricated test structures containing piezoresistors formed by poly-Si with different dimensions. The poly-Si material reveals a longitudinal gauge factor (GF) of 12.31 and a transversal GF of −4.90, evaluated using a four-point bending setup. Additionally, the material has a linear temperature coefficient of resistance (TCR) of −2471 ppm/°C. These results illustrate the potential of using this low-temperature film for pressure, force, or temperature sensors. The developed film also demonstrated sensitivity to light, indicating that the developed material can also be explored in photo-sensitive applications. Full article
13 pages, 2744 KiB  
Article
Growth of MoS2 Nanosheets on Brush-Shaped PI–ZnO Hybrid Nanofibers and Study of the Photocatalytic Performance
by Zhenjun Chang, Zhengzheng Liao, Jie Han, Qiang Liu and Xiaoling Sun
Nanomaterials 2025, 15(1), 44; https://doi.org/10.3390/nano15010044 - 30 Dec 2024
Viewed by 259
Abstract
The design and preparation of advanced hybrid nanofibers with controllable microstructures will be interesting because of their potential high-efficiency applications in the environmental and energy domains. In this paper, a simple and efficient strategy was developed for preparing hybrid nanofibers of zinc oxide–molybdenum [...] Read more.
The design and preparation of advanced hybrid nanofibers with controllable microstructures will be interesting because of their potential high-efficiency applications in the environmental and energy domains. In this paper, a simple and efficient strategy was developed for preparing hybrid nanofibers of zinc oxide–molybdenum disulfide (ZnO–MoS2) grown on polyimide (PI) nanofibers by combining electrospinning, a high-pressure hydrothermal process, and in situ growth. Unlike simple composite nanoparticles, the structure is shown in PI–ZnO to be like the skeleton of a tree for the growth of MoS2 “leaves” as macro-materials with controlled microstructures. The surface morphology, structure, composition, and photocatalytic properties of these structures were characterized using scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and UV–vis spectroscopy. The ultra high-volume fraction of MoS2 can be grown on the brush-shaped PI–ZnO. Decorating ZnO with nanosheets of MoS2 (a transition metal dichalcogenide with a relatively narrow band gap) is a promising way to increase the photocatalytic activity of ZnO. The hybrid nanofibers exhibited high photocatalytic properties, which decomposed about 92% of the methylene blue in 90 min under visible light irradiation. The combination of MoS2 and ZnO with more abundant surface-active sites significantly increases the spectral absorption range, promotes the separation and migration of carriers, and improves the photocatalytic characteristics. Full article
(This article belongs to the Section Synthesis, Interfaces and Nanostructures)
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Figure 1
<p>Scheme for the preparation of PI-ZnO-MoS<sub>2</sub>.</p>
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<p>Field emission scanning electron micrographs of different composite fiber samples: PI nanofibers (<b>a</b>) and ZnO seed layer covering PI nanofibers (<b>b</b>), PI-ZnO nanocomposite nanofibers (<b>c</b>), PI-ZnO-MoS<sub>2</sub> hybrid nanofibers (<b>d</b>).</p>
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<p>XRD patterns of different composite nanofibers (<b>a</b>). XPS spectra of the PI-ZnO-MoS<sub>2</sub> nanocomposite structure of full range (<b>b</b>), Zn 2p (<b>c</b>), O 1s (<b>d</b>), Mo 3d (<b>e</b>), and S 2p (<b>f</b>).</p>
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<p>EDS spectra of PI-ZnO-MoS<sub>2</sub> composite nanofibers.</p>
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<p>Visible light absorption spectra of methylene blue (MB) as a function of visible light irradiation time (λ = 380–780 nm) in the presence of the PI-ZnO-MoS<sub>2</sub> composite nanofibers (<b>a</b>); time-dependent visible light absorbance of the MB solution after photodegradation by different membranes (<b>b</b>). The ln(C<sub>0</sub>/C) versus time (<b>c</b>) and reaction rate constants (<span class="html-italic">k</span>) of the MB photodegradation by different catalysts (<b>d</b>).</p>
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<p>Stability and repeatability of PI-ZnO-MoS<sub>2</sub> for MB photodegradation.</p>
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<p>UV–vis DRS spectra of samples (<b>a</b>), and picture of (Ahν)<sup>2</sup> versus hν for the samples (<b>b</b>).</p>
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<p>The proposed mechanism for photocatalytic degradation of MB solution in the presence of PI-ZnO-MoS<sub>2</sub> nanofibers under visible light irradiation.</p>
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21 pages, 17021 KiB  
Article
Impact of Particular Stages of the Manufacturing Process on the Reliability of Flexible Printed Circuits
by Andrzej Kiernich, Jerzy Kalenik, Wojciech Stęplewski, Marek Kościelski and Aneta Chołaj
Sensors 2025, 25(1), 140; https://doi.org/10.3390/s25010140 - 29 Dec 2024
Viewed by 239
Abstract
The purpose of the experiment was to indicate which element of the production process of flexible printed circuit boards is optimal in terms of the reliability of final products. According to the Taguchi method, in the experiment, five factors with two levels each [...] Read more.
The purpose of the experiment was to indicate which element of the production process of flexible printed circuit boards is optimal in terms of the reliability of final products. According to the Taguchi method, in the experiment, five factors with two levels each were chosen for the subsequent analysis. These included the number of conductive layers, the thickness of the laminate layer, the type of the laminate, the diameter of the plated holes, and the current density in the galvanic bath. The reliability of the PCBs in the produced variations was verified using the Interconnect Stress Test environmental test. The qualitatively best variant of the board construction was indicated using the signal-to-noise ratio and the analysis of variance method for each factor. The factors determined to be the most important in terms of reliability were the number of conductive layers and the current density in the galvanic bath. The optimal variant of the board construction was two conductive layers on a polyimide laminate, where the laminate layer was 100 μm thick, the hole diameter was equal to 0.4 mm, and current density was 2 A/dm2 in the galvanic bath. Therefore, the plated experiment indicated the factors needed to obtain a high-quality product with a low failure rate. Full article
(This article belongs to the Special Issue RFID-Enabled Sensor Design and Applications)
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<p>Scheme of production path of PCB.</p>
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<p>Design of samples, with the two-layer PCB above and the four-layer PCB below.</p>
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<p>Example of a PCB used as the sample.</p>
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<p>Work station used during the experiment. (<b>a</b>) The whole work station; (<b>b</b>) a zoomed image of one testing unit.</p>
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<p>IST results.</p>
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<p>Main effect—number of conductive layers. (<b>a</b>) Table showing the following statistics: the arithmetical mean and SNR; (<b>b</b>) graph showing the trajectory of the SNR coefficient.</p>
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<p>Main effect—thickness of laminate. (<b>a</b>) Table showing the following statistics: the arithmetical mean and SNR; (<b>b</b>) graph showing the trajectory of the SNR coefficient.</p>
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<p>Main effect—type of laminate. (<b>a</b>) Table showing the following statistics: arithmetical mean and SNR; (<b>b</b>) graph showing the trajectory of the SNR coefficient.</p>
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<p>Main effect—diameter of holes. (<b>a</b>) Table showing the following statistics: the arithmetical mean and SNR; (<b>b</b>) graph showing the trajectory of the SNR coefficient.</p>
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<p>Main effect—current density in the galvanic bath. (<b>a</b>) Table showing the following statistics: the arithmetical mean and SNR; (<b>b</b>) graph showing the trajectory of the SNR coefficient.</p>
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<p>The test board during the heating cycle.</p>
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<p>Location of the failure on the test board.</p>
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<p>Crack of metallization in PTH (<b>a</b>) metallographic cross-section—magnification ×700; (<b>b</b>) metallographic cross-section—magnification ×1500.</p>
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<p>Crack of metallization in microvia (<b>a</b>) metallographic cross-section—magnification ×500; (<b>b</b>) metallographic cross-section—magnification ×1000.</p>
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<p>Copper layers with metallization 1 A/dm<sup>2</sup>: (<b>a</b>) magnification ×1000; (<b>b</b>) magnification ×10,000.</p>
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<p>Copper layers with metallization 2 A/dm<sup>2</sup>: (<b>a</b>) magnification ×2000; (<b>b</b>) magnification ×10,000.</p>
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17 pages, 4791 KiB  
Article
Photoreconfigurable Metasurface for Independent Full-Space Control of Terahertz Waves
by Zhengxuan Jiang, Guowen Ding, Xinyao Luo and Shenyun Wang
Sensors 2025, 25(1), 119; https://doi.org/10.3390/s25010119 - 27 Dec 2024
Viewed by 459
Abstract
We present a novel photoreconfigurable metasurface designed for independent and efficient control of electromagnetic waves with identical incident polarization and frequency across the entire spatial domain. The proposed metasurface features a three-layer architecture: a top layer incorporating a gold circular split ring resonator [...] Read more.
