Microcrystalline silicon films fabricated by bias-assisted hot-wire chemical vapor deposition

Microcrystalline silicon films (μc-Si:H) were deposited on stainless steel substrates by bias-assisted hot-wire chemical vapor deposition. The effect of substrate bias and substrate temperature on the crystallinity of μc-Si:H films was studied by Raman spectroscopy, X-ray diffraction and scanning electron microscopy. The results show that both the Raman peak position and the crystalline fraction of the μc-Si:H films deposited at 200 °C were obviously improved by introducing ?800 V substrate bias. The films deposited at 200 °C with ?800 V substrate bias show strongly sharpened Si (111) peak together with Si (220) and Si (311) peaks, which was different from a weak Si (111) peak for those deposited without substrate bias. By increasing the substrate temperature from 200 to 300 °C, while keeping the substrate bias at ?800 V, the crystallinity of the silicon films was further improved, and μc-Si:H films with crystalline fraction of 74 % was obtained.     

Orientation dependence of fracture toughness measured by indentation methods and its relation to surface energy in single crystal silicon

Fracture toughness of silicon crystals has been investigated using indentation methods, and their surface energies have been calculated by molecular dynamics (MD). In order to determine the most preferential fracture plane at room temperature among the crystallographic planes containing the 〈001〉, 〈110〉 and 〈111〉 directions, a conical indenter was forced into (001), (110) and (111) silicon wafers at room temperature. Dominant {110}, {111} and {110} cracks were introduced from the indents on (001), (011) and (111) wafers, respectively. Fracture occurs most easily along {110}, {111} and {110} planes among the crystallographic planes containing the 〈001〉, 〈011〉 and 〈111〉 directions, respectively. A series of surface energies of those planes were calculated by MD to confirm the orientation dependence of fracture toughness. The surface energy of the {110} plane is the minimum of 1.50 Jm⁻² among planes containing the 〈001〉 and 〈111〉 directions, respectively, and that of the {111} plane is the minimum of 1.19 Jm⁻² among the planes containing the 〈011〉 direction. Fracture toughness of those planes was also derived from the calculated surface energies. It was shown that the K _IC value of the {110} crack plane was the minimum among those for the planes containing the 〈001〉 and 〈111〉 directions, respectively, and that K _IC value of the {111} crack plane was the minimum among those for the planes containing the 〈011〉 direction. These results are in good agreement with that obtained conical indentation.     

Nanocrystalline silicon carbon doped films prepared by hot wire technique

In this work we present data concerning the structure, composition and electro-optical performances of nanocrystalline silicon carbide doped films produced at the different filament temperatures and hydrogen dilution ratios. The XRD spectra reveal the presence of the typical Si peaks ascribed to (111) (220) and (311) diffraction planes, where no traces of the carbon peaks were found. The average grain sizes ranges from 10 nm to 30 nm, depending on the temperature of filament and hydrogen dilution used. We observed an enhaneement of the peak ascribed to the (220) plane when high H dilution rates are used, meaning that the film starts being textured. The infrared data reveal the typical silicon carbide modes and a hydrogen content that varies from 3% to 1%, with the increase of the filament temperature. Besides that, the IR spectra show the typical SiO₂ and SiO modes, associated to the oxide species that are mainly incorporated in the surface of the films and can be removed by proper wet etching. The planar conductivity is enhanced as the temperature of the filament is increased, being the highest conductivity achieved in the range of 0.2 (Ωcm)⁻¹ and almost non activated.     

磁控溅射制备Cu2O和Cu2O/TiO2复合膜及其光催化活性

采用直流反应磁控溅射的方法在普通玻璃上沉积得到Cu2O、TiO2和Cu2O/TiO2复合薄膜.用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和X射线能谱仪(EDS)对薄膜的晶体结构、表面形态和薄膜元素组成进行了分析.XRD结果表明,当反应溅射时间为5 min时,Cu2O薄膜由单一的(111)晶面组成;反应时间的延长促进了Cu2O(110)和(220)晶面的生长.通过计算得出Cu2O(111)更有利于对O2的吸附.进一步使用氙灯作为光源,用薄膜对亚甲基蓝(MB)的降解率来表征光催化活性.结果表明,Cu2O/TiO2复合薄膜的光催化效果随着Cu2O含量的增加升高而后降低,当Cu2O含量为2.6mol%时,光催化活性最高.光催化效率的提高主要归因于Cu2O的加入引起光生电子-空穴的分离,而过量的Cu2O会延长光生电子迁移到Cu2O/TiO2界面和空穴迁移至表面所需要的时间,使电子和空穴复合的几率增大,从而降低了量子效率.     

