Thin Solid Films最新文献

In situ TEM crystallization of free-standing amorphous silicon nitride (a-SiNX) 独立非晶氮化硅（a-SiNX）的原位TEM结晶

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-02-01 DOI: 10.1016/j.tsf.2026.140865

Elijah M. Davis , Paul Kotula , Calvin Parkin , Carlos Chacon , Edwin Chiu , Aashique Rezwan , Tesia D. Janicki , J. Matthew D. Lane , Hojun Lim , Christopher Bishop , Khalid Hattar

Amorphous silicon nitride (a‑SiN_X) is widely used in microelectronics and MEMS; however, the long‑term structural stability under elevated temperatures and repeated thermal cycling remains an active field of study. This study employs in situ transmission electron microscopy (TEM) to investigate the crystallization mechanisms and kinetics of amorphous silicon nitride thin films. Real-time observation during localized laser-induced heating enables direct visualization of devitrification processes and phase evolution with nanometer-scale resolution. In situ TEM observations show that localized material defects can lower the stability of the amorphous phase and promote crystallization. Notably, the magnitude and distribution of thermal stresses appear to strongly influence crystallization dynamics: intense, localized heating leads to rapid nucleation and near-instantaneous growth, whereas broader, lower-intensity heating induces a slower, two-stage crystallization process. These results are consistent with a strong role of thermal stress in modulating crystallization behavior and offer insights into the thermal reliability of a-SiN_X. Such insights contribute to a deeper understanding of the thermal stability and inform the design of robust thin-film components for high-performance microdevices.

非晶氮化硅（a - SiNX）广泛应用于微电子和MEMS；然而，高温和反复热循环下的长期结构稳定性仍然是一个活跃的研究领域。采用原位透射电镜（TEM）研究了非晶态氮化硅薄膜的结晶机理和动力学。在局部激光诱导加热过程中的实时观察，可以以纳米级分辨率直接可视化脱硝过程和相演化。原位TEM观察表明，材料局部缺陷降低了非晶相的稳定性，促进了非晶相的结晶。值得注意的是，热应力的大小和分布似乎强烈影响结晶动力学：强烈的局部加热导致快速成核和近乎瞬时的生长，而广泛的低强度加热则导致较慢的两阶段结晶过程。这些结果与热应力在调节结晶行为中的重要作用一致，并为a- sinx的热可靠性提供了见解。这些见解有助于更深入地了解热稳定性，并为高性能微器件的坚固薄膜组件的设计提供信息。

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引用次数: 0

The influence of different electron transport layers on the hydrothermal Sb2S3 quasi-epitaxial growth 不同电子输运层对水热Sb2S3准外延生长的影响

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-02-01 DOI: 10.1016/j.tsf.2026.140873

Jun-Cai Zhang , Hu Li , Jie Huang , Jin-Rui Cai , Zhi-Ping Huang , Li-Mei Lin , Chuan-Dong Zuo , Xin Jin , Gui-Lin Chen

Sb₂S₃ has attracted much attention due to its high absorption coefficient, abundant elemental reserves and stable chemical properties. However, key issues such as interface recombination and poor energy level matching have restricted the improvement of device performance. This study investigated the effects of three electron transport layers (ETLs), CdS, TiO₂ and SnO₂, on the hydrothermal quasi-epitaxial growth of Sb₂S₃. CdS could induce the formation of a continuous and dense Sb₂S₃ film through S-Sb chemical bridge bonds, while TiO₂ and SnO₂, due to their surface inertness, led to island-like growth of Sb₂S₃, accompanied by interface holes and defects. Device test results indicated that the device with CdS as the ETL had the best performance: power conversion efficiency (PCE) of 6.11 %, the lowest saturation current density (J₀), and effective suppression of interface recombination. Devices with TiO₂ and SnO₂ as ETLs exhibited lower open-circuit voltage (V_oc) and short-circuit current density (J_sc), and poor device performance (2.82 % and 1.09 %) due to severe interface recombination. SCAPS-1D simulation further confirmed that CdS had significant advantages in energy level matching and interface defect control, making it the most suitable ETL among the three for the quasi-epitaxial growth of Sb₂S₃, providing a key reference for the development of high-efficiency Sb₂S₃ solar cells.