We present a novel photoreconfigurable metasurface designed for independent and efficient control of electromagnetic waves with identical incident polarization and frequency across the entire spatial domain. The proposed metasurface features a three-layer architecture: a top layer incorporating a gold circular split ring resonator (CSRR) filled with perovskite material and dual C-shaped perovskite resonators; a middle layer of polyimide dielectric; and a bottom layer comprising a perovskite substrate with an oppositely oriented circular split ring resonator filled with gold. By modulating the intensity of a laser beam, we achieve autonomous manipulation of incident circularly polarized terahertz waves in both transmission and reflection modes. Simulation results demonstrate that the metasurface achieves a cross-polarized transmission coefficient of 0.82 without laser illumination and a co-polarization reflection coefficient of 0.8 under laser illumination. Leveraging the geometric phase principle, adjustments to the rotational orientation of the reverse split ring and dual C-shaped perovskite structures enable independent control of transmission and reflection phases. Furthermore, the proposed metasurface induces a +1 order orbital angular momentum in transmission and +2 order in reflection, facilitating beam deflection through metasurface convolution principles. Imaging using metasurface digital imaging technology showcases patterns “NUIST” in reflection and “LOONG” in transmission, illustrating the metasurface design principles via the proposed metasurface. The proposed metasurface’s capability for full-space control and reconfigurability presents promising applications in advanced imaging systems, dynamic beam steering, and tunable terahertz devices, highlighting its potential for future technological advancements. Full article
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<p>(<b>a</b>) OAM Mode 1 in transmission mode under high laser beam illumination for Metasurface I. (<b>b</b>) OAM Mode 2 in reflection mode without laser beam illumination for Metasurface I. (<b>c</b>) Holographic imaging with high laser beam illumination, generating a holographic image of the letters “NUIST” in reflection mode for Metasurface II. (<b>d</b>) Holographic imaging without laser beam illumination, generating a holographic image of the letters “LOONG” in transmission mode for Metasurface II.</p>
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<p>(<b>a</b>) Schematic of the proposed three-layer metasurface. (<b>b</b>) Top layer with CSRR and dual <span class="html-italic">C</span>-shaped resonators. (<b>c</b>) Bottom layer with circular split ring resonator.</p>
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<p>(<b>a</b>) Phase of co-polarized reflection coefficients (<span class="html-italic">r<sub>xx</sub></span> and <span class="html-italic">r<sub>yy</sub></span>) and co-polarized transmission coefficients (<span class="html-italic">t<sub>xx</sub></span> and <span class="html-italic">t<sub>yy</sub></span>) under laser beam illumination. (<b>b</b>) Phase of co-polarized reflection coefficients (<span class="html-italic">r<sub>xx</sub></span> and <span class="html-italic">r<sub>yy</sub></span>) and co-polarized transmission coefficients (<span class="html-italic">t<sub>xx</sub></span> and <span class="html-italic">t<sub>yy</sub></span>) without laser beam illumination. (<b>c</b>) Amplitude of co-polarized transmission coefficients (<span class="html-italic">t<sub>xx</sub></span> and <span class="html-italic">t<sub>yy</sub></span>) and co-polarized transmission coefficients (<span class="html-italic">t<sub>xx</sub></span> and <span class="html-italic">t<sub>yy</sub></span>) under laser beam illumination. (<b>d</b>) Amplitude of co-polarized transmission coefficients (<span class="html-italic">t<sub>xx</sub></span> and <span class="html-italic">t<sub>yy</sub></span>) and co-polarized transmission coefficients (<span class="html-italic">t<sub>xx</sub></span> and <span class="html-italic">t<sub>yy</sub></span>) without laser beam illumination.</p>
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<p>(<b>a</b>) Reflection amplitude and transmission amplitude at different rotation angles when unit is under laser beam illumination. (<b>b</b>) Transmission amplitude and reflection amplitude at different rotation angles when unit is without laser beam illumination. (<b>c</b>) Reflection phase at different rotation angles when unit is under laser beam illumination. (<b>d</b>) Transmission phase at different rotation angles when unit is without laser beam illumination.</p>
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<p>(<b>a</b>) Surface current distribution on the top layer under strong laser beam illumination, showing time-varying current distribution within the period. (<b>b</b>) Surface current distribution on the bottom layer under strong laser beam illumination, showing time-varying current distribution within the period. (<b>c</b>) Surface current distribution on the top layer without laser beam illumination, showing time-varying current distribution within the period. (<b>d</b>) Surface current distribution on the bottom layer without laser beam illumination, showing time-varying current distribution within the period.</p>
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<p>(<b>a</b>) Phase gradients along the +<span class="html-italic">x</span> direction. (<b>b</b>) Phase gradients along the −<span class="html-italic">x</span> direction. (<b>c</b>) Far-field distribution of a +1 order vortex beam deflected by 30° in the +<span class="html-italic">x</span> direction under strong laser beam illumination. (<b>d</b>) Far-field distribution of a −2 order vortex beam deflected by 30° in the −<span class="html-italic">x</span> direction without laser beam illumination. (<b>e</b>) Planar electric field intensity and phase distribution of the +1 order vortex beam under strong laser beam illumination, perpendicular to the 30° direction. (<b>f</b>) Planar electric field intensity and phase distribution of the −2 order vortex beam without laser beam illumination, perpendicular to the −30° direction.</p>
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<p>(<b>a</b>) Target images: “Zhu” in reflection mode, “Long” in transmission mode. (<b>b</b>) Phase distribution for holographic images, with phase changes from 0° to 360°. (<b>c</b>) Metasurface design layout with 50 × 50 unit structures in top and bottom layers. (<b>d</b>) Simulation results under different laser beam illumination: “Zhu” in reflection mode under laser beam illumination; “Long” in transmission mode without laser beam illumination.</p>
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<p>(<b>a</b>) Target images in reflection mode. (<b>b</b>) Phase distribution for reflection mode calculated using the GS algorithm. (<b>c</b>) Reproduced image of “NUIST” in reflection mode. (<b>d</b>) Target images in transmission mode. (<b>e</b>) Phase distribution for transmission mode calculated using the GS algorithm. (<b>f</b>) Reproduced image of “LOOGN” in transmission mode.</p>
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<p>(<b>a</b>) Near-field imaging results. (<b>b</b>) Far-field electric field distribution in reflection mode. (<b>c</b>) Far-field electric field distribution in transmission mode.</p>
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18 pages, 7823 KiB  
Article
Goniopolarimetric Properties of Typical Satellite Material Surfaces: Intercomparison with Semi-Empirical pBRDF Modeled Results
by Min Yang, Hongxia Mao, Jun Wu, Chong Zheng and Li Wang
Photonics 2025, 12(1), 17; https://doi.org/10.3390/photonics12010017 - 27 Dec 2024
Viewed by 168
Abstract
Light reflected from satellite surfaces is polarized light, which plays a crucial role in space target identification and remote sensing. To deepen our understanding of the polarized reflectance property for satellite material surface, we present the experiments of polarimetric laboratory measurements from two [...] Read more.
