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Keywords = room-temperature Si-Si bonding

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18 pages, 4195 KiB  
Article
Study of the Process of Sorption of Iron and Copper from Sulfuric Acid in Their Joint Presence by Natural Zeolite
by Raushan Kaiynbayeva, Raissa Chernyakova, Gita Sultanbayeva, Nazym Kozhabekova, Umirzak Jussipbekov and Ersin Tussupkaliyev
Crystals 2025, 15(6), 494; https://doi.org/10.3390/cryst15060494 - 22 May 2025
Viewed by 364
Abstract
The most promising method for the purification of concentrated technical sulfuric acid is the purification sorption method, which is the most effective and innovative, using a natural sorbent. Study of the process of sorption of iron and copper cations from concentrated technical sulfuric [...] Read more.
The most promising method for the purification of concentrated technical sulfuric acid is the purification sorption method, which is the most effective and innovative, using a natural sorbent. Study of the process of sorption of iron and copper cations from concentrated technical sulfuric acid by a natural zeolite. The specific surface area of the zeolite isolated from reactive sulfuric acid is 4.781 m2/g. The true absorption volume in the zeolite after the purification of sulfuric acid decreases to a value of 147.0068 mL/g for a zeolite sample. The adsorption pore volume for the zeolite after the acid purification calculated from the obtained results is 0.229 mL/g. The physicochemical methods of analysis (NGR, IR, X-ray diffraction, DTA, porosimetry, electron microscopy) and chemical methods revealed that in concentrated sulfuric acid the Fe–O bonds of octahedrons and SiO bonds of tetrahedrons of the zeolite framework are stable. The sorption process was carried out under conditions of a room temperature of T = 25 °C, the ratio “zeolite: H2SO4” of 10:100, and a process time of 5–50 min. The specified concentration of the Fe and Cu cations was created by introducing the calculated amount of FeSO4·7H2O and CuSO4·5H2O, in order to identify the patterns of the sorption process of copper and iron in their joint presence (CFe > CCu; CFe = CCu). The regularities of sorption of iron and copper cations by zeolite in their joint presence on the model system “H2SO4–zeolite–Fe–Cu” were studied and selective sorption capacity of zeolite with respect to iron cations was revealed. The maximum degree of sorption of iron cations in concentrated sulfuric acid is achieved in 10–15 min and makes up 95% and that of copper 30.6%. The process of iron sorption from sulfuric acid occurs according to the types of ion isomorphism and ion exchange, as indicated by a very high number of sorbed Fe ions and the absence of their release (desorption) from the zeolite into the solution. The Cu cations are sorbed by zeolite from acid by the ion exchange method, which is confirmed by the physicochemical analysis methods. Full article
(This article belongs to the Special Issue Adsorption Capabilities of Porous Materials)
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14 pages, 3406 KiB  
Article
Implication of Surface Passivation on the In-Plane Charge Transport in the Oriented Thin Films of P3HT
by Nisarg Hirens Purabiarao, Kumar Vivek Gaurav, Shubham Sharma, Yoshito Ando and Shyam Sudhir Pandey
Electron. Mater. 2025, 6(2), 6; https://doi.org/10.3390/electronicmat6020006 - 7 May 2025
Viewed by 1109
Abstract
Optimizing charge transport in organic semiconductors is crucial for advancing next-generation optoelectronic devices. The performance of organic field-effect transistors (OFETs) is significantly influenced by the alignment of films in the channel direction and the quality of the dielectric surface, which should be uniform, [...] Read more.