Sb2S3因其高吸收系数、丰富的元素储量和稳定的化学性质而备受关注。然而，接口重组和能级匹配差等关键问题制约了器件性能的提高。本文研究了CdS、TiO2和SnO2三种电子传输层（ETLs）对Sb2S3水热准外延生长的影响。CdS可以通过S-Sb化学桥键诱导形成连续致密的Sb2S3薄膜，而TiO2和SnO2由于其表面惰性导致Sb2S3呈岛状生长，并伴有界面空穴和缺陷。器件测试结果表明，以CdS作为ETL的器件具有最佳性能：功率转换效率（PCE）为6.11%，饱和电流密度（J0）最低，有效抑制了界面复合。以TiO2和SnO2为etl的器件具有较低的开路电压（Voc）和短路电流密度（Jsc），但由于界面重组严重，器件性能较差（分别为2.82%和1.09%）。SCAPS-1D仿真进一步证实了CdS在能级匹配和界面缺陷控制方面具有显著优势，是三种ETL中最适合Sb2S3准外延生长的ETL，为开发高效Sb2S3太阳能电池提供了关键参考。

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引用次数: 0

On the compositional and thermal stability of sputter deposited Inconel based multilayer solar absorber coating 溅射沉积铬镍铁合金基多层太阳能吸收涂层的组成和热稳定性

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-02-01 DOI: 10.1016/j.tsf.2026.140868

S. Vedavarshni , P. Pranav Pradeep , Srinivas G․ , Praveen Kumar , Siju John , Harish C. Barshilia

A multilayer concept has been used to coat Inconel-718 in the presence of Ar+O₂ atmosphere. The coating structure of metal oxide/metal/metal oxide was deposited on stainless steel SS304 substrate with the bottom most oxide layer as non-stoichiometric and the top oxide layer as stoichiometric in nature. This led to the solar absorptance of 0.887 and emissivity of 0.19. The absorption of this multilayer stack was increased by depositing an additional layer of SiO₂ which improves the absorptance in the range of 0.940–0.951 without affecting the emittance (0.17 – 0.19). Field Emission Scanning Electron Microscopy analysis was carried out for studying the morphological properties of the coating. The reflectance properties of the coating were analyzed using UV–Vis-NIR spectroscopy and the X-ray diffraction analysis was used for the structural properties. The findings of these studies highlight Inconel's suitability as a solar selective absorber coating. Contrary to high temperature stability of bulk Inconel, thermal stability investigations of the coating reveal its stability only up to 300 °C in air for long durations. A detailed metallographic analysis conducted on both the bulk and the metal layer, to compare the intermetallic phases present, revealed the absence of the intermetallic phases in the metallic layer. This absence indeed caused the deterioration in thermal stability of the absorber layer. Further, energy dispersive X-ray analysis revealed that, unlike the bulk material, the sputtered Inconel layer exhibited absence of Nb composition. This absence of Nb is significant, as it contributes to the formation of intermetallic phases, thereby, influencing the observed differences in thermal behavior.

在存在Ar+O2气氛的情况下，采用多层概念涂覆Inconel-718。在不锈钢SS304基材上沉积了金属氧化物/金属/金属氧化物的涂层结构，最底部的氧化层为非化学计量性质，顶部的氧化层为化学计量性质。这导致太阳吸收率为0.887，发射率为0.19。在不影响发射度（0.17 ~ 0.19）的情况下，在0.940 ~ 0.951范围内增加了SiO2的吸光度，提高了吸光度。采用场发射扫描电镜对涂层的形貌进行了研究。利用紫外-可见-近红外光谱分析了涂层的反射特性，并用x射线衍射分析了涂层的结构特性。这些研究结果突出了铬镍铁合金作为太阳能选择性吸收涂层的适用性。与大块铬镍铁合金的高温稳定性相反，涂层的热稳定性研究表明其在空气中长时间的稳定性仅为300°C。对大块和金属层进行了详细的金相分析，比较了存在的金属间相，发现金属层中没有金属间相。这种缺失确实导致了吸收层热稳定性的恶化。此外，能量色散x射线分析显示，与块状材料不同，溅射Inconel层表现出Nb成分的缺失。Nb的缺失很重要，因为它有助于形成金属间相，从而影响观察到的热行为差异。

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引用次数: 0

Influence of silver content on the antibacterial properties of TiZrAg thin films 银含量对TiZrAg薄膜抗菌性能的影响

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-02-01 DOI: 10.1016/j.tsf.2026.140872

