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Keywords = thermal atomic layer deposition

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25 pages, 15569 KiB  
Article
Studies on the Chemical Etching and Corrosion Resistance of Ultrathin Laminated Alumina/Titania Coatings
by Ivan Netšipailo, Lauri Aarik, Jekaterina Kozlova, Aivar Tarre, Maido Merisalu, Kaisa Aab, Hugo Mändar, Peeter Ritslaid and Väino Sammelselg
Corros. Mater. Degrad. 2025, 6(3), 36; https://doi.org/10.3390/cmd6030036 - 2 Aug 2025
Viewed by 210
Abstract
We investigated the protective properties of ultrathin laminated coatings, comprising three pairs of Al2O3 and TiO2 sublayers with coating thicknesses < 150 nm, deposited on AISI 310 stainless steel (SS) and Si (100) substrates at 80–500 °C by atomic [...] Read more.
We investigated the protective properties of ultrathin laminated coatings, comprising three pairs of Al2O3 and TiO2 sublayers with coating thicknesses < 150 nm, deposited on AISI 310 stainless steel (SS) and Si (100) substrates at 80–500 °C by atomic layer deposition. The coatings were chemically etched and subjected to corrosion, ultrasound, and thermal shock tests. The coating etching resistance efficiency (Re) was determined by measuring via XRF the change in the coating sublayer mass thickness after etching in hot 80% H2SO4. The maximum Re values of ≥98% for both alumina and titania sublayers were obtained for the laminates deposited at 250–400 °C on both substrates. In these coatings, the titania sublayers were crystalline. The lowest Re values of 15% and 50% for the alumina and titania sublayers, respectively, were measured for laminate grown at 80 °C on silicon. The coatings deposited at 160–200 °C demonstrated a delay in the increase of Re values, attributed to the changes in the titania sublayers before full crystallization. Coatings grown at higher temperatures were also more resistant to ultrasound and liquid nitrogen treatments. In contrast, coatings deposited at 125 °C on SS had better corrosion protection, as demonstrated via electrochemical impedance spectroscopy and a standard immersion test in FeCl3 solution. Full article
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13 pages, 3623 KiB  
Article
Fabrication and Characterization of Ferroelectric Capacitors with a Symmetric Hybrid TiN/W/HZO/W/TiN Electrode Structure
by Ha-Jung Kim, Jae-Hyuk Choi, Seong-Eui Lee, So-Won Kim and Hee-Chul Lee
Materials 2025, 18(15), 3547; https://doi.org/10.3390/ma18153547 - 29 Jul 2025
Viewed by 252
Abstract
In this study, Hf0.5Zr0.5O2 (HZO) thin-films were deposited using a Co-plasma atomic layer deposition (CPALD) process that combined both remote plasma and direct plasma, for the development of ferroelectric memory devices. Ferroelectric capacitors with a symmetric hybrid TiN/W/HZO/W/TiN [...] Read more.