Optimizing charge transport in organic semiconductors is crucial for advancing next-generation optoelectronic devices. The performance of organic field-effect transistors (OFETs) is significantly influenced by the alignment of films in the channel direction and the quality of the dielectric surface, which should be uniform, smooth, and free of charge-trapping defects. Our study reports the enhancement of OFET performance using large-area, uniform, and oriented thin films of regioregular poly[3-hexylthiophene] (RR-P3HT), prepared via the Floating Film Transfer Method (FTM) on octadecyltrichlorosilane (OTS) passivated SiO2 surfaces. SiO2 surfaces inherently possess dangling bonds that act as charge traps, but these can be effectively passivated through optimized surface treatments. OTS treatment has improved the optical anisotropy of thin films and the surface wettability of SiO2. Notably, using octadecene as a solvent during OTS passivation, as opposed to toluene, resulted in a significant enhancement of charge carrier transport. Specifically, passivation with OTS-F (10 mM OTS in octadecene at 100 °C for 48 h) led to a >150 times increase in mobility and a reduction in threshold voltage compared to OTS-A (5 mM OTS in toluene for 12 h at room temperature). Under optimal conditions, these FTM-processed RR-P3HT films achieved the best device performance, with a saturated mobility (μsat) of 0.18 cm2V−1s−1. Full article
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8 pages, 18357 KiB  
Article
Wafer Bonding of GaAs and SiC via Thin Au Film at Room Temperature
by Kai Takeuchi and Eiji Higurashi
Micromachines 2025, 16(4), 439; https://doi.org/10.3390/mi16040439 - 7 Apr 2025
Viewed by 766
Abstract
Effective thermal management is a critical challenge in achieving high-power output for semiconductor laser devices. A key factor in laser device packaging is the bonding between the laser device on a GaAs substrate and a heat spreader, typically composed of high thermal conductivity [...] Read more.
Effective thermal management is a critical challenge in achieving high-power output for semiconductor laser devices. A key factor in laser device packaging is the bonding between the laser device on a GaAs substrate and a heat spreader, typically composed of high thermal conductivity materials such as SiC. Conventional soldering methods introduce thick bonding layers with relatively low thermal conductivity, resulting in high thermal resistance at the interface. In this study, we demonstrate the room temperature bonding of GaAs and SiC via a 30 nm thick Au layer, eliminating the need for a thermal reaction bonding layer or vacuum process. Using surface-activated bonding (SAB), GaAs and SiC were successfully bonded, with a strength comparable to bulk fracture. A uniform and ultrathin Au bonding interface significantly reduces thermal resistance compared to conventional soldering methods. These results highlight the potential of SAB with thin Au films as a promising approach for improving thermal management in high-power semiconductor laser devices. Full article
(This article belongs to the Special Issue Advanced Packaging for Microsystem Applications, 3rd Edition)
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12 pages, 4609 KiB  
Article
Reduction of Interface State Density in 4H-SiC MOS Capacitors Modified by ALD-Deposited Interlayers
by Zhenyu Wang, Zhaopeng Bai, Yunduo Guo, Chengxi Ding, Qimin Huang, Lin Gu, Yi Shen, Qingchun Zhang and Hongping Ma
Nanomaterials 2025, 15(7), 555; https://doi.org/10.3390/nano15070555 - 5 Apr 2025
Viewed by 754
Abstract
This study proposed an innovative method for growing gate oxide on silicon carbide (SiC), where silicon oxide (SiO2) was fabricated on a deposited Al2O3 layer, achieving high quality gate oxide. A thin Al2O3 passivation layer [...] Read more.
This study proposed an innovative method for growing gate oxide on silicon carbide (SiC), where silicon oxide (SiO2) was fabricated on a deposited Al2O3 layer, achieving high quality gate oxide. A thin Al2O3 passivation layer was deposited via atomic layer deposition (ALD), followed by Si deposition and reoxidation to fabricate a MOS structure. The effects of different ALD growth cycles on the interface chemical composition, trap density, breakdown characteristics, and bias stress stability of the MOS capacitors were systematically investigated. X-ray photoelectron spectroscopy (XPS) analyses revealed that an ALD Al2O3 passivation layer with 10 growth cycles effectively suppresses the formation of the proportion of Si-OxCy bonds. Additionally, the SiO2/Al2O3/SiC gate stack with 10 ALD growth cycles exhibited optimal electrical properties, including a minimum interface state density (Dit) value of 3 × 1011 cm−2 eV−1 and a breakdown field (Ebd) of 10.9 MV/cm. We also systematically analyzed the bias stress stability of the capacitors at room temperature and elevated temperatures. Analysis of flat-band voltage (ΔVfb) and midgap voltage (ΔVmg) hysteresis after high-temperature positive and negative bias stress demonstrated that incorporating a thin Al2O3 layer at the interface is the key factor in enhancing the stability of Vfb and midgap voltage Vmg. Full article
(This article belongs to the Section Nanoelectronics, Nanosensors and Devices)
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19 pages, 7989 KiB  
Article
Study on the Macroscopic Properties and Microstructure of High Fly Ash Content Alkali-Activated Fly Ash Slag Concrete Cured at Room Temperature
by Zhu Yuan, Yanmin Jia, Xuanben Xie and Junming Xu
Materials 2025, 18(3), 547; https://doi.org/10.3390/ma18030547 - 25 Jan 2025
Cited by 3 | Viewed by 844
Abstract
Fly ash and granulated blast furnace slag are both bulk industrial solid wastes. Using these two raw materials to completely replace cement and prepare alkali-activated fly ash slag concrete (AAFSC) at room temperature can not only efficiently utilize industrial solid waste and reduce [...] Read more.