S.Y. Huang, C.K. Chen, J.C. Huang

This study employs magnetron sputtering to fabricate TiZrAg alloy thin films containing 6 at% and 12 at% silver, with Ti-Zr thin films without silver serving as a control. The aim is to investigate the influence of varying silver content on the antibacterial performance and biocorrosion resistance of the coatings. Experimental results indicate that an increase in silver content correlates with a significant enhancement in the antibacterial efficacy of the Ti-Zr-Ag coatings. The film comprising 6 at% silver demonstrates notable antibacterial effects, while the film with 12 at% silver further augments these properties, confirming the positive impact of higher silver concentrations on antibacterial activity. The improved antimicrobial efficacy is attributed to enhanced Ag⁺ release, reduced film grain size from 114 to 42 nm, decreased surface roughness from 5.7 to 2.8 nm, and increased water contact angle from 69.2 to 87.4°. The coatings also exhibit excellent biocorrosion resistance and long-term stability in chloride-containing saline sterilizing environments. Overall, these Ti-Zr-Ag coatings show strong potential for the surface functionalization of medical devices.

本研究采用磁控溅射法制备了含6 at%和12 at%银的TiZrAg合金薄膜，并以不含银的Ti-Zr薄膜为对照。目的是研究不同银含量对涂层抗菌性能和耐生物腐蚀性能的影响。实验结果表明，银含量的增加与Ti-Zr-Ag涂层的抗菌效果显著增强有关。含有6 at%银的膜显示出显著的抗菌效果，而含有12 at%银的膜进一步增强了这些性能，证实了高银浓度对抗菌活性的积极影响。抗菌效果的提高是由于Ag+释放增强，膜的粒径从114 nm减小到42 nm，表面粗糙度从5.7 nm减小到2.8 nm，水接触角从69.2°增加到87.4°。该涂层还具有优异的耐生物腐蚀性和在含氯盐水灭菌环境中的长期稳定性。总的来说，这些Ti-Zr-Ag涂层在医疗设备的表面功能化方面显示出强大的潜力。

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引用次数: 0

Conductivity mechanisms of the nanocomposite SiOx(Si)&CuyO(Cu) films 纳米复合SiOx(Si)&CuyO（Cu）薄膜的导电机理

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-01-24 DOI: 10.1016/j.tsf.2026.140874

Oleh Bratus , Antonina Kykot , Anton Semeniuk , Slawomir Prucnal , Pavels Onufrijevs , Jevgenijs Kaupuzs , Svitlana Bugaychuk , Tetiana Sydorenko , Volodymyr Ilchenko , Volodymyr Marin , Igor Sokolovskyi , Tomash Sabov , Anatoliy Evtukh

Nanocomposite films were obtained by simultaneous sputtering of the combined Cu/Si target in the O₂/Ar atmosphere by ion-plasma sputtering. As a result of the investigation of the structure of the films by X-ray diffraction, crystalline inclusions of Cu, Cu₂O were detected іn the as-deposited film and Cu, Cu₂O, CuO in the one annealed at temperature T = 400°C. The main mechanisms of electron transport through nanocomposite SiO_x(Si)&Cu_yO(Cu) films containing Cu nanoparticles and amorphous Si inclusions have been established. In the low voltage range, annealing of nanocomposite SiO_x(Si)&Cu_yO(Cu) films leads to a redistribution of the density of electronic states and the concentration of the traps near the Fermi level, which changes the superposition of ohmic conductivity with the Mott, Efros-Shklovskii, Arrhenius mechanisms. In the region of low temperatures and medium voltages the Poole-Frenkel mechanism is realized for both samples. But at the higher measurement temperatures 170 K < T < 350 K the space-charge-limited current mechanism with the exponential distribution of traps in the band gap is revealed for the initial and annealed films. In the range of low temperatures and high voltages trap-assisted tunneling is observed for the initial sample. The dielectric-metal transition was detected in the case of initial films in the high voltage range. The effect of temperature annealing of nanocomposite SiO_x(Si)&Cu_yO(Cu) films on their electrical conductivity is the consequence of their structural transformation, which leads to the change in the concentration and energy position of electron traps in the band gap, which participate in conductivity.