Light reflected from satellite surfaces is polarized light, which plays a crucial role in space target identification and remote sensing. To deepen our understanding of the polarized reflectance property for satellite material surface, we present the experiments of polarimetric laboratory measurements from two typical satellite materials in the wavelength range of 400–1000 nm by using a goniometer instrument. The bidirectional polarized reflectance factor (BPRF) is used to describe the polarization characteristics of our samples. The polarized spectral reflectance and distribution of BPRF for our datasets are analyzed. Furthermore, five semi-empirical polarized bidirectional reflectance distribution functions (pBRDFs) models for polarized reflectance of typical satellite material surfaces (Preist–Germer model, Maxwell–Beard model, three-component model, Cook–Torrance model, and Kubelka–Munk model) are quantitatively intercompared using the measured BPRFs. The results suggest that the measured BPRFs of our samples are spectrally irrelevant, and the hemispherical distribution of BPRFs is obviously anisotropic. Except for the Preist–Germer model, the other semi-empirical models are in good agreement with the measured BPRF at the selected wavelengths, indicating that we can accurately simulate the polarized reflectance property of the satellite surface by using the existing polarimetric models. The Kubelka–Munk pBRDF model best fits the silver polyimide film and white coating surfaces with RMSE equal to 3.25% and 2.03%, and the correlation coefficient is 0.994 and 0.984, respectively. This study can be applied to provide an accurate pBRDF model for space object scene simulation and has great potential for polarization remote sensing. Full article
(This article belongs to the Special Issue Polarization Optics)
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<p>The picture of typical satellite material: (<b>a</b>) silver polyimide film, and (<b>b</b>) white coating.</p>
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<p>(<b>a</b>) The schematic diagram of measurement. (<b>b</b>) The grid is the hemispherical sampling pattern when the incident zenith angle is 40°.</p>
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<p>The BRF spectrum curves of the (<b>a</b>) silver polyimide film and (<b>b</b>) white coating at different viewing zenith angles (Δ<span class="html-italic">ϕ</span> = 180°) when the incident zenith angle is 40°.</p>
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<p>The DoLP curves of the (<b>a</b>) silver polyimide film and (<b>b</b>) white coating at different viewing zenith angles (Δ<span class="html-italic">ϕ</span> = 180°) when the incident zenith angle is 40°.</p>
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<p>The BPRF curves of the (<b>a</b>) silver polyimide film and (<b>b</b>) white coating at different viewing zenith angles (Δ<span class="html-italic">ϕ</span> = 180°) when the incident zenith angle is 40°.</p>
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<p>The hemisphere distribution of BPRF of the silver polyimide film at (<b>a</b>) 560 nm, (<b>b</b>) 670 nm, and (<b>c</b>) 865 nm, and the incident zenith angle is 40°.</p>
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<p>The hemisphere distribution of BPRF of the white coating at (<b>a</b>) 560 nm, (<b>b</b>) 670 nm, and (<b>c</b>) 865 nm, and the incident zenith angle is 40°.</p>
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<p>The hemisphere distribution of BPRF of the silver polyimide film at 670 nm, and the incident zenith angles are (<b>a</b>) 30°, (<b>b</b>) 50°, and (<b>c</b>) 60°.</p>
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<p>The hemisphere distribution of BPRF of the white coating at 670 nm, and the incident zenith angles are (<b>a</b>) 30°, (<b>b</b>) 50°, and (<b>c</b>) 60°.</p>
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<p>The hemisphere distribution of (<b>a</b>) the measured BPRF and (<b>b</b>–<b>f</b>) the modeled BPRF of the silver polyimide film at 865 nm, and the incident zenith angle is 40°.</p>
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<p>The hemisphere distribution of (<b>a</b>) the measured BPRF and (<b>b</b>–<b>f</b>) the modeled BPRF of the white coating at 865 nm, and the incident zenith angle is 40°.</p>
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<p>The comparison between measurements and modeled BPRF of our samples over all measured directions in all incident zenith angles.</p>
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13 pages, 6926 KiB  
Article
Annealing Study on Praseodymium-Doped Indium Zinc Oxide Thin-Film Transistors and Fabrication of Flexible Devices
by Zhenyu Wu, Honglong Ning, Han Li, Xiaoqin Wei, Dongxiang Luo, Dong Yuan, Zhihao Liang, Guoping Su, Rihui Yao and Junbiao Peng
Micromachines 2025, 16(1), 17; https://doi.org/10.3390/mi16010017 - 26 Dec 2024
Viewed by 460
Abstract
The praseodymium-doped indium zinc oxide (PrIZO) thin-film transistor (TFT) is promising for applications in flat-panel displays, due to its high carrier mobility and stability. Nevertheless, there are few studies on the mechanism of annealing on PrIZO films and the fabrication of flexible devices. [...] Read more.
