Research of microstructural characteristics on nanocrystalline diamond by microwave plasma CVD

In this study, the nanocrystalline diamond (NCD) films were carried out by microwave plasma chemical vapor deposition (CVD) with CH₄/Ar/H₂ gas concoction on Si substrate at moderate temperatures. The characteristics of NCD films were evaluated using scanning electron microscopy, Raman spectroscopy, transmission electron microscopy, optical emission spectroscopy and optical contact angle meter. The analytical results revealed that C₂ radial was the dominant species in the deposited process. From TEM observation, the NCD films were formed via the etching of hydrocarbons and a small amount of H₂ content additive into gas mixture has improved the aggregation of the nucleation film to form the NCD films. The more hydrophobic surfaces imply that NCD films are the potential biomaterial in the application of article heart valve or stent.     

CEMS study of stainless steel films deposited by pulsed laser ablation of AISI316

Thin stainless steel films deposited on SiO₂/Si wafer were prepared by a pulsed laser ablation of austenite stainless steel (AISI316), and characterized by conversion electron Mössbauer spectrometry (CEMS) using a He gas proportional counter. As-deposited films were composed of a magnetic phase. When deposited films were heated in air at various temperatures, the hyperfine field of the magnetic phase increased. Hematite was produced on the surface, and the magnetic orientation changed from parallel to in-plane at random with the increase of heating temperatures. The metallic iron and magnetite were produced at 400°C in dry Ar + 5%H₂ atmosphere. When the film was heated in wet Ar + 5%H₂ atmosphere at 600°C, maghemite was produced on the surface, and austenite phase was produced in the inner film.     

微波ECR磁控溅射制备SiNx薄膜的XPS结构研究

利用微波电子回旋共振等离子体增强非平衡磁控溅射法在不同N₂流量下制备无氢SiN_x薄膜.通过X光电子能谱、纳米硬度仪等表征技术,研究了不同N₂流量下制备的SiN_x薄膜的化学键结构、化学键含量、元素配比及各元素沿深度分布.研究结果表明,N₂流量是影响SiN_x薄膜化学键结构、元素配比、元素延深度分布等性质的主要因素.在N_{2关键词： x}')" href="#">SiN_x 磁控溅射 XPS 化学键结构     

Effect of complexing agent on the properties of electrochemically deposited Cu2ZnSnS4 (CZTS) thin films

The Cu₂ZnSnS₄ (CZTS) thin films have been electrochemically deposited on Mo-coated glass substrate from weak acidic medium (pH 4.5-5) at room temperature. The effect of complexing agent (tri-sodium citrate) on the structural, morphological and compositional properties of CZTS thin films has been investigated. The as-deposited and annealed thin films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM),EDAX and X-ray photoelectron spectroscopy (XPS) techniques for their structural, morphological, compositional and chemical properties, respectively. XRD studies reveal that the amorphous nature of as-deposited thin film changes into polycrystalline with kesterite crystal structure after annealing in Ar atmosphere. The film prepared without complexing agent showed well-covered surface morphology on the substrate with some cracks on the surface of the film whereas those prepared using complexing agent, exhibited uneven and slightly porous and some overgrown particles on the surface of the films. After annealing, morphology changes into the flat grains, uniformly distributed over the entire surface of the substrate. The EDAX and XPS study reveals that the films deposited using 0.2 M tri-sodium citrate are nearly stoichiometric.     

Synthesis and characterization of tantalum nitride films prepared by cathodic vacuum arc technique

Tantalum nitride films were deposited on silicon wafer and steel substrates by cathodic vacuum arc in N₂/Ar gas mixtures. The chemical composition, crystalline microstructure and morphology of the films were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM), respectively. According to the results, film composition and microstructure depends strongly on the N₂ partial pressure and the applied negative bias (V_s).     

Effect of oxygen content and deposition temperature on the characteristics of thin silver films deposited by magnetron sputtering

Thin silver films were prepared by direct current magnetron sputtering in a single-ended in-line sputter system at various substrate temperatures and in O₂ contents in sputter gas, and their electrical, optical, structural and morphological properties together with the compositional properties were investigated. When deposited at room temperature, the electrical and optical properties of Ag films deteriorated with addition of O₂ to sputter gas. Deposition of Ag films in O₂ added sputter gas promoted the formation of Ag crystallites with (2 0 0) plane parallel to the substrate surface. The electrical resistivity and optical reflection of Ag films deposited above 100 °C were not affected by the sputtering plasma containing oxygen. X-ray photoelectron spectroscopic analysis showed that Ag films deposited above 100 °C in O₂ added sputter gas did not possess surplus oxygen in the film, and that the oxidation states of these films were almost identical to that of Ag films deposited in pure Ar gas.     