采用离子等离子溅射的方法，在O2/Ar气氛中溅射Cu/Si复合靶，获得了纳米复合膜。通过x射线衍射对膜的结构进行了研究，在沉积膜中发现了Cu， Cu2O的结晶夹杂物，在T = 400℃退火膜中发现了Cu， Cu2O， CuO的结晶夹杂物。建立了含Cu纳米粒子和非晶Si包体的SiOx(Si)& CuyO（Cu）纳米复合薄膜中电子传递的主要机制。在低电压范围内，纳米复合材料SiOx(Si)& CuyO（Cu）薄膜的退火导致了电子态密度和陷阱浓度在费米能级附近的重新分布，从而改变了欧姆电导率与Mott、Efros-Shklovskii、Arrhenius机制的叠加。在低温中压区域，两种样品均实现了普尔-弗伦克尔机制。但在较高的测量温度（170 K < T < 350 K）下，初始膜和退火膜的带隙中陷阱呈指数分布，显示出空间电荷限制电流机制。在低温和高压范围内，观察到初始样品的陷阱辅助隧穿现象。在高电压范围内的初始膜中检测到介电-金属转变。纳米复合材料SiOx(Si)& CuyO（Cu）薄膜的温度退火对其电导率的影响是其结构转变的结果，这导致带隙中参与电导率的电子陷阱的浓度和能量位置发生变化。

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引用次数: 0

Short-range order and optical properties of thin GeOx films obtained by thermal evaporation of GeO and GeO2 GeO和GeO2热蒸发制备的GeOx薄膜的近程阶数和光学性质

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-01-23 DOI: 10.1016/j.tsf.2026.140869

Ghaithaa Hamoud , Alexey Samus , Alexey Matsynin , Sergey Komogortsev , Vyacheslav Zhandun , Igor Prosvirin , Ksenia Astankova , Ivan Azarov , Pavel Geydt , Ilya Milekhin , Vladimir Volodin

A simple method for producing GeO_x thin films by thermal evaporation of GeO₂, GeO and GeO_x targets is proposed. The method does not require high vacuum and electron (or ion) beams or plasma discharge for target evaporation. The atomic structure, optical properties and thicknesses of the obtained GeO_x films grown on silicon and glass substrates were studied using a set of methods: X-ray photoelectron spectroscopy, Raman scattering spectroscopy, infrared spectroscopy, transmission and reflection spectroscopies, and spectral ellipsometry. Optical bandgaps (absorption edges) were determined for films grown from different targets.

提出了一种利用GeO2、GeO和GeOx靶材热蒸发制备GeOx薄膜的简单方法。该方法不需要高真空和电子（或离子）束或等离子体放电来进行目标蒸发。采用x射线光电子能谱、拉曼散射能谱、红外能谱、透射和反射能谱、椭偏光谱等方法研究了在硅和玻璃衬底上生长的GeOx薄膜的原子结构、光学性质和厚度。测定了不同靶材生长薄膜的光带隙（吸收边）。

引用次数: 0

Tailoring multifunctional properties of Co80La20 thin films via annealing and substrate engineering for advanced spintronic and optoelectronic applications 通过退火和衬底工程定制Co80La20薄膜的多功能特性，用于先进的自旋电子和光电子应用

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-01-22 DOI: 10.1016/j.tsf.2026.140866

Shih-Hung Lin , Yung-Huang Chang , Yuan-Tsung Chen , Yu-Chieh Liao , Yun-Sheng Zheng , Huang-Wei Chang

Nanostructured cobalt lanthanum (Co₈₀La₂₀) thin films with thicknesses of 10–50 nm were deposited on glass and silicon (Si)(100) substrates by direct current (DC) magnetron sputtering and subsequently annealed at 100, 200, and 300 °C. Structural analysis via X-ray diffraction (XRD) and atomic force microscopy (AFM) revealed improved crystallinity, grain growth, and increased surface roughness with annealing. Magnetic force microscopy (MFM) demonstrated a transition from fragmented to well-aligned stripe-like magnetic domains, associated with enhanced in-plane magnetic anisotropy. Magnetic characterization confirmed soft magnetic behavior, showing reduced coercivity (Hc) and increased remanence magnetization (Mr) after annealing. Mechanical measurements indicated significant increases in hardness and Young’s modulus, attributed to grain boundary strengthening and defect reduction. Optical transmittance decreased with increasing film thickness (t_f) and roughness due to enhanced scattering, while electrical conductivity improved as a result of increased carrier mobility and reduced resistivity, despite a minor decrease in carrier concentration after annealing. This work highlights the synergistic effect of annealing temperature (T_A) and substrate crystallinity on tuning the structural, magnetic, mechanical, optical, and electrical properties of Co₈₀La₂₀ thin films. The findings demonstrate their promising potential for multifunctional applications including flexible spintronic devices, magnetic sensors, and transparent conductive films.