The praseodymium-doped indium zinc oxide (PrIZO) thin-film transistor (TFT) is promising for applications in flat-panel displays, due to its high carrier mobility and stability. Nevertheless, there are few studies on the mechanism of annealing on PrIZO films and the fabrication of flexible devices. In this work, we first optimized the annealing-process parameters on the glass substrate. As the annealing temperature rises, the film tends to be denser and obtains a lower surface roughness, a narrower optical-band gap and less oxygen-vacancy content. However, the μ-PCD test shows the 250 °C-annealed film obtains the least defects. And the PrIZO TFT annealed at 250 °C exhibited a desired performance with a saturation mobility (μsat) of 14.26 cm2·V−1·s−1, a subthreshold swing (SS) of 0.14 V·dec−1, an interface trap density (Dit) of 3.17 × 1011, an Ion/Ioff ratio of 1.83 × 108 and a threshold voltage (Vth) of −1.15 V. The flexible devices were prepared using the optimized parameters on the Polyimide (PI) substrate and subjected to static bending tests. After bending at a radius of 5 mm, the mobility of devices decreases slightly from 12.48 to 10.87 cm2·V−1·s−1, demonstrating the great potential of PrIZO for flexible displays. Full article
(This article belongs to the Special Issue Thin Film Microelectronic Devices and Circuits)
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<p>Schematic diagram of PrIZO TFT: (<b>a</b>) glass substrate, (<b>b</b>) PI substrate.</p>
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<p>XRD patterns of PrIZO thin films annealed at different temperatures.</p>
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<p>PrIZO thin films annealed at different temperature: (<b>a</b>) XRR, (<b>b</b>) thickness and density.</p>
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<p>AFM images of PrIZO thin films: (<b>a</b>) untreated, (<b>b</b>) 200 °C, (<b>c</b>) 250 °C, (<b>d</b>) 300 °C and AFM images of insulators: (<b>e</b>) on the PI substrate, (<b>f</b>) on the glass substrate.</p>
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<p>PrIZO thin films: (<b>a</b>) transmission spectra, (<b>b</b>) optical band gap.</p>
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<p>O 1s peak of XPS spectra of PrIZO thin films: (<b>a</b>) untreated, (<b>b</b>) 200 °C, (<b>c</b>) 250 °C, (<b>d</b>) 300 °C.</p>
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<p>The µ-PCD mapping scan result of PrIZO films: (<b>a</b>) untreated, (<b>b</b>) 200 °C, (<b>c</b>) 250 °C, (<b>d</b>) 300 °C.</p>
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<p>The output curves of PrIZO TFTs: (<b>a</b>) 200 °C, (<b>b</b>) 250 °C, (<b>c</b>) 300 °C and transfer curves of PrIZO TFTs: (<b>d</b>) I<sub>D</sub>, (<b>e</b>) |I<sub>G</sub>|.</p>
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<p>NBIS stabilities of PrIZO TFTs: (<b>a</b>) 200 °C, (<b>b</b>) 250 °C, (<b>c</b>) 300 °C, (<b>d</b>) ΔV<sub>th</sub>.</p>
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<p>The transfer curves of flexible PrIZO TFTs: (<b>a</b>) I<sub>D</sub>, (<b>b</b>) |I<sub>G</sub>|.</p>
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16 pages, 22416 KiB  
Article
A Combinatory Therapy of Metformin and Dexamethasone Reduces the Foreign Body Reaction to Intraneural Electrodes
by Bruno Rodríguez-Meana, Jaume del Valle and Xavier Navarro
Cells 2024, 13(24), 2112; https://doi.org/10.3390/cells13242112 - 20 Dec 2024
Viewed by 309
Abstract
Neural electrodes used for bidirectional communication between the nervous system and external devices like prosthetic limbs have advanced in neuroprosthetic applications. However, their effectiveness is hindered by the foreign body reaction, a natural immune response causing inflammation and fibrosis around the implanted device. [...] Read more.
Neural electrodes used for bidirectional communication between the nervous system and external devices like prosthetic limbs have advanced in neuroprosthetic applications. However, their effectiveness is hindered by the foreign body reaction, a natural immune response causing inflammation and fibrosis around the implanted device. This process involves protein adsorption, immune cell recruitment, cytokine release, and fibroblast activation, leading to a fibrous capsule formation and a decrease in electrode functionality. Anti-inflammatory and antifibrotic strategies have the potential to diminish the impact of the foreign body response. In this work, we have evaluated long-term metformin administration and short-term dexamethasone administration as a combined therapy to modulate the foreign body reaction induced by a polyimide intraneural implant in the sciatic nerve of rats. After a 12-week implant, the foreign body reaction was significantly reduced only in the group administered both drugs. Full article
(This article belongs to the Section Cells of the Nervous System)
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Figure 1
<p>Results of the functional tests in rats with a PI device implanted in the tibial nerve. (<b>A</b>) Algesimetry test results expressed as percentages of force thresholds for withdrawal (vs. contralateral control paw) of animals before the implantation and after the implantation and treatments for 12 weeks. (<b>B</b>) The plot of the SFI obtained in the walking track test. No significant differences were found.</p>
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<p>Results of the functional tests in rats with a PI intraneural device implanted in the tibial nerve. Motor nerve conduction parameters of animals before implantation (Pre) and after the implantation of PI devices for 12 weeks and drug administration. (<b>A</b>,<b>B</b>) CMAP amplitudes of GM (<b>A</b>) and PL (<b>B</b>) muscles. (<b>C</b>,<b>D</b>) CMAP onset latencies of GM (<b>C</b>) and PL (<b>D</b>) muscles. No significant differences were found in electrophysiological test results.</p>
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<p>The effect of drug administration on the FBR to intraneural implants. (<b>A</b>) The number of inflammatory Iba1+ cells in the tibial nerve of animals implanted with PI devices and administered metformin, dexamethasone, or both. (<b>B</b>,<b>C</b>) Tissue capsule thickness around the devices in the tibial nerve of animals implanted with PI receiving the different treatments. Measurements were made using immunofluorescence sections (<b>B</b>) and thin sections of epon-embedded nerves (<b>C</b>). (<b>D</b>–<b>F</b>) Correlation between the number of Iba1+ cells and capsule thickness (IF) at 2, 8, and 12 weeks after implantation. The solid lines represent the linear regression, while the shaded area represents the 95% CIL. * <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01, *** <span class="html-italic">p</span> &lt; 0.001, **** <span class="html-italic">p</span> &lt; 0.0001, and ### <span class="html-italic">p</span> &lt; 0.01 time variable, two-way ANOVA followed by Tukey’s multiple comparison test.</p>
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<p>Representative images of inflammatory cells (red, Iba 1+ cell) infiltrating the tibial nerve after 2, 8, and 12 weeks of the PI intraneural device implantation in the different groups studied. Note the intense fluorescence emitted by the PI. The area limited by the dotted line corresponds to the tibial fascicle of the sciatic nerve that was used to analyze the number of labeled cells. Scale bar: 100 μm.</p>
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<p>Representative images of nerve cross-sections around the PI intraneural implant after 2, 8, and 12 weeks of the implantation in the different groups studied. Nerve fibers are labeled with antibody RT97. Note the intense fluorescence emitted by the PI. The measured capsule surrounding the PI device is the area delimited by the dotted line, which separates the PI from the nerve fibers, excluding tissue-empty regions. Scale bar: 50 μm.</p>
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<p>Representative images of cross-sections of the nerves embedded in epon resin and stained with toluidine blue, corresponding to samples taken at 2, 8, and 12 weeks for the different study groups. The images show the PI implants (pointed to by a red arrow in the top-right panel) within the nerve, surrounded by the capsule and axons. The thickness of the capsule from the implant to the first axons is marked with a red bar in the top-right panel. Images were acquired and transformed to greyscale. Scale bar: 50 μm for all the panels.</p>
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<p>Representative images of the capsule composition around the PI intraneural implant. Immunohistochemical labeling for macrophages (red, Iba 1+), fibroblasts (green, CD90, arrowheads), and nuclei (blue, DAPI) of tibial nerves of animals of the different groups implanted with a PI device after 2, 8, and 12 weeks. Scale bar: 10 μm. Images with the individual channels are presented as <a href="#app1-cells-13-02112" class="html-app">Supplementary Materials Figures S1–S3</a>.</p>
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<p>Representative images of nerve sections stained with Masson’s trichrome stain, showing the deposition of collagen in the capsule around the PI intraneural implant. At 2 weeks, the pink-stained area, outlined by the dotted line, corresponds to macrophages around the implant. At 8 and 12 weeks, the pink areas around the devices decreased, while the blue-stained areas (dotted line), composed of collagen fibers, were more preeminent surrounding the implant. Scale bar: 50 and 20 μm.</p>
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15 pages, 2114 KiB  
Article
Laser-Induced Graphene Electrodes for Flexible pH Sensors
by Giulia Massaglia, Giacomo Spisni, Tommaso Serra and Marzia Quaglio
Nanomaterials 2024, 14(24), 2008; https://doi.org/10.3390/nano14242008 - 14 Dec 2024
Viewed by 404
Abstract
In the growing field of personalized medicine, non-invasive wearable devices and sensors are valuable diagnostic tools for the real-time monitoring of physiological and biokinetic signals. Among all the possible multiple (bio)-entities, pH is important in defining health-related biological information, since its variations or [...] Read more.
