Characterization of Ti-Zr-N films deposited by cathodic vacuum arc with different substrate bias

Ti-Zr-N (multi-phase) films were prepared by cathodic vacuum arc technique with different substrate bias (0 to −500 V), using Ti and Zr plasma flows in residual N₂ atmosphere. It was found that the microstructure and mechanical properties of the composite films are strongly dependent on the deposition parameters. All the films studied in this paper are composed of ZrN, TiN, and TiZrN ternary phases. The grains change from equiaxial to columnar and exhibit preferred orientation as a function of substrate bias. With the increase of substrate bias the atomic ratio of Ti to Zr elements keeps almost constant, while the N to (Ti + Zr) ratio increases to about 1.1. The composite films present an enhanced nanohardness compared with the binary TiN and ZrN films deposited under the same condition. The film deposited with bias of −300 V possesses the maximum scratch critical load (L_c).     

X-ray photoelectron spectroscopy of nano-multilayered Zr-O/Al-O coatings deposited by cathodic vacuum arc plasma

Nano-multilayered Zr-O/Al-O coatings with alternating Zr-O and Al-O layers having a bi-layer period of 6-7 nm and total coating thickness of 1.0-1.2 μm were deposited using a cathodic vacuum arc plasma process on rotating Si substrates. Plasmas generated from two cathodes, Zr and Al, were deposited simultaneously in a mixture of Ar and O₂ background gases. The Zr-O/Al-O coatings, as well as bulk ZrO₂ and Al₂O₃ reference samples, were studied using X-ray photoelectron spectroscopy (XPS). The XPS spectra were analyzed on the surface and after sputtering with a 4 kV Ar⁺ ion gun. High resolution angle resolved spectra were obtained at three take-off angles: 15°, 45° and 75° relative to the sample surface.It was shown that preferential sputtering of oxygen took place during XPS of bulk reference ZrO₂ samples, producing ZrO and free Zr along with ZrO₂ in the XPS spectra. In contrast, no preferential sputtering was observed with Al₂O₃ reference samples. The Zr-O/Al-O coatings contained a large amount of free metals along with their oxides. Free Zr and Al were observed in the coating spectra both before and after sputtering, and thus cannot be due solely to preferential sputtering.Transmission electron microscopy revealed that the Zr-O/Al-O coatings had a nano-multilayered structure with well distinguished alternating layers. However, both of the alternating layers of the coating contained of a mixture of aluminum and zirconium oxides and free Al and Zr metals. The concentration of Zr and Al changed periodically with distance normal to the coating surface: the Zr maximum coincided with the Al minimum and vice versa. However the concentration of Zr in both alternating layers was significantly larger than that of Al. Despite the large free metal concentration, the Knoop hardness, 21.5 GPa, was relatively high, which might be attributed to super-lattice formation or formation of a metal-oxide nanocomposite within the layers.     

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     

Low-temperature deposited ZnO thin films on the flexible substrate by cathodic vacuum arc technology

In this paper, un-doped zinc oxide (ZnO) films with various thicknesses (150, 250, 350, 450 and 550 nm) were successfully prepared onto PET substrates using cathodic vacuum arc technique at low-temperature (<40 °C). Their microstructure, optical and electrical properties were investigated and discussed. The films showed (0 0 2) peaks, an average transmittance over 80% in the visible region. Calculated values of the band gap are around 3.29-3.33 eV when the film thickness increased, indicating a slight blue shift of optical transmission spectra. The lowest resistivity about 5.26 × 10⁻³ Ω cm could be achieved for the un-doped ZnO film with thickness of 550 nm.     