铜铟硒薄膜的外延生长和表面重构及其电池性能研究

在GaAs的(110)、(001)和(111)A、(111)B等极性晶面上, 通过铜铟共溅-硒蒸镀的方法, 分布外延生长出(220/204)、(001)和(112)结晶取向的单晶CIS薄膜. 系统考察了CIS薄膜外延生长的结晶取向和表面微结构, 发现了这些CIS外延薄膜均需表面重构化而形成比表面能低的CIS(112)晶面, 结合晶体结构研究了各种晶面和比表面能的相关性. 通过各种衬底下不同结晶取向的CIS薄膜的太阳能电池组装, 发现当CIS薄膜生长具有(220/204)结晶取向时电池器件性能最好、效率最高, 说明可通过控制CIS薄膜的沉积条件和选用合适取向的衬底, 增加吸收层(220/204)的结晶取向, 从而显著提高CIS薄膜太阳电池的光电性能.     

Investigation of titanium nitride films deposited at room temperature by energetic cluster impact

Energetic cluster impact (ECI) deposition was applied to grow titanium nitride films on silicon (100) substrate at room temperature. Proton elastic scattering (PES), X-ray diffraction (XRD) and atomic force microscopy (AFM) were employed to characterize the composition, structure and morphology of TiN_x films, respectively. The PES results reveal that the films are N-deficient and there exists a certain amount of oxygen impurity in the films. It is found from the XRD results that the structure of TiN_x films is sensitive to experimental conditions such as nitrogen gas partial pressure, sputtering current and substrate bias voltage and that TiN_x films are (220) preferred orientation within some range of experimental conditions. The AFM observation indicates that the films become more uniform and compact with increasing substrate bias voltage. The root mean square roughness also decreases with increasing bias voltage. Some interpretation for the above results are also given in this paper.     

Epitaxial growth of platinum-rhodium and gold-palladium alloys on rock salt

Single-crystal Pt-40 wt.% Rh and Au-50 wt.% Pd alloy films have been grown epitaxially by vacuum evaporation on (100), (110) and (111) planes of heated rock salt by the simultaneous evaporation of their components from separate sources. The structure of the films was investigated by transmission electron microscopy as a function of substrate temperature and thickness. Annealing experiments were done on the films inside the electron microscope.     

Texture of CoSi2 films on Si(111), (110) and (001) substrates

Synchrotron radiation was used to study the texture of polycrystalline CoSi₂ films that were formed by a solid-state reaction between a 30 nm Co film and Si(111), (110) and (001) substrates. All films were strongly textured, and several texture components were identified. We discuss the simultaneous occurrence of axiotaxy (i.e. alignment of lattice planes across the interface) and several different types of epitaxy in each of the films. Comparison of the different texture components observed on the three substrate orientations suggests a strong preference for the alignment of CoSi₂{110} planes in the film with Si{110} planes in the substrate, and twinning around Si[111] directions.     

Structural investigation of silicon films chemically vapour deposited onto amorphous SiO2 substrates

The influence of substrate temperature and the silane-to-nitrogen ratio on the structure of silicon films 0.5–0.6 μm thick deposited onto amorphous SiO₂ substrates was investigated by X-ray diffraction. The investigations were carried out for silicon films deposited at various temperatures in the range 500–750 °C and with various silane-to-nitrogen ratios in the range 3.04 × 10^-4-2.84 × 10^-3 by volume. The silicon films deposited at 500 °C were amorphous while the films deposited at 550 °C were randomly oriented polycrystalline. The films deposited in the temperature range 600–700 °C were polycrystalline with a preferred orientation that changed from 〈110〉 through 〈100〉 to 〈111〉. The structure of the films deposited at 750 °C was randomly oriented polycrystalline. Investigations of the influence of the silane-to-nitrogen ratio on the silicon film structure revealed that the structure of films deposited at a substrate temperature of 500 °C was independent of the silane-to-nitrogen ratio. The structure of the films deposited at 600 °C depended on the silane-to-nitrogen ratio and changed from polycrystalline with a 〈110〉 preferred orientation to randomly oriented polycrystalline when the ratio was increased. The structure of films deposited at 700 °C also depended on the silane-to-nitrogen ratio and changed from randomly oriented polycrystalline to polycrystalline with double preferred orientation (〈100〉 and 〈111〉) when the ratio was increased.     