In the growing field of personalized medicine, non-invasive wearable devices and sensors are valuable diagnostic tools for the real-time monitoring of physiological and biokinetic signals. Among all the possible multiple (bio)-entities, pH is important in defining health-related biological information, since its variations or alterations can be considered the cause or the effect of disease and disfunction within a biological system. In this work, an innovative (bio)-electrochemical flexible pH sensor was proposed by realizing three electrodes (working, reference, and counter) directly on a polyimide (Kapton) sheet through the implementation of CO2 laser writing, which locally converts the polymeric sheet into a laser-induced graphene material (LIG electrodes), preserving inherent mechanical flexibility of Kapton. A uniform distribution of nanostructured PEDOT:PSS was deposited via ultrasonic spray coating onto an LIG working electrode as the active material for pH sensing. With a pH-sensitive PEDOT coating, this flexible sensor showed good sensitivity defined through a linear Nernstian slope of (75.6 ± 9.1) mV/pH, across a pH range from 1 to 7. We demonstrated the capability to use this flexible pH sensor during dynamic experiments, and thus concluded that this device was suitable to guarantee an immediate response and good repeatability by measuring the same OCP values in correspondence with the same pH applied. Full article
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<p>The schematic representation of the process workflows proposed: in (<b>a</b>), the workflow referring to the realization of the LIG-PEDOT pH sensor is sketched, while in (<b>b</b>), the one followed for fabricating the commercial-PEDOT pH sensor is represented.</p>
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<p>(<b>a</b>) Morphological properties of LIG electrodes realized on Kapton sheet by implementing CO<sub>2</sub> laser writing; (<b>b</b>) morphological features of 200 μg/cm<sup>2</sup> of PEDOT onto LIG electrode.</p>
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<p>Raman spectrum of PEDOT:PSS nanostructured layer deposited onto LIG electrodes by implementing USC process. It is possible to underline the prevalence of the benzoid group (purple line) over the quinoid one (green line).</p>
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<p>(<b>a</b>) Equivalent circuit used to determine electrochemical parameters; (<b>b</b>) double-layer capacitance and charge transfer resistance variation of the electrochemical sensor with pH values.</p>
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<p>OCP measurements conducted at different pH values, defined in the range from 1 to 7, mimicking the acidic environment. Experimental data for LIG-PEDOT pH sensors (pink dot) were compared with those for commercial-PEDOT (red dot), highlighting a linear pH response (pink line for LIG-PEDOT pH sensor and red line for commercial PEDOT, respectively).</p>
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<p>OCP measurements conducted at different pH values in a dynamic way. LIG-PEDOT pH sensors were immersed in the electrolyte solution, and pH values were continuously modified by adding NaOH and HCl to move from a basic environment to a strong acidic one.</p>
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14 pages, 4193 KiB  
Article
Simultaneous Temperature and Relative Humidity Measurement Using Machine Learning in Rayleigh-Based Optical Frequency Domain Reflectometry
by Mateusz Mądry, Bogusław Szczupak, Mateusz Śmigielski and Bartosz Matysiak
Sensors 2024, 24(24), 7913; https://doi.org/10.3390/s24247913 - 11 Dec 2024
Viewed by 472
Abstract
This paper presents, for the first time to the best of our knowledge, simultaneous temperature and relative humidity (RH) measurement using a machine learning (ML) model in Rayleigh-based Optical Frequency Domain Reflectometry (OFDR). The sensor unit consists of two segments: bare and polyimide-coated [...] Read more.
This paper presents, for the first time to the best of our knowledge, simultaneous temperature and relative humidity (RH) measurement using a machine learning (ML) model in Rayleigh-based Optical Frequency Domain Reflectometry (OFDR). The sensor unit consists of two segments: bare and polyimide-coated fibers, each with different sensitivities to temperature. The polyimide-coated fiber is RH-sensitive, unlike the bare fiber. We propose the ML approach to avoid manual post-processing data and maintain relatively high accuracy of the sensor. The root mean square error (RMSE) values for the 3 cm length of the sensor unit were 0.36 °C and 1.73% RH for temperature and RH, respectively. Furthermore, we investigated the impact of sensor unit lengths and number of data points on RMSE values. This approach eliminates the need for manual data processing, reduces analysis time, and enables accurate, simultaneous measurement of temperature and RH in Rayleigh-based OFDR. Full article
(This article belongs to the Section Optical Sensors)
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<p>The scheme of the experimental setup consisted of LUNA OBR 4600 as Rayleigh-based OFDR, a PC (Personal Computer) with dedicated software, SMF-28, bare fiber—SM1500(7.8/125), PI-coated fiber—SM1500(7.8/125P), and the climate chamber. The sensor unit consists of bare and PI-coated fibers.</p>
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<p>The backscattered trace from LUNA OBR 4600 to the end of the fiber line.</p>
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<p>The algorithm for measurement data processing in this study.</p>
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<p>(<b>a</b>) The exemplary spectral shift as a function of fiber length (limited to the investigated section) for different RH values at a constant temperature of 40 °C. (<b>b</b>) Spectral shift values as a function of RH changes.</p>
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<p>The exemplary spectral shift as a function of fiber length (limited to the investigated section) for different temperature values at constant 50% RH.</p>
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<p>The spectral shift as a function of ascending and descending RH for PI-coated fiber.</p>
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<p>The spectral shift for ascending and descending temperatures in a range of 30–80 °C for (<b>a</b>) bare fiber and (<b>b</b>) PI-coated fiber.</p>
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<p>The spectral shift as a function of strain for bare and PI-coated fibers.</p>
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<p>The RMSE values for different sensor lengths (3–10 cm) for temperature and RH, respectively.</p>
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<p>The RMSE values for different numbers of measurement points with constant value of sensor length (10 cm) for temperature and RH, respectively.</p>
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<p>The RMSE values for different numbers of measurement points with constant values of sensor length (3 cm) for temperature and RH, respectively.</p>
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14 pages, 2881 KiB  
Article
Preparation and Characterization of a Novel Self-Healing Transparent Polyimide Film Based on Dynamic Disulfide Bonds
by Xin Li, Yan Zhai, Kai Yang, Jingjing Bai, Yu Qiu and Yulong Wang
Polymers 2024, 16(24), 3461; https://doi.org/10.3390/polym16243461 - 11 Dec 2024
Viewed by 421
Abstract
Self-healing optically transparent polyimides have potential applications in optoelectronic device fabrication. In this study, for the first time, we successfully prepared a novel self-healing polyimide film containing reversible disulfide bonds through chemical imidization by introducing cystamine as a self-healing functional monomer into the [...] Read more.