In this study, Hf0.5Zr0.5O2 (HZO) thin-films were deposited using a Co-plasma atomic layer deposition (CPALD) process that combined both remote plasma and direct plasma, for the development of ferroelectric memory devices. Ferroelectric capacitors with a symmetric hybrid TiN/W/HZO/W/TiN electrode structure, incorporating W electrodes as insertion layers, were fabricated. Rapid thermal annealing (RTA) was subsequently employed to control the crystalline phase of the films. The electrical and structural properties of the capacitors were analyzed based on the RTA temperature, and the presence, thickness, and position of the W insertion electrode layer. Consequently, the capacitor with 5 nm-thick W electrode layers inserted on both the top and bottom sides and annealed at 700 °C exhibited the highest remnant polarization (2Pr = 61.0 μC/cm2). Moreover, the symmetric hybrid electrode capacitors annealed at 500–600 °C also exhibited high 2Pr values of approximately 50.4 μC/cm2, with a leakage current density of approximately 4 × 10−5 A/cm2 under an electric field of 2.5 MV/cm. The findings of this study are expected to contribute to the development of electrode structures for improved performance of HZO-based ferroelectric memory devices. Full article
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22 pages, 10488 KiB  
Article
Morphological and Functional Evolution of Amorphous AlN Thin Films Deposited by RF-Magnetron Sputtering
by Maria-Iulia Zai, Ioana Lalau, Marina Manica, Lucia Chiriacescu, Vlad-Andrei Antohe, Cristina C. Gheorghiu, Sorina Iftimie, Ovidiu Toma, Mirela Petruta Suchea and Ștefan Antohe
Surfaces 2025, 8(3), 51; https://doi.org/10.3390/surfaces8030051 - 17 Jul 2025
Viewed by 314
Abstract
Aluminum nitride (AlN) thin films were deposited on SiO2 substrates by RF-magnetron sputtering at varying powers (110–140 W) and subsequently subjected to thermal annealing at 450 °C under nitrogen atmosphere. A comprehensive multi-technique investigation—including X-ray reflectometry (XRR), X-ray diffraction (XRD), scanning electron [...] Read more.
Aluminum nitride (AlN) thin films were deposited on SiO2 substrates by RF-magnetron sputtering at varying powers (110–140 W) and subsequently subjected to thermal annealing at 450 °C under nitrogen atmosphere. A comprehensive multi-technique investigation—including X-ray reflectometry (XRR), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), optical profilometry, spectroscopic ellipsometry (SE), and electrical measurements—was performed to explore the physical structure, morphology, and optical and electrical properties of the films. The analysis of the film structure by XRR revealed that increasing sputtering power resulted in thicker, denser AlN layers, while thermal treatment promoted densification by reducing density gradients but also induced surface roughening and the formation of island-like morphologies. Optical studies confirmed excellent transparency (>80% transmittance in the near-infrared region) and demonstrated the tunability of the refractive index with sputtering power, critical for optoelectronic applications. The electrical characterization of Au/AlN/Al sandwich structures revealed a transition from Ohmic to trap-controlled space charge limited current (SCLC) behavior under forward bias—a transport mechanism frequently present in a material with very low mobility, such as AlN—while Schottky conduction dominated under reverse bias. The systematic correlation between deposition parameters, thermal treatment, and the resulting physical properties offers valuable pathways to engineer AlN thin films for next-generation optoelectronic and high-frequency device applications. Full article
(This article belongs to the Special Issue Surface Engineering of Thin Films)
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30 pages, 4865 KiB  
Article
Thermal Behavior and Smoke Suppression of Polyamide 6,6 Fabric Treated with ALD-ZnO and DOPO-Based Silane
by Wael Ali, Raphael Otto, Ana Raquel Lema Jimenez, Sebastian Lehmann, Eui-Young Shin, Ying Feng, Milijana Jovic, Sabyasachi Gaan, Jochen S. Gutmann, Kornelius Nielsch, Amin Bahrami and Thomas Mayer-Gall
Materials 2025, 18(13), 3195; https://doi.org/10.3390/ma18133195 - 7 Jul 2025
Viewed by 638
Abstract
Polyamide 6,6 (PA6,6) fabrics are widely used in textiles due to their high mechanical strength and chemical stability. However, their inherent flammability and melting behavior under fire pose significant safety challenges. In this study, a dual-layer flame-retardant system was developed by integrating atomic [...] Read more.