Fly ash and granulated blast furnace slag are both bulk industrial solid wastes. Using these two raw materials to completely replace cement and prepare alkali-activated fly ash slag concrete (AAFSC) at room temperature can not only efficiently utilize industrial solid waste and reduce the carbon footprint, but also reduce the economic cost and technical difficulty of construction, which is of great significance for promoting the sustainable development of the concrete industry. In this article, the content of fly ash accounted for 80% of the total precursor (fly ash + slag), and a mixed solution of sodium silicate and sodium hydroxide was used as alkali activator to prepare AAFSC by curing at room temperature. The effects of alkali equivalent and activator modulus on compressive strength, impermeability, water absorption, and microstructure were systematically studied and compared with ordinary Portland cement concrete. The conclusions drawn were as follows. The 7-day compressive strength of AAFSC was lower than that of cement concrete, while its 28-day compressive strength was 104.86% to 131.94% of that of cement concrete. AAFSC exhibited excellent impermeability protection performance. The water absorption rate of AAFSC was lower, with A8M1 having a water absorption rate of 2.13%, which was only 60.86% of cement concrete. Through microscopic analysis, it was found that the alkali-activated fly ash slag cementitious matrix had good bonding with the aggregate, and there existed fly ash particles with different degrees of reaction. The Ca/Si value of AAFSC was smaller than that of cement concrete. Full article
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14 pages, 2584 KiB  
Article
The Mechanism Underlying the Increase in Bread Hardness in Association with Alterations in Protein and Starch Characteristics During Room-Temperature Storage
by Huaiwen Wang, Wei Liu, Peipei Zhang and Xijun Lian
Foods 2024, 13(23), 3921; https://doi.org/10.3390/foods13233921 - 4 Dec 2024
Cited by 1 | Viewed by 1140
Abstract
Hardness constitutes one of the primary performance indices of bread. However, there is scarce literature regarding the study of the mechanisms of increased hardness in different breads. In this paper, the hardness and retrogradation rates of five popular brands of bread (DaliGarden, Mankattan, [...] Read more.