Effect of nitrogen flow ratio on structure and properties of zirconium nitride films on Si(100) prepared by ion beam sputtering

In this study, zirconium nitride thin films were deposited on Si substrates by ion beam sputtering (IBS). Influence of N₂/(N₂+Ar) on the structural and physical properties of the films has been investigated with respect to the atomic ratio between nitrogen and zirconium. It was found that the thickness of layers decreased by increasing the F(N₂). Moreover, crystalline plane peaks such as (111), (200) and (220) with (111) preferred orientation were observed due to strain energy which associate with (111) orientation in ZrN. Also, the fluctuation in nitrogen flow ratio results in colour and electrical resistivity of films.     

在室温条件下制备高质量纳米结构TiN薄膜研究

在室温条件下,利用磁过滤等离子体在单晶硅和不锈钢表面上制备了性能优异的纳米结构TiN薄膜.运用原子力显微镜和掠角入射X射线衍射仪对其结构与形貌进行了表征,利用纳米压痕仪测量了TiN薄膜的硬度和弹性模量.结果表明:TiN薄膜表面光滑,致密,无柱状晶;TiN晶粒的平均尺寸为50nm,薄膜硬度达50 GPa,是传统CVD和PVD技术沉积氮化钛的两倍多;XRD衍射试验表明,纳米TiN的衍射角都普遍向小角度移动,TiN晶粒沿(111)择优生长.     

Bias effect on microstructure and mechanical properties of magnetron sputtered nanocrystalline titanium carbide thin films

Nanocrystalline titanium carbide (TiC) thin films were prepared by magnetron sputtering deposition at 473 K. The effect of substrate bias on microstructure and mechanical properties was studied in details using X-ray photoelectron spectroscopy, X-ray diffraction, field emission scanning electron microscopy, indentation and scanning microscratch. The TiC films exhibit a (111) preferential orientation. Substrate bias decreases grain size and deposition rate of the TiC films. The TiC films have columnar structure which becomes finer at high substrate bias. Nanoindentation hardness, Young's modulus, and toughness of the films are increased as the substrate bias goes up. However, the adhesion peaks at substrate bias of − 100 V and drops when bias is increased further.     

Mechanical properties of amorphous and microcrystalline silicon films

Hydrogen-free amorphous silicon (a-Si) films with thickness of 4.5-6.5 μm were prepared by magnetron sputtering of pure silicon. Mechanical properties (hardness, intrinsic stress, elastic modulus), and film structure (Raman spectra, electron diffraction) were investigated in dependence on the substrate bias and temperature. The increasing negative substrate bias or Ar pressure results in simultaneous reducing compressive stress, the film hardness and elastic modulus. Vacuum annealing or deposition of a-Si films at temperatures up to 600 °C saving amorphous character of the films, results in reducing compressive stress and increasing the hardness and elastic modulus. The latter value was always lower than that for monocrystalline Si(111). The crystalline structure (c-Si) starts to be formed at deposition temperature of ∼ 700 °C. The hardness and elastic modulus of c-Si films were very close to monocrystalline Si(111). Phase transformations observed in the samples at indentation depend not only on the load and loading rate but also on the initial phase of silicon. However, the film hardness is not too sensitive to the presence of phase transformations.     

Hydrogenated microcrystalline silicon films prepared by VHF-PECVD and single junction solar cell

Intrinsic microcrystalline silicon films have been prepared with very high frequency plasma enhanced chemical vapor deposition (VHF-PECVD) from silane/hydrogen mixture at 180°C. The effect of silane concentration and discharge power on the growth of silicon films was investigated. Samples were investigated by Fourier transform infrared spectroscopy, Raman scattering and X-ray diffraction. The Raman spectrum shows that the morphological transition from microcrystalline to amorphous occurs under conditions of high silane concentration and low discharge power. X-ray diffraction spectra indicate a preferential growth direction of all microcrystalline silicon films in the (111) plane. In addition, a solar cell with an efficiency of 5.1% has been obtained with the intrinsic microcrystalline layer prepared at 10W.     

正偏压对纳米金刚石薄膜结构和电阻率的影响

采用电子辅助热丝化学气相沉积工艺, 在1kPa反应气压和施加不同的偏流条件下, 沉积了纳米金刚石薄膜. 用X射线衍射, 场发射扫描电镜和半导体特性表征系统对该薄膜进行了表征和分析. 结果表明, 施加偏流可以使薄膜晶粒呈现明显的(110)晶面择优取向, 表面形貌发生较大变化. 当偏流为8A时, 薄膜晶粒达到最小值, 约为20nm, 薄膜表面也最光滑. 本文讨论了在低气压和电子轰击条件下(110)晶面择优取向的形成机制及其对薄膜显微形貌和电阻率的影响关系.     