Polyamide 6,6 (PA6,6) fabrics are widely used in textiles due to their high mechanical strength and chemical stability. However, their inherent flammability and melting behavior under fire pose significant safety challenges. In this study, a dual-layer flame-retardant system was developed by integrating atomic layer deposition (ALD) of ZnO with a phosphorus–silane-based flame retardant (DOPO-ETES). ALD allowed precise control of ZnO layer thickness (50, 84, and 199 nm), ensuring uniform coating. Thermal analysis (TGA) and microscale combustion calorimetry (MCC) revealed that ZnO altered the degradation pathway of PA6,6 through catalytic effects, promoting char formation and reducing heat release. The combination of ZnO and DOPO-ETES resulted in further reductions in heat release rates. However, direct flame tests showed that self-extinguishing behavior was not achieved, emphasizing the limitations related to the melting of PA6,6. TG-IR and cone calorimetry confirmed that ZnO coatings suppressed the release of smoke-related volatiles and incomplete combustion products. These findings highlight the potential of combining metal-based catalytic flame retardants like ZnO with phosphorus-based coatings to improve flame retardancy while addressing the specific challenges of polyamide textiles. This approach may also be adapted to other fabric types and integrated with additional flame retardants, broadening its relevance for textile applications. Full article
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15 pages, 5997 KiB  
Article
Novel 3D Capacitors: Integrating Porous Nickel-Structured and Through-Glass-Via-Fabricated Capacitors
by Baichuan Zhang, Libin Gao, Hongwei Chen and Jihua Zhang
Nanomaterials 2025, 15(11), 819; https://doi.org/10.3390/nano15110819 - 28 May 2025
Viewed by 412
Abstract
In this research work, two distinct types of three-dimensional (3D) capacitors were successfully fabricated, each with its own unique features and advantages. The first type of capacitor is centered around a 3D nanoporous structure. This structure is formed on a nickel substrate through [...] Read more.
In this research work, two distinct types of three-dimensional (3D) capacitors were successfully fabricated, each with its own unique features and advantages. The first type of capacitor is centered around a 3D nanoporous structure. This structure is formed on a nickel substrate through anodic oxidation. After undergoing high-temperature thermal oxidation, a monolithic Ni-NiO-Pt metal–insulator–metal (MIM) capacitor with a nanoporous dielectric architecture is achieved. Structurally, this innovative design brings about several remarkable benefits. Due to the nanoporous structure, it has a significantly increased surface area, which can effectively store more charges. As a result, it exhibits an equivalent capacitance density of 69.95 nF/cm2, which is approximately 18 times higher than that of its planar, non-porous counterpart. This high capacitance density enables it to store more electrical energy in a given volume, making it highly suitable for applications where miniaturization and high energy storage in a small space is crucial. The second type of capacitor makes use of Through-Glass Via (TGV) technology. This technology is employed to create an interdigitated blind-via array within a glass substrate, attaining an impressively high aspect ratio of 22.5:1 (with a via diameter of 20 μm and a depth of 450 μm). By integrating atomic layer deposition (ALD), a conformal interdigital electrode structure is realized. Glass, as a key material in this capacitor, has outstanding insulating properties. This characteristic endows the capacitor with a high breakdown field strength exceeding 8.2 MV/cm, corresponding to a withstand voltage of 5000 V. High breakdown field strength and withstand voltage mean that the capacitor can handle high-voltage applications without breaking down easily, which is essential for power-intensive systems like high-voltage power supplies and some high-power pulse-generating equipment. Moreover, due to the low-loss property of glass, the capacitor can achieve an energy conversion efficiency of up to 95%. Such a high energy conversion efficiency ensures that less energy is wasted during the charge–discharge process, which is highly beneficial for energy-saving applications and systems that require high-efficiency energy utilization. Full article
(This article belongs to the Section Nanoelectronics, Nanosensors and Devices)
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13 pages, 3697 KiB  
Article
Interfacial Chemical and Electrical Performance Study and Thermal Annealing Refinement for AlTiO/4H-SiC MOS Capacitors
by Yu-Xuan Zeng, Wei Huang, Hong-Ping Ma and Qing-Chun Zhang
Nanomaterials 2025, 15(11), 814; https://doi.org/10.3390/nano15110814 - 28 May 2025
Viewed by 385
Abstract
The gate reliability issues in SiC-based devices with a gate dielectric formed through heat oxidation are important factors limiting their application in power devices. Aluminum oxide (Al2O3) and titanium dioxide (TiO2) were combined using the ALD process [...] Read more.