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 pulsed bias on properties of ZrN/TiZrN films deposited by cathodic vacuum arc

ZrN/TiZrN multilayer are deposited by cathodic vacuum arc method with different substrate bias (from 0 to -800 V), using Ti and Zr plasma flows in residual N₂ atmosphere, combined with ion bombardment of sample surfaces. The effect of pulsed bias on structure and properties of films is investigated. Microstructure of the coating is analyzed by X-ray diffraction (XRD), and scanning electron microscopy (SEM). Meanwhile, the nanohardness, Young's modulus, and scratch tests are performed. The experimental results show that the films exhibit a nanoscale multilayer structure consisting of TiZrN and ZrN phases. Solid solutions are formed for component TiZrN films. The dominant preferred orientation of TiZrN films is (111) and (220). At pulsed bias of -200 V, the nanohardness and the adhesion strength of ZrN/TiZrN multilayer reach a maximum of 38 GPa, and 78 N, respectively. The ZrN/TiZrN multilayer demonstrates an enhanced nanohardness compared with binary TiN and ZrN films deposited under equivalent conditions.     

Effect of pulsed bias on the properties of ZrN/TiZrN films deposited by a cathodic vacuum arc

ZrN/TiZrN multilayers are deposited by using the cathodic vacuum arc method with different substrate bias(from 0 to 800 V),using Ti and Zr plasma flows in residual N 2 atmosphere,combined with ion bombardment of sample surfaces.The effect of pulsed bias on the structure and properties of films is investigated.Microstructure of the coating is analyzed by X-ray diffraction(XRD),and scanning electron microscopy(SEM).In addition,nanohardness,Young’s modulus,and scratch tests are performed.The experimental results show that the films exhibit a nanoscale multilayer structure consisting of TiZrN and ZrN phases.Solid solutions are formed for component TiZrN films.The dominant preferred orientation of TiZrN films is(111) and(220).At a pulsed bias of 200 V,the nanohardness and the adhesion strength of the ZrN/TiZrN multilayer reach a maximum of 38 GPa,and 78 N,respectively.The ZrN/TiZrN multilayer demonstrates an enhanced nanohardness compared with binary TiN and ZrN films deposited under equivalent conditions.     

Optimization of annealing conditions of In2S3 thin films deposited by vacuum thermal evaporation

In₂S₃ thin films were grown on glass substrates by means of the vacuum thermal evaporation technique and subsequently thermally annealed in nitrogen and free air atmosphere from 250 to 350 °C for different durations. Experimental parameters have been adjusted in order to optimize the annealing conditions, and to obtain high band gap energy at low deposition temperature, as required for photovoltaic applications. In order to improve our understanding of the influence of the deposition and annealing parameters on device performance, we have investigated our indium sulfide material by X-ray diffraction, energy dispersive X-ray analysis (EDAX), atomic force microscopy (AFM) and spectrophotometry. The optical and structural properties of the films were studied as a function of the annealing temperature and durations. X-ray diffraction analysis shows the initial amorphous nature of deposited In-S thin films and the phase transition into crystalline In₂S₃ upon thermal annealing. Films show a good homogeneity and optical direct band gap energy about 2.2 eV. An annealing temperature of 350 °C during 60 min in air atmosphere were the optimal conditions.     

Electrochemically deposited photoactive CdIn2Se4 thin films: Structural and optical studies

Electrochemical synthesis of photoactive cadmium-indium-selenide (CdIn₂Se₄) thin films at ambient temperature was reported. The nanocrystalline nature and 1:2:4 elemental chemical stoichiometric ratio for Cd, In and Se were obtained from the X-ray diffraction and energy dispersive X-ray analysis, respectively. Irregular shaped islands of about 400-500 nm in sizes composed of large number of small (∼30-40 nm) spherical grains were confirmed from the atomic force microscopy and the scanning electron microscopy images. The photoelectrochemical measurement of CdIn₂Se₄ film electrode in presence of 1 M polysulphide electrolyte revealed 0.42% photoelectrochemical device conversion efficiency, under the light illumination intensity of 80 mW/cm².     