采用直流（DC）磁控溅射技术在玻璃和硅（Si）（100）衬底上沉积了厚度为10-50 nm的纳米结构钴镧（Co80La20）薄膜，并在100、200和300°C下退火。通过x射线衍射（XRD）和原子力显微镜（AFM）进行的结构分析表明，退火改善了材料的结晶度、晶粒生长和表面粗糙度。磁力显微镜（MFM）显示了从碎片到整齐排列的条纹状磁畴的转变，与增强的面内磁各向异性有关。磁性表征证实了软磁行为，表明退火后矫顽力（Hc）降低，剩磁强度（Mr）增加。力学测量表明，由于晶界强化和缺陷减少，硬度和杨氏模量显著增加。光学透射率随着薄膜厚度（tf）和粗糙度的增加而下降，这是由于散射增强，而导电性则由于载流子迁移率的增加和电阻率的降低而提高，尽管退火后载流子浓度略有下降。这项工作强调了退火温度（TA）和衬底结晶度对调整Co80La20薄膜的结构、磁性、机械、光学和电学性能的协同效应。这一发现显示了它们在多功能应用方面的巨大潜力，包括柔性自旋电子器件、磁传感器和透明导电薄膜。

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引用次数: 0

Spray-coated films of water-dispersible polyaniline complexes as hole-injection layers of organic light-emitting diodes: film morphology aspects 水分散聚苯胺配合物作为有机发光二极管空穴注入层的喷涂膜：膜形态方面

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-01-21 DOI: 10.1016/j.tsf.2026.140870

Sergey I. Pozin, Oxana L. Gribkova, Ekaterina I. Rodina, Dmitriy A. Lypenko, Artem V. Dmitriev, Alexander A. Nekrasov

The paper describes results of comparative testing spray-coated layers of water-dispersible polyaniline (PANI) complexes with polyacids of different chemical structure as hole-injection layers (HILs) in an organic light-emitting diode (OLED) based on a poly(1,4-phenylenevinylene) copolymer (Super Yellow) as an emissive layer. OLEDs using HILs made of poly(3,4-ethylenedioxythiophene) complex with polystyrene sulfonate prepared by spin and spray coating were used as references. OLEDs using HILs based on PANI complexes with poly(4,4′-(2,2′-disulfonic acid)-diphenylene-tere-phthalamide) (t-PASA) and poly(2-acrylamido-2-methyl-1-propanesulfonic acid) (PAMPSA) demonstrated the highest current efficiencies of 6–7 cd/A, that is about 20% higher than this value in the best reference sample. The results were discussed in terms of crucial influence of the HIL morphology (analyzed in two scales) on the OLEDs' efficiency. Morphology of the HILs made of PANI:t-PASA and PANI:PAMPSA complexes were found to be most favorable in the following scales: few microns scale – moderately rough (but not completely smooth) intrinsic film texture derived from intermolecular packing; tens of microns scale – weak manifestation of irregularities induced by the spray coating method.

本文介绍了不同化学结构聚酸的水分散聚苯胺（PANI）配合物在聚1,4-苯乙烯共聚物（超黄）为发光层的有机发光二极管（OLED）中作为空穴注入层（HILs）的喷涂层的对比测试结果。以自旋和喷涂法制备的聚（3,4-乙烯二氧噻吩）与聚苯乙烯磺酸盐配合物制备的发光二极管为对照。基于聚(4,4 ' -（2,2 ' -二磺酸）-二苯二苯酰胺（t-PASA）和聚（2-丙烯酰胺-2-甲基-1-丙磺酸）（PAMPSA）的聚苯胺配合物的HILs的oled显示出最高的电流效率为6-7 cd/A，比最佳参考样品高出约20%。结果讨论了HIL形态（在两个尺度上分析）对oled效率的关键影响。由PANI:t-PASA和PANI:PAMPSA配合物制成的HILs的形貌在以下尺度上是最有利的：几微米尺度-由分子间堆积形成的中等粗糙（但不完全光滑）的固有膜结构；几十微米尺度-弱表现的不规则引起的喷涂方法。

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引用次数: 0

Trisylilamine derivative for plasma-assisted fabrication of SiCN:H copper diffusion barrier with reduced value of permittivity 等离子体辅助制备具有降低介电常数的SiCN:H铜扩散势垒的三苯胺衍生物

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-01-21 DOI: 10.1016/j.tsf.2026.140871

Evgeniya Ermakova , Vladimir Shayapov , Andrey Saraev , Eugene Maximovsky , Viktor Kirienko , Veronica Sulyaeva , Evgeny Gerasimov , Marina Kosinova