The gate reliability issues in SiC-based devices with a gate dielectric formed through heat oxidation are important factors limiting their application in power devices. Aluminum oxide (Al2O3) and titanium dioxide (TiO2) were combined using the ALD process to form a composite AlTiO gate dielectric on a 4H-SiC substrate. TDMAT and TMA were the precursors selected and deposited at 200 °C, and the samples were Ar or N2 annealed at temperatures ranging from 300 °C to 700 °C. An XPS analysis suggested that the AlTiO film had been deposited with a high overall quality and the involvement of Ti atoms had increased the interfacial bonding with the substrate. The as-deposited MOS structure had band shifts of ΔEC = 1.08 eV and ΔEV = 2.41 eV. After annealing, the AlTiO bandgap increased by 0.85 eV at most, and better band alignment was attained. Leakage current and breakdown voltage characteristic investigations were conducted after Al electrode deposition. The leakage current density and electrical breakdown field of an MOS capacitor structure with a SiC substrate were ~10−3 A/cm2 and 6.3 MV/cm, respectively. After the annealing process, both the measures of the JV performance of the MOS capacitor had improved to ~10−6 A/cm2 and 7.2 MV/cm. The interface charge Neff of the AlTiO layer was 4.019 × 1010 cm−2. The AlTiO/SiC structure fabricated in this work proved the feasibility of adjusting the properties of single-component gate dielectric materials using the ALD method, and using a suitable thermal annealing process has great potential to improve the performance of the compound MOS dielectric layer. Full article
(This article belongs to the Special Issue Advanced Studies in Wide-Bandgap Nanomaterials and Devices)
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14 pages, 3791 KiB  
Article
Deposition of HfO2 by Remote Plasma ALD for High-Aspect-Ratio Trench Capacitors in DRAM
by Jiwon Kim, Inkook Hwang, Byungwook Kim, Wookyung Lee, Juha Song, Yeonwoong Jung and Changbun Yoon
Nanomaterials 2025, 15(11), 783; https://doi.org/10.3390/nano15110783 - 23 May 2025
Viewed by 1039
Abstract
Dynamic random-access memory (DRAM) is a vital component in modern computing systems. Enhancing memory performance requires maximizing capacitor capacitance within DRAM cells, which is achieved using high-k dielectric materials deposited as thin, uniform films via atomic layer deposition (ALD). Precise film deposition that [...] Read more.
Dynamic random-access memory (DRAM) is a vital component in modern computing systems. Enhancing memory performance requires maximizing capacitor capacitance within DRAM cells, which is achieved using high-k dielectric materials deposited as thin, uniform films via atomic layer deposition (ALD). Precise film deposition that minimizes electronic defects caused by charged vacancies is essential for reducing leakage current and ensuring high dielectric strength. In this study, we fabricated metal–insulator–metal (MIM) capacitors in high-aspect-ratio trench structures using remote plasma ALD (RP-ALD) and direct plasma ALD (DP-ALD). The trenches, etched into silicon, featured a 7:1 aspect ratio, 76 nm pitch, and 38 nm critical dimension. We evaluated the electrical characteristics of HfO2-based capacitors with TiN top and bottom electrodes, focusing on leakage current density and equivalent oxide thickness. Capacitance–voltage analysis and X-ray photoelectron spectroscopy (XPS) revealed that RP-ALD effectively suppressed plasma-induced damage, reducing defect density and leakage current. While DP-ALD offered excellent film properties, it suffered from degraded lateral uniformity due to direct plasma exposure. Given its superior lateral uniformity, lower leakage, and defect suppression, RP-ALD shows strong potential for improving DRAM capacitor performance and serves as a promising alternative to the currently adopted thermal ALD process. Full article
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24 pages, 5625 KiB  
Review
A Review of High-Temperature Resistant Silica Aerogels: Structural Evolution and Thermal Stability Optimization
by Zhenyu Zhu, Wanlin Zhang, Hongyan Huang, Wenjing Li, Hao Ling and Hao Zhang
Gels 2025, 11(5), 357; https://doi.org/10.3390/gels11050357 - 13 May 2025
Cited by 1 | Viewed by 1560
Abstract
Silica aerogels exhibit exceptionally low thermal conductivity and a low apparent density, as they are unique porous nanomaterials. They are extensively used in thermal insulation in terms of aerospace and building construction, adsorption processes for environmental applications, concentrating solar power systems, and so [...] Read more.