Hardness constitutes one of the primary performance indices of bread. However, there is scarce literature regarding the study of the mechanisms of increased hardness in different breads. In this paper, the hardness and retrogradation rates of five popular brands of bread (DaliGarden, Mankattan, MianLunSi, TOLY, and ZhengMao) in China during storage at room temperature were determined, and the mechanism of increased hardness was revealed by the results in terms of Fourier transform infrared spectroscopy (FTIR), disulfide bonds, 13C solid-state nuclear magnetic resonance (NMR), X-ray diffraction, and differential scanning calorimetry (DSC). The results showed that the sequence for the degree of hardness increase among the five bread brands was DaliGarden > TOLY >Mankattan > MianLunSi > ZhengMao. The bread hardness was likely associated with the gliadin content; the more gliadin, the higher the hardness of the bread. All bread hardness values underwent a rapid increase during storage at room temperature. The hardness level of the bread preferred by Chinese individuals was approximately 105 g, and the hardness of the TOLY bread underwent relatively minor changes during storage at room temperature. The disulfide bond content of all breads apart from Mankattan decreased during storage at room temperature. The increase in the hardness of the bread was attributed to the ordered configuration of the amylopectin structures resulting from water evaporation. The results given in this paper offer a practical hardness index to control the quality of bread. This study is expected to contribute to better quality control and optimization in bread production, enhancing consumers’ satisfaction and extending products’ shelf lives. Full article
(This article belongs to the Special Issue Advances in the Quality and Marketability Improvement of Cereals)
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14 pages, 4268 KiB  
Article
‘Rhythmite’, Ca29(SiO4)8Cl26, an Anthropogenic Phase from the Chelyabinsk Coal Basin (Ural, Russia) with a Complex Modular Structure Related to α-Ca3SiO4Cl2 (‘Albovite’): Crystal Structure, Raman Spectra, and Thermal Expansion
by Margarita S. Avdontceva, Andrey A. Zolotarev, Anastasia S. Brazhnikova, Vladimir N. Bocharov, Natalia S. Vlasenko, Mikhail A. Rassomakhin and Sergey V. Krivovichev
Minerals 2024, 14(10), 1048; https://doi.org/10.3390/min14101048 - 18 Oct 2024
Cited by 1 | Viewed by 1110
Abstract
‘Rhythmite’, Ca29(SiO4)8Cl26, an anthropogenic calcium chloride silicate from the Chelyabinsk coal basin (South Ural, Russia), was investigated using chemical microprobe analysis, in situ single-crystal X-ray diffraction analysis (27–727 °C), and Raman spectroscopy. ‘Rhythmite’ is orthorhombic, [...] Read more.
‘Rhythmite’, Ca29(SiO4)8Cl26, an anthropogenic calcium chloride silicate from the Chelyabinsk coal basin (South Ural, Russia), was investigated using chemical microprobe analysis, in situ single-crystal X-ray diffraction analysis (27–727 °C), and Raman spectroscopy. ‘Rhythmite’ is orthorhombic, Pnma: a = 17.0749(6), b = 15.1029(5), c = 13.2907(4) Å, and V = 3427.42(18) Å3 (R1 = 0.045). The crystal structure of ‘rhythmite’ consists of a porous framework formed by Ca-O bonds and SiO4 tetrahedra with additional Ca2+ cations and Cl anions in the structure interstices. The framework is built up from multinuclear [Ca15(SiO4)4]14+ fundamental building blocks (FBBs) cut from the crystal structure of α-Ca3SiO4Cl2 (‘albovite’). The FBBs are linked by sharing common Ca atoms to form a network with an overall pcu topology. The empirical chemical formula was calculated as Ca29.02(Si7.89Al0.05P0.05)Ʃ7.99O32Cl26 (on the basis of Cl + O = 58). ‘Rhythmite’ is stable up to 627 °C and expands slightly anisotropically (αmaxmin = 1.40) in the ab and bc planes and almost isotropically in the ac plane (α3311 = 1.02) with the following thermal expansion coefficients (×106 °C−1): α11 = 14.6(1), α22 = 20.5(4), α33 = 15.0(3), and αV = 50.1(6) (room temperature). During expansion, the silicate tetrahedra remain relatively rigid with average bond length changes of less than 0.5%. A structural complexity analysis indicates that ‘rhythmite’ is complex, with IG,total = 920.313 (bits/u.c.), which significantly exceeds the average value of structural complexity for silicates and is caused by the modular framework construction and the presence of a large number of independent positions in the crystal structure. Full article
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10 pages, 2781 KiB  
Article
Interface and Size Effects of Amorphous Si/Amorphous Silicon Oxynitride Multilayer Structures on the Photoluminescence Spectrum
by Chao Song, Jie Song and Xiang Wang
Coatings 2024, 14(8), 977; https://doi.org/10.3390/coatings14080977 - 2 Aug 2024
Cited by 2 | Viewed by 1360
Abstract
A room-temperature photoluminescence (PL) study of amorphous Si/amorphous silicon oxynitride multilayer films prepared by plasma-enhanced chemical vapor deposition is reported. The PL peak position can be tuned from 800 nm to 660 nm by adjusting the oxygen/nitride ratio in the a-SiOxN [...] Read more.