Tris(trimethylsilyl)amine was employed as a single-source precursor for plasma-enhanced chemical vapor deposition of dielectric silicon carbonitride films, which act as copper diffusion barriers, at low-to-moderate temperatures. The influence of key process parameters—including precursor partial pressure, plasma power, and deposition temperature—on the deposition rate, chemical bonding structure, composition, and film properties was investigated using Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, and spectroscopic ellipsometry. Plasma chemistry was studied by in-situ optical emission spectroscopy. The refractive index of the films ranged from 1.53 to 1.76, while their permittivity (k-value) varied from 2.7 to 4.5. Post-deposition thermal annealing reduced the permittivity to a value as low as 2.5. The Cu diffusion barrier properties were characterized by analyzing the interfaces of a Si/SiOC:H/SiCN:H/Cu stack annealed at 400 °C using transmission electron microscopy.

采用三甲基硅基胺作为单源前驱体，在中低温度下等离子体增强化学气相沉积介质碳氮化硅薄膜，作为铜扩散屏障。利用傅里叶变换红外光谱、x射线光电子能谱、能量色散x射线分析和光谱椭偏仪研究了前驱体分压、等离子体功率和沉积温度等关键工艺参数对沉积速率、化学键结构、成分和薄膜性能的影响。用原位发射光谱法研究了等离子体化学。薄膜的折射率在1.53 ~ 1.76之间，介电常数k值在2.7 ~ 4.5之间。沉积后的热退火将介电常数降低到低至2.5。利用透射电镜分析了400℃退火后Si/SiOC:H/SiCN:H/Cu复合材料的界面，表征了Cu的扩散势垒性能。

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引用次数: 0

Crystallization kinetics of TiO2 thin films: A comparative study of film deposition conditions TiO2薄膜的结晶动力学：薄膜沉积条件的比较研究

IF 2 4区材料科学 Q3 MATERIALS SCIENCE, COATINGS & FILMS

Thin Solid Films

Pub Date : 2026-01-17 DOI: 10.1016/j.tsf.2026.140867

Daniel F. Fernandes , Jaime J. Hernández , Seohan Kim , Alberto Martín–Asensio , Patricia Pedraz , Jang–Hee Yoon , Isabel Rodríguez , Lars Österlund , Tomas Kubart

This study investigates the crystallization kinetics of TiO₂ thin films deposited by reactive magnetron sputtering, with the aim of identifying optimal process conditions for initially X-ray amorphous films subjected to post-deposition annealing. Thin films were grown using both high-power impulse magnetron sputtering (HiPIMS) and pulsed direct current magnetron sputtering (pDCMS). Particular attention was given to the different reactive modes of operation and the ionization of the deposition flux. As-deposited films contained traces of anatase, brookite, and rutile phases, revealed by TEM and Raman spectroscopy analysis. The crystallization process during post-deposition annealing was monitored in situ using Grazing Incidence Wide-Angle X-ray Scattering (GIWAXS). All films crystallized into the anatase phase; however, the crystallization kinetics were strongly dependent on the growth conditions. Films deposited by HiPIMS exhibited faster crystallization compared to pDCMS, especially in the absence of substrate heating. Notably, films deposited in the so-called metal mode – characterized by high deposition rates and low oxygen partial pressures – crystallized more rapidly, an effect attributed to the higher internal energy of the as-deposited material. Furthermore, a combination of moderate substrate temperature (100 °C), high oxygen partial pressure and low flux energy input during deposition promoted the formation of a (001)-oriented anatase texture after annealing.

本研究研究了反应磁控溅射沉积的tio2薄膜的结晶动力学，旨在确定沉积后退火的初始x射线非晶薄膜的最佳工艺条件。采用高功率脉冲磁控溅射（HiPIMS）和脉冲直流磁控溅射（pDCMS）制备薄膜。特别注意了不同的反应操作模式和沉积通量的电离。通过透射电镜和拉曼光谱分析发现，as沉积膜中含有锐钛矿、brookite和金红石相。利用掠入射广角x射线散射（GIWAXS）原位监测沉积后退火的结晶过程。所有薄膜结晶成锐钛矿相；然而，结晶动力学强烈依赖于生长条件。与pDCMS相比，HiPIMS沉积的薄膜表现出更快的结晶速度，特别是在没有衬底加热的情况下。值得注意的是，以所谓的金属模式沉积的薄膜——以高沉积速率和低氧分压为特征——结晶得更快，这是由于沉积材料的内能更高。此外，沉积过程中适中的衬底温度（100°C）、高氧分压和低通量能量输入的组合促进了退火后（001）取向锐钛矿织构的形成。

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