Silica aerogels exhibit exceptionally low thermal conductivity and a low apparent density, as they are unique porous nanomaterials. They are extensively used in thermal insulation in terms of aerospace and building construction, adsorption processes for environmental applications, concentrating solar power systems, and so on. However, the degradation of the silica aerogel’s nanoporous structure at high temperatures seriously restricts their practical applications. Through a comprehensive review of the high-temperature structural evolution and sintering mechanisms of silica aerogels, this paper introduces two strategies to enhance their thermal stability, including heteroatom doping and surface heterogeneous structure construction. In particular, atomic layer deposition (ALD) of ultra-thin coatings on silica aerogel holds significant potential for enhancing thermal stability, while preserving its ultra-low thermal conductivity. Full article
(This article belongs to the Special Issue Advanced Aerogels: From Design to Application)
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13 pages, 2642 KiB  
Review
Advancements in Inorganic Hole-Transport Materials for Perovskite Solar Cells: A Comparative Review
by Johannes Zanoxolo Mbese
Energies 2025, 18(9), 2374; https://doi.org/10.3390/en18092374 - 6 May 2025
Viewed by 957
Abstract
Single-junction perovskite solar cells (PSCs) have been one of the most promising photovoltaic technologies owing to their high-power conversion efficiencies (PCEs) of ~27% and the low-cost fabrication processes involved, which pay off significantly given their distinct structural characteristics. Recently, inorganic hole-transport materials (HTMs) [...] Read more.
Single-junction perovskite solar cells (PSCs) have been one of the most promising photovoltaic technologies owing to their high-power conversion efficiencies (PCEs) of ~27% and the low-cost fabrication processes involved, which pay off significantly given their distinct structural characteristics. Recently, inorganic hole-transport materials (HTMs) such as nickel oxide (NiOx) have been developed and received considerable attention for use in OPVs due to their excellent thermal stability, low-cost materials, and compatibility with scalable deposition methods. Here, we summarize the recent progress on inorganic HTMs for PSCs, which can be divided into three categories: NiOx, copper-based compounds, and emerging new alternatives. The deposition method (sputtering, atomic layer deposition, or a solution-based technique) is one of the most important factors affecting the performance and stability of PSCs. Finally, we review interfacial engineering strategies, such as surface modifications and doping, which can enhance charge transport and extend a device’s lifetime. We also balance the benefits of inorganic HTMs against the key challenges in advancing to commercialization, namely interior defects and environmental degradation. In this review, we summarize the recent progress and challenges toward developing cost-efficient and stable PSCs with inorganic HTMs and provide insights into the future development of these materials. Full article
(This article belongs to the Section A2: Solar Energy and Photovoltaic Systems)
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15 pages, 6305 KiB  
Article
A Study on the Spectral Characteristics of 83.4 nm Extreme Ultraviolet Filters
by Qian Liu, Aiming Zhou, Hanlin Wang, Pingxu Wang, Chen Tao, Guang Zhang, Xiaodong Wang and Bo Chen
Coatings 2025, 15(5), 535; https://doi.org/10.3390/coatings15050535 - 30 Apr 2025
Viewed by 617
Abstract
Extreme ultraviolet (EUV) imagers are key tools to monitor the space environment and forecast space weather. EUV filters are important components to block radiation in the ultraviolet (UV), visible, and near-infrared (IR) regions. In this study, various characterization methods were proposed for the [...] Read more.