微波等离子体化学汽相沉积法沉积CNx膜的研究

对用微波等离子体化学汽相沉积法沉积在Si基片上的CN_x膜分别进行Raman散射、X射线光电子能谱、X射线衍射和扫描电子显微镜等技术的分析与测试. Raman散射的研究结果表明在CH₄与N₂的流量比低于1∶8时，CN_x膜的散射谱中以非晶石墨峰的形式出现.当流量比为1∶8时，则表现为较尖锐的C≡N键(2190cm^-1)的特征峰；从X射线光电子能谱的分析结果可以看出C，N成键的方式主要是C≡N键和C—N 关键词：     

Superhard Nb-Si-N composite films synthesized by reactive magnetron sputtering

By means of the reactive magnetron sputtering method, a series of Nb-Si-N composite films with different Si contents were deposited in an Ar, N₂ and SiH₄ mixture atmosphere. These films’ chemical composition, phase formation, microstructure and mechanical properties were characterized by the energy dispersive spectroscopy, X-ray diffraction, transmission electron microcopy, atomic force microscopy and nanoindentation. The experimental results showed that the silicon content in the Nb-Si-N composite films can be conveniently controlled by adjusting the SiH₄ partial pressure in mixed gas. The hardness and elastic modulus of the Nb-Si-N films were remarkably increased with a small amount of silicon addition and reached their maximum values of 53 and 521 GPa, respectively, at 3.4 at.% Si. Such an obvious enhancement of mechanical properties is related to the increment of crystal defects in the Nb-Si-N films. With silicon content increasing in the films further, the mechanical properties decreased gradually to somewhat a bit lower than those of the NbN film.     

H2对Ar稀释SiH4等离子体CVD制备多晶硅薄膜的影响

以SiH₄，Ar和H₂为反应气体，采用射频等离子体化学气相沉积方法在300℃下制备了低温多晶Si薄膜.实验发现，反应气体中H₂的比例是影响薄膜结晶质量的重要因素，在适量的H₂比例下制备的多晶Si薄膜具有结晶相体积分数高，氢含量低，生长速率快、抗杂质污染等特性. 关键词： 低温多晶Si薄膜 等离子体CVD 4')" href="#">Ar稀释SiH₄ 2比例')" href="#">H₂比例     

Synthesis of molybdenum silicide by both ion implantation and ion beam assisted deposition

Two groups of Mo/Si films were deposited on surface of Si(1 0 0) crystal. The first group of the samples was prepared by both ion beam assisted deposition (IBAD) and metal vapor vacuum arc (MEVVA) ion implantation technologies under temperatures from 200 to 400 °C. The deposited species of IBAD were Mo and Si, and different sputtering Ar ion densities were selected. The mixed Mo/Si films were implanted by Mo ion with energy of 94 keV, and fluence of Mo ion was 5 × 10¹⁶ ions/cm². The second group of the samples was prepared only by IBAD under the same test temperature range. The Mo/Si samples were analyzed by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), sheet resistance, nanohardness, and modulus of the Mo/Si films were also measured. For the Mo/Si films implanted with Mo ion, XRD results indicate that phase of the Mo/Si films prepared at 400 and 300 °C was pure MoSi₂. Sheet resistance of the Mo/Si films implanted with Mo ion was less than that of the Mo/Si films prepared without ion implantation. Nanohardness and modulus of the Mo/Si films were obviously affected by test parameters.     