Self-healing optically transparent polyimides have potential applications in optoelectronic device fabrication. In this study, for the first time, we successfully prepared a novel self-healing polyimide film containing reversible disulfide bonds through chemical imidization by introducing cystamine as a self-healing functional monomer into the molecular structure of conventional polyimides. The incorporation of cystamine enabled the films to maintain high transmittance (>87%) and tensile strength (>99 MPa). Meanwhile, tensile tests showed that the prepared film with a cystamine content of 50% achieved an excellent self-healing efficiency of up to 91.8%. Stress relaxation tests further revealed that disulfide bonds were rapidly cleaved upon thermal stimulation and the network topology was rearranged to complete the self-healing process. These results suggest that the dynamic covalent polymer network made of aliphatic disulfide bonds presents a new strategy for the development of optically transparent polyimides with excellent self-healing properties. Full article
(This article belongs to the Section Polymer Membranes and Films)
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<p>Structural properties of SHPI films: (<b>a</b>) FT-IR spectra; (<b>b</b>) H<sup>1</sup> NMR spectrum of SHPI-0.5; (<b>c</b>) high-resolution S 2p XPS spectra of SHPI-0.5; and (<b>d</b>) XRD spectra.</p>
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<p>UV–Vis spectra of SHPI films. The inserted image shows the excellent optical transparency of the SHPI films.</p>
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<p>Thermal properties of SHPI films: (<b>a</b>) TGA curves; (<b>b</b>) DTG curves; (<b>c</b>) DSC curves; and (<b>d</b>) DMA curves.</p>
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<p>Self-healing processes of scratched SHPI films observed using an BX41 polarizing microscope.</p>
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<p>SEM images of SHPI-0.5 films: (<b>a</b>) scratched film; (<b>b</b>) healed film; (<b>c</b>) EDS spectra of scratched and healed SHPI-0.5 films; and (<b>d</b>) high-resolution S 2p XPS spectra of SHPI-0.5 films before scratching and after healing.</p>
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<p>Mechanical properties and healing capacities of SHPI films: (<b>a</b>) stress–strain curves of SHPI films (bold line: pristine films; dashed line: healed films); and (<b>b</b>) tensile strength and self-healing efficiencies of SHPI films.</p>
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<p>Stress relaxation behaviors of SHPI films. Normalized stress-relaxation curves of: (<b>a</b>) SHPI-0; (<b>b</b>) SHPI-0.1; (<b>c</b>) SHPI-0.3; and (<b>d</b>) SHPI-0.5 films at different temperatures. (<b>e</b>) The Arrhenius analysis of SHPI films; and (<b>f</b>) activation energy of SHPI films.</p>
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<p>The procedure of synthesizing SHPIs.</p>
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15 pages, 6123 KiB  
Article
Impact of Moisture Absorption on Optical Fiber Sensors: New Bragg Law Formulation for Monitoring Composite Structures
by Pietro Aceti and Giuseppe Sala
J. Compos. Sci. 2024, 8(12), 518; https://doi.org/10.3390/jcs8120518 - 9 Dec 2024
Viewed by 533
Abstract
In recent decades, the aviation industry has increasingly adopted composite materials for various aircraft components, due to their high strength-to-weight ratio and durability. To ensure the safety and reliability of these structures, Health and Usage Monitoring Systems (HUMSs) based on fiber optics (FO), [...] Read more.
In recent decades, the aviation industry has increasingly adopted composite materials for various aircraft components, due to their high strength-to-weight ratio and durability. To ensure the safety and reliability of these structures, Health and Usage Monitoring Systems (HUMSs) based on fiber optics (FO), particularly Fiber Bragg Grating (FBG) sensors, have been developed. However, both composite materials and optical fibers are susceptible to environmental factors such as moisture, in addition to the well-known effects of mechanical stress and thermal loads. Moisture absorption can lead to the degradation of mechanical properties, posing a risk to the structural integrity of aircraft components. This research aims to quantify and monitor the impact of moisture on composite materials. A new formulation of the Bragg equation is introduced, incorporating mechanical strain, thermal expansion, and hygroscopic swelling to accurately measure Bragg wavelength variations. Experimental validation was performed using both uncoated and polyimide-coated optical fibers subjected to controlled hygrothermal conditions in a climate chamber. The results demonstrate that uncoated fibers are insensitive to humidity, whereas coated fibers exhibit measurable wavelength shifts due to moisture absorption. The proposed model effectively predicts these shifts, with errors consistently below 2.6%. This approach is crucial for improving the performance and reliability of HUMSs in monitoring composite structures, ensuring long-term safety in extreme environmental conditions. Full article
(This article belongs to the Section Composites Manufacturing and Processing)
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<p>Accidents due to hygrothermal effects.</p>
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<p>Coated optical fiber scheme.</p>
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<p>Experimental setup.</p>
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<p>Wavelength trend in time for an uncoated fiber.</p>
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<p>Linear interpolation and sensitivities, uncoated fiber.</p>
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<p>Coated fiber response.</p>
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<p>Linear interpolation and sensitivities. (<b>a</b>) Linear interpolation for temperature sensitivities. (<b>b</b>) Linear interpolation for humidity sensitivities.</p>
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<p>Comparison between theoretical and experimental wavelengths at each constant temperature.</p>
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<p>Comparison between theoretical and experimental wavelengths at each constant temperature and relative humidity.</p>
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18 pages, 6783 KiB  
Review
Polyimide-Based Dielectric Materials for High-Temperature Capacitive Energy Storage
by Lingling Liu, Li Li, Shixian Zhang, Wenhan Xu and Qing Wang
Electron. Mater. 2024, 5(4), 303-320; https://doi.org/10.3390/electronicmat5040019 - 8 Dec 2024
Viewed by 739
Abstract
Polyimide (PI) has received great attention for high-temperature capacitive energy storage materials due to its remarkable thermal stability, relatively high breakdown strength, strong mechanical properties, and ease of synthesis and modification. In this review, several key parameters for evaluating capacitive energy storage performance [...] Read more.
Polyimide (PI) has received great attention for high-temperature capacitive energy storage materials due to its remarkable thermal stability, relatively high breakdown strength, strong mechanical properties, and ease of synthesis and modification. In this review, several key parameters for evaluating capacitive energy storage performance are introduced. Subsequently, the properties of the commercially available PIs are presented. Then, the recent development of designing and tailoring all-organic PI-based polymers is discussed in detail, focusing on molecular composition and spatial configuration to enhance dielectric constant, breakdown strength, discharged energy density, and charge-discharge efficiency. Finally, we outline the current challenges and future development directions of PI-based high-temperature energy storage dielectric materials. Full article
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<p>Schematic of <span class="html-italic">D</span>–<span class="html-italic">E</span> loop for calculating energy density and charge-discharge efficiency.</p>