Extreme ultraviolet (EUV) imagers are key tools to monitor the space environment and forecast space weather. EUV filters are important components to block radiation in the ultraviolet (UV), visible, and near-infrared (IR) regions. In this study, various characterization methods were proposed for the nickel mesh-supported indium (In) filter, and their spectral characteristics were comprehensively studied. The material and thickness of the filter were chosen based on atomic scattering principles, determined through theoretical calculation and software simulation. The metal film was deposited using the vacuum-resistive thermal evaporation method. The measured transmission of the filter was 10.06% at 83.4 nm. The surface elements of the sample were analyzed using X-ray photoelectron spectroscopy (XPS). The surface and cross-sectional morphologies of the filter were observed using a scanning electron microscope (SEM). The impact of the oxide layer and carbon contamination on the filter’s transmittance was investigated using an ellipsometer. A multilayer “In-In2O3-C” model was established to determine the thickness of both the oxide layer and carbon contamination layer on the filter. This model introduces the filling factor based on the original model and considers the diffusion of the contamination layer, resulting in more accurate fitting results. The transmittance of the filter in the visible light range was measured using a UV-VIS spectrophotometer, and the measurement error was analyzed. This article provides preparation methods and test methods for the 83.4 nm EUV filter and conducts a detailed analysis of the spectral characteristics of the prepared optical filters, which hold significant value for space exploration applications. Full article
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15 pages, 8949 KiB  
Article
Ellipsometric Surface Oxidation Model of ALD-Grown Vanadium Oxide Mixed-Valence System
by Xiaojie Sun, Shuguang Wang, Qingyuan Cai, Jingze Liu, Changhai Li, Ertao Hu, Jing Li, Songyou Wang, Yuxiang Zheng, Liangyao Chen and Youngpak Lee
Nanomaterials 2025, 15(9), 645; https://doi.org/10.3390/nano15090645 - 24 Apr 2025
Viewed by 484
Abstract
Vanadium and oxygen form a complex system of vanadium oxides with multiple phases and mixed valency, increasing the difficulty of characterization. In this work, amorphous vanadium oxide thin films with mixed valence states were fabricated by atomic layer deposition, and then post-annealing was [...] Read more.
Vanadium and oxygen form a complex system of vanadium oxides with multiple phases and mixed valency, increasing the difficulty of characterization. In this work, amorphous vanadium oxide thin films with mixed valence states were fabricated by atomic layer deposition, and then post-annealing was conducted for crystalline films. For the surface analysis of this mixed-valence system, X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) were employed. However, XPS is only able to quasi-quantitatively determine the surface-proximity oxidation states. To account for the inadequacy of surface-sensitive XPS and AES techniques, a surface oxidation model (SOM) was proposed for the ellipsometric modeling of the mixed-valence system. Furthermore, by conducting air thermal oxidation (ATO) experiments, the four sets of fitting parameters of SOM were decreased to three, lowering the system complexity. This study is expected to help with the analysis of vanadium oxide mixed-valence systems and other multivalent metal oxide systems. Full article
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14 pages, 7415 KiB  
Article
Enhancing Thermal Conductivity of SiC Matrix Pellets for Accident-Tolerant Fuel via Atomic Layer Deposition of Al2O3 Coating
by Yumeng Zhao, Wenqing Wang, Jiquan Wang, Xiao Liu, Yu Li, Zongshu Li, Rong Chen and Wei Liu
Energies 2025, 18(8), 2130; https://doi.org/10.3390/en18082130 - 21 Apr 2025
Viewed by 396
Abstract
This study investigates the enhancement of thermal conductivity in silicon carbide (SiC) matrix pellets for accident-tolerant fuels via atomic layer deposition (ALD) of alumina (Al2O3) coatings. Pressure-holding ALD protocols ensured precursor saturation, enabling precise coating control (0.09 nm/cycle). The [...] Read more.