A room-temperature photoluminescence (PL) study of amorphous Si/amorphous silicon oxynitride multilayer films prepared by plasma-enhanced chemical vapor deposition is reported. The PL peak position can be tuned from 800 nm to 660 nm by adjusting the oxygen/nitride ratio in the a-SiOxNy:H sublayer. The Fourier transform infrared (FTIR) absorption spectra indicate that the shift of the PL peak position is accompanied by an increase in the Si-O-Si absorption peak’s intensity, which induces the structural disorder at the interface, resulting in an increase in band gap energy. The effects of size on the photoluminescence spectrum have been studied. As a result, it has been observed that the addition of oxygen atoms introduces a large number of localized states at the interface, causing a blue shift in the emission peak position. With an increase in oxygen atoms, the localized states tend to saturate, and the quantum phenomenon caused by the a-Si sublayer becomes more pronounced. It is found that, as the thickness of the a-Si sublayer decreases, the increase in the [O/N] ratio is more likely to cause an increase in disordered states, leading to a decrease in luminescence intensity. For a-Si/a-SiOxNy:H samples with thinner a-Si sublayers, an appropriate value of [O/N] is required to achieve luminescence enhancement. When the value of [O/N] is one, the enhanced luminescence is obtained. It is also suggested that the PL originates from the radiative recombination in the localized states’ T3- level-related negatively charged silicon dangling bond in the band tail of the a-Si:H sublayer embedded in an a-Si/a-SiOxNy:H multilayer structure. Full article
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13 pages, 3193 KiB  
Article
High Emissivity MoSi2-SiC-Al2O3 Coating on Rigid Insulation Tiles with Enhanced Thermal Protection Performance
by Xukun Yang, Yange Wan, Jiancun Li, Jiachen Liu, Mingchao Wang and Xin Tao
Materials 2024, 17(1), 220; https://doi.org/10.3390/ma17010220 - 30 Dec 2023
Cited by 7 | Viewed by 2487
Abstract
High emissivity coatings with sol as the binder have the advantages of room temperature curing, good thermal shock resistance, and high emissivity; however, only silica sol has been used in the current systems. In this study, aluminum sol was used as the binder [...] Read more.
High emissivity coatings with sol as the binder have the advantages of room temperature curing, good thermal shock resistance, and high emissivity; however, only silica sol has been used in the current systems. In this study, aluminum sol was used as the binder for the first time, and MoSi2 and SiC were used as emittance agents to prepare a high emissivity MoSi2-SiC-Al2O3 coating on mullite insulation tiles. The evolution of structure and composition at 1000–1400 °C, the spectral emissivity from 200 nm to 25 μm, and the insulation performance were studied. Compared with the coating with silica sol as a binder, the MoSi2-SiC-Al2O3 coating has better structural uniformity and greater surface roughness and can generate mullite whiskers at lower temperatures. The total emissivity is 0.922 and 0.897, respectively, at the wavelength range of 200–2500 nm and 2.5–25 μm, and the superior emissivity at a low wavelength (<10 μm) is related to a higher surface roughness and reduced feature absorption. The emissivity reduction related to the oxidation of emittance agents at a high temperature (−10.2%) is smaller than that of the silica-sol-bonded coating (−18.6%). The cold surface temperature of the coated substrate is 215 °C lower than the bare substrate, suggesting excellent thermal insulation performance of the coating. Full article
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15 pages, 3576 KiB  
Article
Nickel Coatings on Ceramic Materials Using Different Diffusion Techniques
by Mala M. Sharma, Amanda M. Stutzman, Jeremy M. Schreiber, Douglas E. Wolfe and Timothy J. Eden
Coatings 2023, 13(12), 2072; https://doi.org/10.3390/coatings13122072 - 12 Dec 2023
Viewed by 1598
Abstract
Diffusion bonding is a process that has proven effective for the joining of metal to ceramic, but the differences in coefficient of thermal expansion still pose challenges during and after the bonding process. This work details the exploration of traditional diffusion-bonding processes using [...] Read more.