脉冲偏压电弧离子镀CNx薄膜研究

用脉冲偏压电弧离子镀通过控制不同的氮流量在(100)单晶Si基片上制备了不同成分的CN_x薄膜.用光学显微镜,XPS,XRD,激光Raman和Nanoindenter等方法研究了薄膜的形貌、成分、结构和性能.结果表明,薄膜表面平整致密、氮含量随着氮流量的降低而降低、结构为非晶且为类金刚石薄膜;随着氮含量从18.9%降低到5.3%(摩尔百分比,全文同),薄膜的硬度和弹性模量单调增加而且增幅较大,其中硬度从15.0 GPa成倍增加到30.0 GPa;通过氮流量的调整能够敏感地改变薄膜中的sp³键的含量,是CN_x薄膜的硬度和弹性模量获得大幅度调整的本质原因. 关键词： x薄膜')" href="#">CN_x薄膜 脉冲偏压 电弧离子镀 硬度     

等离激元钼掺杂二氧化钛半导体的光催化固氮反应机理研究

近年来光催化固氮引起了广泛的关注,其代表了将N₂有效转化为NH₃的“绿色工业”的可持续发展路线,如何有效合理地设计这方面的光催化剂仍然是本领域地一个挑战. 本文提出了一种策略,即在高浓度掺杂的TiOsub>2中利用等离激元热电子来激活惰性Nsub>2分子. 成功合成的Mo掺杂TiOsub>2催化剂在常温常压条件下显示出高达134 μmol·g^-1·h^-1的NH₃催化效率,这与传统的等离激元贵金属所实现的催化效率相当. 通过超快光谱技术,发现该体系中的等离激元热电子激活了N₂分子,从而提高了TiO₂的催化活性. 本文为基于等离激元半导体的光催化固氮反应开辟了一条新的途径.     

Characterization of AgInS2 thin films prepared by vacuum evaporation

We characterized AgInS₂ thin films prepared by vacuum evaporation. In the case of thin films annealed at 400 °C, diffraction peaks were observed only for the chalcopyrite AgInS₂ phase. The chemical composition of the thin films annealed at 400 °C was 26.5 at% Ag, 23.8 at% In, and 49.7 at% S. PL spectra of the AgInS₂ thin films at 10.7 K showed peaks at 1.70, 1.80, and 1.83 eV. The PL peak at1.80 eV was attributed to sulfur deficiency.     

Investigation on properties of TiO2 thin films deposited at different oxygen pressures

TiO₂ thin films were prepared by electron beam evaporation at different oxygen partial pressures. The influences of oxygen partial pressure on optical, mechanical and structural properties of TiO₂ thin films were studied. The results showed that with the increase of oxygen partial pressure, the optical transmittance gradually increased, the transmittance edge gradually shifted to short wavelength, and the corresponding refractive index decreased. The residual stresses of all samples were tensile, and the value increased as oxygen partial pressure increasing, which corresponded to the evolutions of the packing densities. The structures of TiO₂ thin films all were amorphous because deposition particles did not possess enough energy to crystallize.     

Cu2ZnSnSe4 thin films prepared by selenization of co-electroplated Cu-Zn-Sn precursors

A novel technique for growth of high quality Cu₂ZnSnSe₄ (CZTSe) thin films is reported in our work. The CZTSe thin films were fabricated onto Mo layers by co-electroplating Cu-Zn-Sn precursors followed by annealing in the selenium vapors at the substrate temperature of 550 °C. The morphology and structure of CZTSe thin films were characterized using scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), X-ray diffraction (XRD) and Raman scattering spectrum, respectively. The results revealed that the single phase was in the CZTSe thin films, and the other impurities such as ZnSe and Cu₂SnSe₃ were not existed though they were difficult to distinguish both from EDS and XRD.     