This study investigates the enhancement of thermal conductivity in silicon carbide (SiC) matrix pellets for accident-tolerant fuels via atomic layer deposition (ALD) of alumina (Al2O3) coatings. Pressure-holding ALD protocols ensured precursor saturation, enabling precise coating control (0.09 nm/cycle). The ALD-coated Al2O3 layers on SiC particles were found to be more uniform while minimizing surface oxidation compared to traditional mechanical mixing. Combined with yttria (Y2O3) additives and spark plasma sintering (SPS), ALD-coated samples achieved satisfactory densification and thermal performance. Results demonstrated that 5~7 wt.% ALD-Al2O3 + Y2O3 achieved corrected thermal conductivity enhancements of 14~18% at 100 °C., even with reduced sintering aid content, while maintaining sintered densities above 92% T.D. (theoretical density). This work highlights ALD’s potential in fabricating high-performance, accident-tolerant SiC-based fuels for safer and more efficient nuclear reactors, with implications for future optimization of sintering processes and additive formulations. Full article
(This article belongs to the Section B4: Nuclear Energy)
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13 pages, 4511 KiB  
Article
Crystallographic Engineering of CrN Buffer Layers for GaN Thin Film Epitaxy
by Kyu-Yeon Shim, Seongho Kang, Min-Joo Ahn, Yukyeong Cha, Eojin-Gyere Ham, Dohoon Kim and Dongjin Byun
Materials 2025, 18(8), 1817; https://doi.org/10.3390/ma18081817 - 16 Apr 2025
Viewed by 532
Abstract
Gallium nitride (GaN) is commonly used in various semiconductor systems owing to its high mobility and thermal stability; however, the production of GaN thin films using the currently employed methods requires improvement. To facilitate the growth of high-quality GaN epitaxial thin films, this [...] Read more.
Gallium nitride (GaN) is commonly used in various semiconductor systems owing to its high mobility and thermal stability; however, the production of GaN thin films using the currently employed methods requires improvement. To facilitate the growth of high-quality GaN epitaxial thin films, this study explored the crystallographic structures, properties, and influences of chromium nitride (CrN) buffer layers sputtered under various conditions. The crystallographic orientation of CrN played a crucial role in determining the GaN film quality. For example, even when the crystallinity of the CrN (111) plane was relatively low, a single-phase CrN (111) buffer layer could provide a more favorable template for GaN epitaxy compared to cases where both the CrN (111) and Cr2N (110) phases coexisted. The significance of a low-temperature (LT) GaN nucleation layer deposited onto the CrN buffer layers was assessed using atomic force microscopy and contact angle measurements. The X-ray phi scan results confirmed the six-fold symmetry of the grown GaN, further emphasizing the contribution of an LT-GaN nucleation layer. These findings offer insights into the underlying mechanisms governing GaN thin film growth and provide guidance for the optimization of the buffer layer conditions to achieve high-quality GaN epitaxial films. Full article
(This article belongs to the Section Thin Films and Interfaces)
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17 pages, 5590 KiB  
Article
A Critical Comparison Among High-Resolution Methods for Spatially Resolved Nano-Scale Residual Stress Analysis in Nanostructured Coatings
by Saqib Rashid, Edoardo Rossi, Spyros Diplas, Patricia Almeida Carvalho, Damian Pucicki, Rafal Kuna and Marco Sebastiani
Int. J. Mol. Sci. 2025, 26(7), 3296; https://doi.org/10.3390/ijms26073296 - 2 Apr 2025
Cited by 1 | Viewed by 730
Abstract
Residual stresses in multilayer thin coatings represent a complex multiscale phenomenon arising from the intricate interplay of multiple factors, including the number and thickness of layers, material properties of the layers and substrate, coefficient of thermal expansion (CTE) mismatch, deposition technique and growth [...] Read more.