Diffusion bonding is a process that has proven effective for the joining of metal to ceramic, but the differences in coefficient of thermal expansion still pose challenges during and after the bonding process. This work details the exploration of traditional diffusion-bonding processes using two traditional approaches, which include bonding of a 99.9+% pure Ni foil to SiC, Si3N4, and YSZ disks using (1) a hot isostatic press (HIP), with and without added weight to promote interfacial contact, and (2) field-assisted sintering (FAST). Samples were consolidated by heating to 1200 °C and held for 6 h under vacuum before cooling to room temperature during the HIP method. For the FAST technique, bonding experiments were performed at both 800 °C and 1200 °C in a vacuum environment under 10 MPa uniaxial pressure. After the Ni was bonded to the ceramics, diffusion heat treatments were carried out in the HIP. For electroless-plated samples, the heat-treatment temperature was chosen as 825 °C to avoid melting. For electroplated samples, heat treatment occurred at 925 °C or higher. Electroplated YSZ samples were heat-treated at 1150 °C as the Ni-Si eutectic is not a concern in this system. The time at temperature varied from 6 h to 48 h depending on the material combination tested. Post-heat-treatment diffusion characteristics were analyzed using scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS). A main cause of poor bonding performance in the HIP samples was reduced interfacial contact, while cohesive failures in the FAST samples are likely due to the formation of brittle intermetallic Ni-Si phases. Preliminary results indicate success in bonding Ni to SiC, Si3N4, and YSZ using a diffusion-enhanced approach on electroplated specimens. Full article
(This article belongs to the Special Issue Nanostructured Materials Deposition Techniques and Characterization)
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12 pages, 3966 KiB  
Article
Enhanced Tribological Performance of Micro-Beam Plasma-Cladded Ni60 Coatings with Addition of Mo and Ag Lubricants in a Wide Temperature Range
by Fuxing Ye, Yufeng Zhang, Zhi Lou and Yingfan Wang
Coatings 2023, 13(12), 1996; https://doi.org/10.3390/coatings13121996 - 24 Nov 2023
Cited by 3 | Viewed by 1323
Abstract
In recent years, there has been significant attention on the application potential of medium and high-temperature self-lubricating composites as sliding parts in extreme environments. This study examines the effects of different Mo and Ag content on the composition and wear resistance of Ni60-cladded [...] Read more.
In recent years, there has been significant attention on the application potential of medium and high-temperature self-lubricating composites as sliding parts in extreme environments. This study examines the effects of different Mo and Ag content on the composition and wear resistance of Ni60-cladded coatings at room temperature, 300 °C and 600 °C, while also analyzing their wear mechanism by studying the tribofilm. The results indicate that with an appropriate weight addition of Mo and Ag, one typical lubricant called Ag2MoO4 emerges. At room temperature, the cladding layer containing 5 wt.% Mo and 5 wt.% Ag exhibits a wear rate of 2.08 × 10−6 mm3/Nm, and an average coefficient of friction (COF) of 0.3410. These two are 85% and 11% lower than those of the Ni60 cladding layer, respectively. At 300 °C, MoO3 and Cr2MoO6 act as solid lubricants. Furthermore, at 600 °C, a MoSi2 and SiO2 film forms on the worn surface to prevent further oxidation of MoSi2 and enhance oxidation resistance. The main wear mechanism is adhesion wear. Under higher temperatures, the newly formed Ag2MoO4 in the composite cladding layer adopts a layered cubic spinel structure where low-energy Ag-O bonds preferentially break during friction processes, demonstrating excellent lubrication performance. Full article
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19 pages, 3073 KiB  
Article
Electrically Detected Magnetic Resonance on a Chip (EDMRoC) for Analysis of Thin-Film Silicon Photovoltaics
by Michele Segantini, Gianluca Marcozzi, Denis Djekic, Anh Chu, Daniel Amkreutz, Cham Thi Trinh, Sebastian Neubert, Bernd Stannowski, Kerstin Jacob, Ivo Rudolph, Joseph E. McPeak, Jens Anders, Boris Naydenov and Klaus Lips
Magnetochemistry 2023, 9(7), 183; https://doi.org/10.3390/magnetochemistry9070183 - 15 Jul 2023
Cited by 5 | Viewed by 3212
Abstract
Electrically detected magnetic resonance (EDMR) is a spectroscopic technique that provides information about the physical properties of materials through the detection of variations in conductivity induced by spin-dependent processes. EDMR has been widely applied to investigate thin-film semiconductor materials in which the presence [...] Read more.