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<p>Schematic of self-clearing mechanism.</p>
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<p>(<b>a</b>) Schematic of different carbonyl-containing polyimides. (<b>b</b>) Dielectric constant and dissipation factor as a function of frequency at 25 °C. (<b>c</b>) Weibull breakdown strength of CPI-1–5. Reprinted with permission from Ref. [<a href="#B66-electronicmat-05-00019" class="html-bibr">66</a>]. Copyright 2019 John Wiley and Sons.</p>
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<p>(<b>a</b>) Molecular structure of 12 predicted derived PIs with nine structural blocks. (<b>b</b>) Comparison of energy bandgaps and glass transition temperatures of several commercial dielectric polymers and PI-derived polymers in this work. (<b>c</b>) Quantitative effects of structural unit addition and substitution on <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>E</mi> </mrow> <mrow> <mi>g</mi> </mrow> </msub> </mrow> </semantics></math> and <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>T</mi> </mrow> <mrow> <mi>g</mi> </mrow> </msub> </mrow> </semantics></math>. (<b>d</b>) Discharged energy density and efficiency of PI-derived polymers which have <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>E</mi> </mrow> <mrow> <mi>g</mi> </mrow> </msub> </mrow> </semantics></math> over 3.3 eV at 200 °C and 100 Hz. Reprinted with permission from Ref. [<a href="#B17-electronicmat-05-00019" class="html-bibr">17</a>] from Springer Nature.</p>
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<p>(<b>a</b>) Synthesis of two alicyclic polyimides (CBDA/DCHM and CBDA/TFMB). (<b>b</b>) Weibull breakdown strength of CBDA/DCHM, CBDA/TFMB, and PMDA/ODA at 200 °C. (<b>c</b>) Dielectric capacitive performance of three polyimides at 200 °C. (<b>d</b>) Discharged energy density comparisons of polyimides reported in this work and a previous work at 200 °C. Reprinted with permission from Ref. [<a href="#B71-electronicmat-05-00019" class="html-bibr">71</a>]. Copyright 2023 Royal Society of Chemistry.</p>
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<p>(<b>a</b>) Synthesis of semi-alicyclic SO-PI copolymer. (<b>b</b>) Picture of semi-alicyclic SO-PI copolymer. (<b>c</b>) Atomic force microscopy (AFM) image of semi-alicyclic SO-PI copolymer. (<b>d</b>) Electrostatic potential distribution of SO-PI and semi-alicyclic SO-PI. (<b>e</b>) Temperature-dependent dielectric constant at 1 kHz. (<b>f</b>) Discharged energy density and efficiency of SO-PI and SO-PI-14.3 copolymer at 200 °C. Reprinted with permission from Ref. [<a href="#B27-electronicmat-05-00019" class="html-bibr">27</a>]. Copyright 2024 John Wiley and Sons.</p>
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<p>(<b>a</b>) Energy-favored configuration of four PIs, i.e., regular PI, PI-B, spiral-structured PI-1, and spiral-structured PI-2. (<b>b</b>) Schematic of 3D electrostatic potential distribution of four PIs. (<b>c</b>) Weibull breakdown strength of PI, PI-B, PI-spiro-1, and PI-spiro-2 at 200 °C. (<b>d</b>) Discharge energy density of PIs with <span class="html-italic">η</span> above 90% at 150 and 200 °C. Reprinted with permission from Ref. [<a href="#B14-electronicmat-05-00019" class="html-bibr">14</a>]. Copyright 2023 John Wiley and Sons.</p>
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<p>Polyimide synthesized by two or one-step method.</p>
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14 pages, 3042 KiB  
Article
Enhanced Interfacial Properties of Carbon Fiber/Polymerization of Monomers Reactants Method Polyimide Composite by Polyimide Sizing
by Chengyu Huang, Jinsong Sun, Zhiwei Liu, Bo Li, Mingchen Sun, Hansong Liu, Yan Zhao, Peng Zhang and Jianwen Bao
Materials 2024, 17(23), 5962; https://doi.org/10.3390/ma17235962 - 5 Dec 2024
Viewed by 452
Abstract
Carbon fiber (CF)-reinforced polyimide (PI) resin matrix composites have great application potential in areas such as rail transport, medical devices, and aerospace due to their excellent thermal stability, dielectric properties, solvent resistance, and mechanical properties. However, the epoxy sizing agent used for traditional [...] Read more.
Carbon fiber (CF)-reinforced polyimide (PI) resin matrix composites have great application potential in areas such as rail transport, medical devices, and aerospace due to their excellent thermal stability, dielectric properties, solvent resistance, and mechanical properties. However, the epoxy sizing agent used for traditional carbon fiber cannot withstand the processing temperature of polyimide resin, of up to 350 °C, resulting in the formation of pores or defects at the interface between the fiber and the resin matrix, leading to the degradation of the overall composite properties. To overcome this problem, in this study, a low-molecular-weight thermosetting polyimide sizing agent was prepared and the processability of the sized carbon fiber was optimized by a thermoplastic polyimide. Compared with the unsized carbon fiber polyimide composites, the interfacial properties of the composites after the polyimide sizing treatment were significantly improved, with the interfacial shear strength (IFSS) increasing from 82.08 MPa to 136.27 MPa, the interlaminar shear strength (ILSS) increasing from 103.7 to 124.9 MPa, and the bending strength increasing from 2262.2 MPa to 2562.1 MPa. The sizing agent acts as a bridge between the carbon fiber and polyimide resin, with anchorage and bonding at the interface between the fiber and resin, which are beneficial for enhancing the interface performance of composites. Full article
(This article belongs to the Special Issue Research on Properties of Polymers and Their Engineering Applications)
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<p>Schematic diagram of synthesis of sizing agents and preparation of polyimide composite materials by sizing carbon fiber.</p>
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<p>Infrared spectra (<b>a</b>), TGA curve (<b>b</b>), and DSC curve (<b>c</b>) of the sizing agent and PMR-PI resin.</p>
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<p>SEM and AFM images of carbon fibers under different sizing conditions: (<b>a</b>) Desized-CF; (<b>b</b>) Epoxy-CF; (<b>c</b>) PI-CF; (<b>d</b>) PI/2%TPI-CF; (<b>e</b>) PI/4%TPI-CF; (<b>f</b>) PI/6%TPI-CF; (<b>g</b>) PI/8%TPI-CF; and (<b>h</b>) intrinsic viscosity of different sizing agents.</p>
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<p>Surface morphology of CFs after PI debonding: (<b>a</b>) Desized-CF; (<b>b</b>) Epoxy-CF; (<b>c</b>) PI-CF; (<b>d</b>) PI/4%TPI-CF; and (<b>e</b>) IFSS of CF/PI.</p>
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<p>SEM images of fracture of composites after ILSS test and flexural properties test: (<b>a1</b>–<b>a3</b>) Desized-CF; (<b>b1</b>–<b>b3</b>) Epoxy-CF; (<b>c1</b>–<b>c3</b>) PI-CF; and (<b>d1</b>–<b>d3</b>) PI/4%TPI-CF.</p>
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<p>Mechanical properties test of composites under different sizing conditions: (<b>a</b>) ILSS; (<b>b</b>) bending strength; (<b>c</b>) storage modulus in DMA; and (<b>d</b>) tan δ in DMA.</p>
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<p>Schematic diagram of interface strengthening mechanism.</p>
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15 pages, 3394 KiB  
Article
Synthesis and Characterization of Polyimide with High Blackness and Low Thermal Expansion by Introducing 3,6-bis(thiophen-2-yl)diketopyrrolopyrrole-Based Chromophores
by Yiwu Liu, Xueyuan Liu, Jinghua Tan, Jie Huang, Jiazhen Yuan, Huipeng Li, Jieping Guo, Penghao Yu and Yue Chen
Polymers 2024, 16(23), 3365; https://doi.org/10.3390/polym16233365 - 29 Nov 2024
Viewed by 463
Abstract
The market demand for black polyimide (BPI) has grown hugely in the field of flexible copper-clad laminates (FCCLs) as a replacement for transparent yellow polyimide. The 3,6-bis(thiophen-2-yl)diketopyrrolopyrroles (TDPP) derivative is recognized for its high molar extinction coefficient. In this research, we have synthesized [...] Read more.