Residual stresses in multilayer thin coatings represent a complex multiscale phenomenon arising from the intricate interplay of multiple factors, including the number and thickness of layers, material properties of the layers and substrate, coefficient of thermal expansion (CTE) mismatch, deposition technique and growth mechanism, as well as process parameters and environmental conditions. A multiscale approach to residual stress measurement is essential for a comprehensive understanding of stress distribution in such systems. To investigate this, two AlGaN/GaN multilayer coatings with distinct layer architectures were deposited on sapphire substrates using metalorganic vapor phase epitaxy (MOVPE). High-resolution X-ray diffraction (HRXRD) was employed to confirm their epitaxial growth and structural characteristics. Focused ion beam (FIB) cross-sectioning and transmission electron microscopy (TEM) lamella preparation were performed to analyze the coating structure and determine layer thickness. Residual stresses within the multilayer coatings were evaluated using two complementary techniques: High-Resolution Scanning Transmission Electron Microscopy—Graphical Phase Analysis (HRSTEM-GPA) and Focused Ion Beam—Digital Image Correlation (FIB-DIC). HRSTEM-GPA enables atomic-resolution strain mapping, making it particularly suited for investigating interface-related stresses, while FIB-DIC facilitates microscale stress evaluation. The residual strain values obtained using the FIB-DIC and HRSTEM-GPA methods were −3.2 × 10⁻3 and −4.55 × 10⁻3, respectively. This study confirms that residual stress measurements at different spatial resolutions are both reliable and comparable at the required coating depths and locations, provided that a critical assessment of the characteristic scale of each method is performed. Full article
(This article belongs to the Special Issue Nanomaterials in Novel Thin Films and Coatings)
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12 pages, 3737 KiB  
Article
The Influence of Thermal Annealing on the Chemical Composition, Nanomechanical, and Nanotribological Properties of Tantalum Thin Films
by Debottam Datta, Ali Eskandari, Junaid Syed, Himanshu Rai, Nitya Nand Gosvami and Ting Y. Tsui
Micromachines 2025, 16(4), 427; https://doi.org/10.3390/mi16040427 - 2 Apr 2025
Viewed by 724
Abstract
Tantalum metal and tantalum oxide thin films are commonly used in semiconductor devices, protective coatings, and biomedical implants. However, there is limited information on their nanotribological behavior and small-scale mechanical properties. This study characterized the chemical, mechanical, and tribological properties of as-deposited and [...] Read more.
Tantalum metal and tantalum oxide thin films are commonly used in semiconductor devices, protective coatings, and biomedical implants. However, there is limited information on their nanotribological behavior and small-scale mechanical properties. This study characterized the chemical, mechanical, and tribological properties of as-deposited and 400 °C annealed β-Ta thin films using nanoindentation and atomic force microscope (AFM)-based nanoscale friction and wear tests. X-ray photoelectron spectroscopy (XPS) results revealed that a thermally grown Ta oxide layer forms on the surface of Ta film after being annealed at 400 °C. The nanoindentation data indicated an increase in both the hardness and elastic modulus in the heat-treated sample compared to the as-deposited Ta film (13.1 ± 1.3 GPa vs. 12.0 ± 1.4 GPa for hardness) and (213.1 ± 12.7 GPa vs. 175.2 ± 12.3 GPa for elastic modulus). Our nanotribological results show that the friction increased and wear resistance decreased on the surface of the annealed sample compared to the as-deposited Ta film. This discrepancy may be caused by the oxidation of Ta on the film surface, which induces residual compressive stresses in the film and degrades its wear resistance. Our results highlight the influence of thermal annealing and oxidation on nanotribological behavior and small-scale mechanical properties of Ta thin films. Full article
(This article belongs to the Special Issue Small-Scale Mechanical Behaviors in Advanced Engineering Materials)
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