Synthesis and characterization of 10% Sb doped CdTe thin films by stacked elemental layer (SEL) method

Antimony doped CdTe thin films have been prepared by stacked elemental layer (SEL) method. The X-ray diffraction spectra have demonstrated that the structure of the annealed films are polycrystalline in nature and mixed CdTe and Sb₂Te₃ phases have been observed at high annealing temperature (500 °C). The increased texture coefficient has been observed for planes (311) and (220) rather than (111) plane of CdTe in annealed stack (Te/Cd/Sb). Transmission spectra have been recorded and the calculated band gap lies between 1.45 and 1.68 eV. A pronounced PL spectrum has been noticed at 532 nm and depicted the presence of nano size particles in annealed thin films.     

Microstructure and mechanical properties of CrAlN coatings deposited by modified ion beam enhanced magnetron sputtering on AISI H13 steel

CrAlN coatings were deposited on silicon and AISI H13 steel substrates using a modified ion beam enhanced magnetron sputtering system. At the modified ion beam bombardment, the effects of bias voltage and Al/(Cr + Al) ratio on microstructure and mechanical properties of the coatings were studied. The X-ray diffraction data showed that all CrAlN coatings were crystallized in the cubic NaCl B1 structure, showing the (111), (200), and (220) preferential orientation. It is noted that the (111) diffraction peak intensity decreased and the peaks broadened as the bias voltage increased at the same ratio of Al/Cr targets power, which is attributed to the variation in the grain size and microstrain. The microstructure observation of the coatings by field emission scanning electron microscopy cross-section morphology shows that the columnar grain became more compact and dense with increasing substrate bias voltage and Al concentration. At a substrate bias voltage of −120 V and a Al/(Cr + Al) ratio of 40%, the coating had the highest hardness (33.8 GPa) and excellent adhesion to the substrate.     

高能微波辐照条件下SiC晶粒的生长过程分析

利用高能真空微波辐照, 仅以SiO₂和人造石墨粉为原料, 便捷快速地合成得到结晶良好的β-SiC晶粒。在利用各种表征手段综合分析SiC晶粒微观结构的基础上, 确认高能微波辐照条件下, β-SiC晶粒的生长过程符合“光滑界面的二维形核生长”机制。借助于电子背散射衍射技术(EBSD)进行的原位解析发现, 生长最快的{211}面在晶粒长大过程中逐渐被超覆, 通过形成{421}过渡晶面而最终演变为{220}晶面, 并成为晶粒的侧面; 而生长最慢的{111}面则成为最后保留下来的六角形规则晶面。EBSD的解析结果为SiC晶粒生长过程中晶面演变提供了直接的实验证据。     

Morphology and texture evolution of nanostructured CaF2 films on amorphous substrates under oblique incidence flux

The morphology and biaxial texture of vacuum evaporated CaF(2) films on amorphous substrates as a function of vapour incident angle, substrate temperature and film thickness were investigated by scanning electron microscopy, x-ray pole figure and reflection high energy electron diffraction surface pole figure analyses. Results show that an anomalous [220] out-of-plane texture was preferred in CaF(2) films deposited on Si substrates at < 200?°C with normal vapour incidence. With an increase of the vapour incident angle, the out-of-plane orientation changed from [220] to [111] at a substrate temperature of 100?°C. In films deposited with normal vapour incidence, the out-of-plane orientation changed from [220] at 100?°C to [111] at 400?°C. In films deposited with an oblique vapour incidence at 100?°C, the texture changed from random at small thickness (5 nm) to biaxial at larger thickness (20 nm or more). Using first principles density functional theory calculation, it was shown that [220] texture formation is a consequence of energetically favourable adsorption of CaF(2) molecules onto the CaF(2)(110) facet.     

Micropore x-ray optics using anisotropic wet etching of (110) silicon wafers

To develop x-ray mirrors for micropore optics, smooth silicon (111) sidewalls obtained after anisotropic wet etching of a silicon (110) wafer were studied. A sample device with 19 microm wide (111) sidewalls was fabricated using a 220 microm thick silicon (110) wafer and potassium hydroxide solution. For what we believe to be the first time, x-ray reflection on the (111) sidewalls was detected in the angular response measurement. Compared to ray-tracing simulations, the surface roughness of the sidewalls was estimated to be 3-5 nm, which is consistent with the atomic force microscope and the surface profiler measurements.