The market demand for black polyimide (BPI) has grown hugely in the field of flexible copper-clad laminates (FCCLs) as a replacement for transparent yellow polyimide. The 3,6-bis(thiophen-2-yl)diketopyrrolopyrroles (TDPP) derivative is recognized for its high molar extinction coefficient. In this research, we have synthesized a diamine monomer named 3,6-bis[5-(4-amino-3-fluorophenyl)thiophen-2-yl]-2,5-bis(2-ethylhexyl)pyrrolo[4,3-c]pyrrole-1,4-dione (DPPTENFPDA), featuring a TDPP unit attached by fluorinated benzene rings. The subsequent reaction of DPPTENFPDA with pyromellitic dianhydride (PMDA) yielded an inherent BPI (DPPTENFPPI). By introducing chromophores derived from TDPP, the light absorption spectrum of DPPTENFPPI was broadened and red-shifted, thereby achieving full absorption within the visible spectrum and producing a highly black color that has a cut-off wavelength (λcut) of 717 nm and a CIE-Lab coordinate L* of 0.86. Additionally, DPPTENFPPI exhibited a low coefficient of thermal expansion (CTE) and remarkable thermal and electrical performance. Density functional theory calculations were conducted to explore the electronic nature of DPPTENFPPI. The outcomes revealed that the excellent light absorption of DPPTENFPPI predominantly originates from the transition from HOMO to LUMO + 1 within the chromophore moiety. The FCCL made from DPPTENFPPI films has high solder heat resistance and peel strength. This research contributes valuable insights into the structure and design of high-performance intrinsically black PIs for microelectronics applications. Full article
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<p><sup>1</sup>H NMR (<b>a</b>) and <sup>13</sup>C NMR (<b>b</b>) spectra of DPPTENFPDA in CDCl<sub>3</sub>.</p>
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<p>UV-Vis absorption spectrums of DPPTENFPDA in a DMF solution (the colored area indicates visible-light absorption. Inset: Photograph of a 5 μM DPPTENFPDA solution in DMF).</p>
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<p>(<b>a</b>) The photo images of PAA solutions and PI films with a thickness of 20 μm (DPPTENFPPI (black); Kapton (yellow)); (<b>b</b>) transmission and (<b>c</b>) absorption UV−vis spectra for DPPTENFPPI and Kapton films; (<b>d</b>) CIE lab color parameters.</p>
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<p>The frontier molecular orbitals of the DPPTENFPDA and DPPTENFPPI units.</p>
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<p>UV-Vis absorption spectra of the DPPTENFPDA and DPPTENFPPI units as predicted by the TD-DFT method, with oscillator strengths marked by vertical lines.</p>
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<p>The electronic nature of S<sub>n</sub> excitation in the DPPTENFPDA and DPPTENFPPI units based on hole and electron distribution, with the charge transfer from blue to green.</p>
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<p>DMA (<b>a</b>) and TMA (<b>b</b>) curves of the DPPTENFPPI film.</p>
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<p>Synthesis route of DPPTENFPDA (<b>A</b>) and the coloration mechanism of DPPTENFPPI (<b>B</b>).</p>
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17 pages, 4964 KiB  
Article
Laser-Induced Graphene Decorated with MOF-Derived NiCo-LDH for Highly Sensitive Non-Enzymatic Glucose Sensor
by Longxiao Li, Yufei Han, Yuzhe Zhang, Weijia Wu, Wei Du, Guojun Wen and Siyi Cheng
Molecules 2024, 29(23), 5662; https://doi.org/10.3390/molecules29235662 - 29 Nov 2024
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Abstract
Designing and fabricating a highly sensitive non-enzymatic glucose sensor is crucial for the early detection and management of diabetes. Meanwhile, the development of innovative electrode substrates has become a key focus for addressing the growing demand for constructing flexible sensors. Here, a simple [...] Read more.
Designing and fabricating a highly sensitive non-enzymatic glucose sensor is crucial for the early detection and management of diabetes. Meanwhile, the development of innovative electrode substrates has become a key focus for addressing the growing demand for constructing flexible sensors. Here, a simple one-step laser engraving method is applied for preparing laser-induced graphene (LIG) on polyimide (PI) film, which serves as the sensor substrate. NiCo-layered double hydroxides (NiCo-LDH) are synthesized on LIG as a precursor, utilizing the zeolitic imidazolate framework (ZIF-67), and then reacted with Ni(NO3)2 via solvent-thermal methods. The sensitivity of the non-enzymatic electrochemical glucose sensor is significantly improved by employing NiCo-LDH/LIG as the sensing material. The porous and interconnected structure of NiCo-LDH, derived from ZIF-67, enhances the accessibility of electrochemically active sites, while the incorporation of LIG ensures exceptional conductivity. The combination of NiCo-LDH with LIG enables efficient electron transport, leading to an increased electrochemically active surface area and enhanced catalytic efficiency. The fabricated electrode achieves a low glucose detection limit of 0.437 μM and demonstrates a high sensitivity of 1141.2 and 631.1 μA mM−2 cm−2 within the linear ranges of 0–770 μM and 770–1970 μM, respectively. Furthermore, the NiCo-LDH/LIG glucose sensor demonstrates superior reliability and little impact from other substances. A flexible integrated LIG-based non-enzymatic glucose sensor has been developed, demonstrating high sensitivity and suggesting a promising application for LIG-based chemical sensors. Full article
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Graphical abstract
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<p>Three-dimensional view of the conductivity of LIG under different laser parameters.</p>
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<p>(<b>a</b>) NiCo-LDH/LIG preparation process diagram. Low- and high-resolution SEM images of the (<b>b</b>,<b>f</b>) LIG, (<b>c</b>,<b>g</b>) Co-MOF/LIG, (<b>d</b>,<b>h</b>) and NiCo-LDH/LIG. (<b>e</b>,<b>i</b>) Low- and high-resolution TEM images of the NiCo-LDH.</p>
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<p>(<b>a</b>) LIG’s adsorption/desorption isotherm and pore size distribution. (<b>b</b>) NiCo-LDH/LIG’s adsorption/desorption isotherm and pore size distribution.</p>
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<p>(<b>a</b>) XRD patterns of the LIG, Co-MOF/LIG, and NiCo-LDH/LIG. XPS spectra of the NiCo-LDH in the (<b>b</b>) survey spectrum, (<b>c</b>) Ni 2p, and (<b>d</b>) Co 2p.</p>
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<p>(<b>a</b>) CV curves for LIG and NiCo−LDH/LIG in 0.1 M NaOH, with and without 1 mM glucose, were recorded at a scan rate of 10 mV/s. (<b>b</b>) CV curves of NiCo−LDH/LIG were obtained in solutions with 0, 1, 2, and 3 mM glucose at a scan rate of 10 mV/s. (<b>c</b>) Current responses of five successive injections of 500 μM glucose at different applied voltages. (<b>d</b>) The linear fitting results with error bars.</p>
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<p>(<b>a</b>) Comparative glucose titration experiments of NiCo-LDH/LIG, NiCo-LDH/Ag, Co-MOF/LIG, and Co-MOF/Ag at 0.5 V in 0.1 M NaOH solution. (<b>b</b>) Fitting curves with error bars for the comparative experiments.</p>
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<p>(<b>a</b>) A series of amperometric I–t curves were recorded by sequentially adding different glucose concentrations (5, 10, 20, 50, 100, 200, and 400 μM, with each concentration tested twice) to a solution at an applied potential of 0.5 V using Ag/AgCl as the RE. (<b>b</b>) Linear fitting curve of the response current with glucose concentration, including error bars. (<b>c</b>) Low concentration enlargement of (<b>a</b>). (<b>d</b>) Low concentration fitting curve in (<b>b</b>). (<b>e</b>) Current responses of NiCo-LDH/LIG upon the addition of various different interferences. (<b>f</b>) Reliability test of NiCo-LDH/LIG over 7 days.</p>
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<p>(<b>a</b>) Photograph of LIG patterns on PI and the integrated three-electrode glucose sensor device. (<b>b</b>) Amperometric I–t curves of successive additions of the same concentrations of glucose (400 μM) at an applied potential of 0.5 V. (<b>c</b>) Linear fitting curve of response current with glucose concentration.</p>
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<p>(<b>a</b>) NiCo-LDH/LIG sensor was tested with synthetic blood and glucose solution in 0.1 M NaOH solution. (<b>b</b>) Comparison test of glucose with other sugars in 0.1 M NaOH solution.</p>
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