Characterization of ZnO thin films grown on various substrates by RF magnetron sputtering

In this study we investigated properties of ZnO thin films deposited on both oxygen-containing substrates and a substrate without oxygen content at various O₂/Ar reactant gas ratios. Deposition of ZnO on indium-tin oxide (ITO) resulted in the best crystallinity, whereas the least degree of crystallization was observed from ZnO deposited on glass. All the films were found to have compressive stress, which was relieved by annealing in O₂ environment. ZnO films deposited on glass revealed p-type conductivity when prepared at O₂/Ar ratio of 0.25 whereas those on SiN_x yielded p-type conductivity when prepared at O₂/Ar ratio of 4. In addition, shallower oxygen interstitial seemed to be found from films with better crystallinity. The largest shift in binding energy of Zn_2p3/2 was observed from ZnO prepared on glass at O₂/Ar ratio of 0.25, whereas that of O_1s was obtained from ZnO deposited on SiN_x at O₂/Ar ratio of 4. A model was proposed in terms of O₂ diffusion and hydrogen desorption in order to account for the observed property variations depending on substrates and O₂/Ar ratios.     

Spectroscopic investigation of the physicochemical origin of the spontaneous delamination of the sputtered amorphous carbon nitride films

We present in this study a spectroscopic investigation of the delamination of the amorphous carbon nitride (a-CN_x) films deposited by RF magnetron sputtering of a graphite target in Ar/N₂ gas mixture. The microstructure of the studied films have been analysed prior and after their delamination. The origin of the observed spontaneous delamination have been elucidated in terms of chemical reactions between water and CN bonds at the a-CN_x/Si interface, which support delamination crack advance.     

Structure and elastic recovery of Cr-C:H films deposited by a reactive magnetron sputtering technique

Cr-containing hydrogenated amorphous carbon (Cr-C:H) films were deposited on silicon substrates using a DC reactive magnetron sputtering with Cr target in an Ar and C₂H₂ gas mixture. The composition, bond structure, mechanical hardness and elastic recovery of the films were characterized using energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, Raman spectroscopy and nano-indentation. The film tribological behavior was also studied by a ball-on-disc tribo-tester. The results showed that the films deposited at low C₂H₂ flow rate (<10 sccm) presented a feature of composite Cr-C:H structure, which consisted of hard brittle chromium carbide phases and amorphous hydrocarbon phase, and thus led to the observed low elastic recovery and poor wear resistance of the films. However, the film deposited at high C₂H₂ flow rate (40 sccm) was found to present a typical feature of polymer-like a-C:H structure containing a large amount of sp³ C-H bonds. As a result, the film revealed a high elastic recovery, and thus exhibited an excellent wear resistance.     

Thermal stability of ZnO thin film prepared by RF-magnetron sputtering evaluated by thermal desorption spectroscopy

Thermal stability of sputter deposited ZnO thin films was evaluated by thermal desorption spectroscopy (TDS). Desorption of Zn was mainly observed from the films deposited at low O₂/Ar gas ratio and low RF power. In contrast, O₂ desorption was mainly observed from the films deposited at high O₂/Ar gas ratio and high RF power. The amount of desorbed O₂ from the film increased with increasing the O₂/Ar gas flow ratio and the RF power. Furthermore, the desorption temperature of O₂ increased with increasing the RF power during the deposition. Thermal stability of the ZnO films was controlled not only by the O₂/Ar gas flow ratio, but also applied RF power to the target.     

The effect of different ambient gases, pressures, and substrate temperatures on TiO2 thin films grown on Si(100) by laser ablation technique

Pure titanium dioxide (TiO₂) thin films were deposited on single-crystal Si(100) substrates by laser ablation. We investigated the effects of ambient gas (O₂ or Ar), pressures, and substrate temperatures on film quality. From the annealing experiment of the deposited TiO₂ thin film under Ar or O₂ ambient gas, we see the chemical effect of ambient gas on film quality. The crystallinity of the deposited TiO₂ thin film is best at 700 °C in the substrate temperature range attempted, 400-700 °C, and at pressures of 0.1 Torr and below. The rutile phase is dominant under most experimental conditions. Only under very extreme conditions did we obtain a thin film of the anatase phase.     

Effects of O2/Ar ratio and annealing temperature on electrical properties of Ta2O5 film prepared by magnetron sputtering