Electrically detected magnetic resonance (EDMR) is a spectroscopic technique that provides information about the physical properties of materials through the detection of variations in conductivity induced by spin-dependent processes. EDMR has been widely applied to investigate thin-film semiconductor materials in which the presence of defects can induce the current limiting processes. Conventional EDMR measurements are performed on samples with a special geometry that allows the use of a typical electron paramagnetic resonance (EPR) resonator. For such measurements, it is of utmost importance that the geometry of the sample under assessment does not influence the results of the experiment. Here, we present a single-board EPR spectrometer using a chip-integrated, voltage-controlled oscillator (VCO) array as a planar microwave source, whose geometry optimally matches that of a standard EDMR sample, and which greatly facilitates electrical interfacing to the device under assessment. The probehead combined an ultrasensitive transimpedance amplifier (TIA) with a twelve-coil array, VCO-based, single-board EPR spectrometer to permit EDMR-on-a-Chip (EDMRoC) investigations. EDMRoC measurements were performed at room temperature on a thin-film hydrogenated amorphous silicon (a-Si:H) pin solar cell under dark and forward bias conditions, and the recombination current driven by the a-Si:H dangling bonds (db) was detected. These experiments serve as a proof of concept for a new generation of small and versatile spectrometers that allow in situ and operando EDMR experiments. Full article
(This article belongs to the Special Issue Magnetic Materials, Thin Films and Nanostructures—2nd Edition)
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12 pages, 4618 KiB  
Article
RETRACTED: Influence of DETA on Thermal and Corrosion Protection Properties of GPTMS-TEOS Hybrid Coatings on Q215 Steel
by Shuanqiang Yang, Zhenzhen Jia, Jinjia Xu and Ruoyu Hong
Coatings 2023, 13(7), 1145; https://doi.org/10.3390/coatings13071145 - 24 Jun 2023
Cited by 5 | Viewed by 2310 | Retraction
Abstract
High-performance coating could be used to protect steels in engineering. The GPTMS-TEOS hybrid coatings were successfully prepared using (3-glycidoxypropyl) trimethoxysilane (GPTMS) and tetraethylorthosilicate (TEOS) as reaction raw materials and diethylenetriamine (DETA) as both a curing agent and catalyst at room temperature. The hybrid [...] Read more.
High-performance coating could be used to protect steels in engineering. The GPTMS-TEOS hybrid coatings were successfully prepared using (3-glycidoxypropyl) trimethoxysilane (GPTMS) and tetraethylorthosilicate (TEOS) as reaction raw materials and diethylenetriamine (DETA) as both a curing agent and catalyst at room temperature. The hybrid coating contained amorphous SiO2 and was characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The DETA content of the hybrid coating has a significant impact on the performance of the coating. As the DETA content increases, the thermal stability of the hybrid coating increases at 400–600 °C due to the production of more SiO2 in the amine-rich state. However, the gelation time decreases dramatically, preventing the hybrid coating from better infiltrating the surface of the steel substrate. In addition, there are not enough silicon hydroxyl groups to bond with the hydroxyl groups on the surface of carbon steel and adhesion is significantly reduced. Therefore, hybrid coatings with a moderate DETA content (NH:epoxy ratio equivalent to 1:1) show the best corrosion resistance, with a third-order magnitude increase in corrosion resistance compared to that of carbon steel. Full article
(This article belongs to the Topic Characterization of Electrochemical Materials)
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20 pages, 2082 KiB  
Article
Molecular Structures and Intermolecular Hydrogen Bonding of Silylated 2-Aminopyrimidines
by Marcus Herbig, Edwin Kroke and Jörg Wagler
Crystals 2023, 13(7), 990; https://doi.org/10.3390/cryst13070990 - 21 Jun 2023
Viewed by 2012
Abstract
A series of silylated 2-aminopyrimidines Me(4−n)Si(NHpyr)n (Me = methyl, NHpyr = pyrimid-2-ylamino, n = 1, 2, 3, 4), i.e., compounds 1, 2, 3, and 4, respectively, was prepared from a series of the respective [...] Read more.
A series of silylated 2-aminopyrimidines Me(4−n)Si(NHpyr)n (Me = methyl, NHpyr = pyrimid-2-ylamino, n = 1, 2, 3, 4), i.e., compounds 1, 2, 3, and 4, respectively, was prepared from a series of the respective chlorosilanes Me(4−n)SiCln and 2-aminopyrimidine. Triethylamine was used as a sacrificial base. Compounds 1, 2, 3, and 4 are solid at room temperature. They were analyzed using 1H, 13C, 29Si NMR, and Raman spectroscopy, and their molecular structures were confirmed by single-crystal X-ray diffraction analyses. All structures exhibit intramolecular van der Waals contacts between the silicon atom and one nitrogen atom of the pyrimidine moiety. Thus, their Si coordination spheres can be interpreted as [4+n] coordinated capped tetrahedra. Intermolecular hydrogen bonds (N–H···N bridges between the Si-bound amino groups and the non-Si-capping pyrimidine N atoms) are a constant contributor to the solid-state structures of these compounds. Furthermore, compounds 2 and 4 exhibit N–H···N bridges which involve 50% of their Si-capping N atoms as hydrogen bridge acceptors. Consequently, 50% of the non-Si-capping pyrimidine N atoms are stabilized by C–H···N contacts. As a result of a particularly dense network of intermolecular hydrogen bridges, the melting point of Si(NHpyr)4 (compound 4) is higher than 300 °C. Full article
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17 pages, 6024 KiB  
Article
Temperature Induced Monoclinic to Orthorhombic Phase Transition in Protonated ZSM-5 Zeolites with Different Si/Al Ratios: An In-Situ Synchrotron X-ray Powder Diffraction Study
by Nicola Precisvalle, Maura Mancinelli, Matteo Ardit, Giada Beltrami, Lara Gigli, Alfredo Aloise, Enrico Catizzone, Massimo Migliori, Girolamo Giordano, Vincenzo Guidi and Annalisa Martucci
Crystals 2023, 13(6), 979; https://doi.org/10.3390/cryst13060979 - 20 Jun 2023
Cited by 3 | Viewed by 2466
Abstract
ZSM-5 zeolite is the synthetic counterpart to mutinaite. After thermal activation of the as-synthesized form, the symmetry of the ZSM-5 zeolite is lowered to the monoclinic P21/n. ZSM-5 then undergoes a polymorphic displacive phase transition from the monoclinic [...] Read more.
ZSM-5 zeolite is the synthetic counterpart to mutinaite. After thermal activation of the as-synthesized form, the symmetry of the ZSM-5 zeolite is lowered to the monoclinic P21/n. ZSM-5 then undergoes a polymorphic displacive phase transition from the monoclinic P21/n to the orthorhombic Pnma, Pn21a or P212121 space groups, which occurs upon heating. This phase transition can be influenced by factors such as the type and amount of sorbate molecules present in the zeolite channels. ZSM-5 has many applications, including as a catalyst or sorbent in various industries, where high thermal stability is required. In this study, four ZSM-5 zeolites with different Si/Al ratios were investigated by synchrotron X-ray powder diffraction at both room temperature and high temperature conditions to determine the effects of chemical composition on the structural response of the zeolite lattice. The results showed that the ZSM-5 zeolites retained their crystallinity and structural features throughout the thermal treatment, indicating that they could be used as effective acid catalysts. Distortions in the zeolite framework can occur after TPA+ decomposition and thermal activation, affecting thermal regeneration and efficiency. The charge balance in ZSM-5 is achieved by the formation of Brønsted acid sites, and variations in bonding geometries are influenced by the initial Si/Al ratio. Full article
(This article belongs to the Special Issue Young Crystallographers Across Europe)
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