The effects of the oxygen-argon ratio on electric properties of Ta2O5 film prepared by radio-frequency magnetron sputtering were investigated.The Ta2O5 partially transforms from the amorphous phase into the crystal phase when annealing temperatures are 800℃ or higher.The lattice constant of Ta2O5 decreases with the increase of the O2/Ar ratio,which indicates that oxygen gas in the working gas mixture contributes to reducing the density of oxygen vacancies during the deposition process.For the films deposited in working gas mixtures with different O2/Ar ratios and subsequently annealed at 700℃,the effective dielectric constant is increased from 14.7 to 18.4 with the increase of the O2/Ar ratio from 0 to 1.Considering the presence of an SiO2 layer between the film and the silicon substrate,the optimal dielectric constant of Ta2O5 film was estimated to be 31.Oxygen gas in the working gas mixture contributes to reducing the density of oxygen vacancies,and the oxygen vacancy density and leakage current of Ta2O5 film both decrease with the increase of the O2/Ar ratio.The leakage current decreases after annealing treatment and it is minimized at 700℃.However,when the annealing temperature is 800℃ or higher,it increases slightly,which results from the partially crystallized Ta2O5 layer containing defects such as grain boundaries and vacancies.     

Structure and mechanical properties of reactive sputtering CrSiN films

CrSiN films with various Si contents were deposited by reactive magnetron sputtering using the co-deposition of Cr and Si targets in the presence of the reactive gas mixture. Comparative studies on microstructure and mechanical properties between CrN and CrSiN films with various Si contents were carried out. The structure of the CrSiN films was found to change from crystalline to amorphous structure as the Si contents increase. Amorphous phase of Si₃N₄ compound was suggested to exist in the CrSiN film. The growth of films has been observed from continuous columnar structure, granular structure to glassy-like appearance morphology with the increase of silicon content. The film fracture changed from continuous columnar structure, granular structure to glassy-like appearance morphology with the increase of silicon content. Two hardness peaks of the films as function of Si contents have been discussed.     

Synthesis and characterization of superhard Ti-Si-N films obtained in an inductively coupled plasma enhanced chemical vapor deposition (ICP-CVD) with magnetic confinement

Using a novel inductively coupled plasma enhanced chemical vapor deposition (ICP-CVD) with magnetic confinement system, Ti-Si-N films were prepared on single-crystal silicon wafer substrates by sputtering Ti and Si (5 at.%:1 at.%) alloyed target in argon/nitrogen plasma. High-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), X-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), atomic force microscopy (AFM) and Nano Indenter XP tester were employed to characterize nanostructure and performances of the films. These films were essentially composed of TiN nanocrystallites embedded in an amorphous Si₃N₄ matrix with maximum hardness value of 44 GPa. Experimental results showed that the film hardness was mainly dependent on the TiN crystallite size and preferred orientation, which could be tailored by the adjustment of the N₂/Ar ratio. When the N₂/Ar ratio was 3, the film possessed the minimum TiN size of 10.5 nm and the maximum hardness of 44 GPa.     

Amorphous carbon nitride film preparation by plasma-assisted pulsed laser deposition method

Amorphous carbon nitride (aCN_x) films were prepared by pulsed laser ablation of graphite in N₂ RF plasma. The film property was compared with that prepared in N₂ gas. The N₂ plasma was generated by a mesh electrode, which was inserted between a graphite target and a Si substrate. The gas pressure p_N2 was varied from 10 to 100 mTorr. The film deposition rate exponentially decreased with p_N2 for both the plasma and gas environment. X-ray photoelectron spectroscopy analysis showed that the ratio of nitrogen content to the carbon one ([N]/[C]) of the aCN_x film surface deposited in the N₂ plasma was 2 times higher than that obtained in the N₂ gas. The film structure was shown by Raman spectroscopy analysis that sp² clustering was enhanced with increasing the [N]/[C]. The effect of plasma on aCN_x film deposition was discussed. PACS 81.15.Fg; 79.60.-i; 81.05.Uw     

离子束反应溅射沉积SiO2薄膜的光学特性

 主要研究采用离子束反应溅射（RIBS）制备SiO2薄膜的折射率、消光系数、化学计量比与氧气在氩氧混合工作气体中含量及其沉积速率的关系。研究结果表明：RIBS制备的SiO2薄膜在0.63 μm处折射率n= 1.48,消光系数小于10-5;随着沉积速率的增加,薄膜的折射率和消光系数随之变大,当沉积速率超过0.3 nm/s,即使是在纯氧环境溅射,折射率值也不低于1.5;通过对红外透射光谱的主吸收峰位置研究得到沉积的SiO2薄膜为缺氧型,化学计量比不超过1.8,且红外吸收峰位置和SiO2折射率存在对应关系,因此在不加热衬底情况下使用RIBS制备SiO2薄膜时,会限制沉积速率的提高。