不同氮流量制备Mn3CuNx薄膜及其电、磁输运性质的研究

采用对靶磁控溅射方法在单晶Si(100)基片上制备了反钙钛矿结构的Mn₃CuN_x薄膜.通过控制制备过程中的反应气体氮气(N₂) 流量(N₂/Ar+N₂), 研究了氮含量对Mn₃CuN_x薄膜结构及物理性能的影响.分别利用X射线衍射仪、俄歇电子能谱、 原子力显微镜、X射线光电子能谱、物理性能测试系统和超导量子干涉仪, 对所制备薄膜的晶体结构、成分、表面形貌和电、磁输运性质进行了测试.结果表明:制备的薄膜均为反钙钛矿立方结构,且沿 (200) 晶面择优生长.随着氮含量的增大,薄膜表面粗糙度和颗粒度尺寸逐渐增大, 导致电阻率增加.氮含量对薄膜的电输运性质没有影响,所有薄膜电阻率均随着温度的降低逐渐增大, 呈现半导体型导电行为,这与对应的块体材料结果相反.Mn₃CuN_x薄膜随着测试温度的增大发生了 亚铁磁到顺磁的磁转变,且N含量的增大降低了磁有序转变温度,主要是由于N缺陷对Mn₆N八面体结构中 磁交换作用的影响所致.     

Characterization of single-crystalline In2O3 films deposited on Y-stabilized ZrO2 (1 0 0) substrates by MOCVD

Epitaxial In₂O₃ films have been deposited on Y-stabilized ZrO₂ (YSZ) (1 0 0) substrates by metalorganic chemical vapor deposition (MOCVD). The films were deposited at different substrate temperatures (450-750 °C). The film deposited at 650 °C has the best crystalline quality, and observation of the interface area shows a clear cube-on-cube epitaxial relationship of In₂O₃(1 0 0)||YSZ(1 0 0) with In₂O₃[0 0 1]||YSZ[0 0 1]. The Hall mobility of the single-crystalline In₂O₃ film deposited at 650 °C is as high as 66.5 cm² V⁻¹ s⁻¹ with carrier concentration of 1.5 × 10¹⁹ cm⁻³ and resistivity of 6.3 × 10⁻³ Ω cm. The absolute average transmittance of the obtained films in the visible range exceeds 95%.     

Far infrared laser frequencies of CH3OD and N2H4

The frequencies of 26 laser lines with wavelengths between 57 and 534 m have been measured in the optically pumped laser gases CH₃OD and N₂H₄. A pair of stabilized cw 12_{CO 2} lasers was used as a frequency standard for the heterodyne frequency measurements. Seven of the 26 lines are new.     

The improvement of Al2O3/AlGaN/GaN MISHEMT performance by N2 plasma pretreatment

This paper discusses the effect of N 2 plasma treatment before dielectric deposition on the electrical performance of a Al2O3 /AlGaN/GaN metal-insulator-semiconductor high electron mobility transistor(MISHEMT),with Al2O3 deposited by atomic layer deposition.The results indicated that the gate leakage was decreased two orders of magnitude after the Al2O3 /AlGaN interface was pretreated by N 2 plasma.Furthermore,effects of N 2 plasma pretreatment on the electrical properties of the AlGaN/Al2O3 interface were investigated by x-ray photoelectron spectroscopy measurements and the interface quality between Al2O3 and AlGaN film was improved.     

Research on the properties of ZnO thin films deposited by using filtered cathodic arc plasma technique on glass substrate under different flow rate of O2

ZnO thin film has been deposited on the glass substrate at a temperature of 200 °C using the filtered cathodic arc plasma (FCAP) technique with the oxygen flow rate of 1.0, 3.0, 5.0, 7.0, 9.0 and 10.0 sccm. The deposition processes are only held in pure oxygen atmosphere. The as-grown films exhibit a polycrystalline hexagonal wurtzite structure. With the oxygen flow rate increase, the crystallinity of the samples first increases and then decreases as measured by X-ray diffractometry (XRD). And the tensile stress exists in all the as-grown thin films. The small grain with a mean diameter of 13 nm is observed by the field emission scanning electron microscopy (FESEM). The electrical resistivity values of the thin films are very low ranging from 5.42 × 10⁻³ Ω cm to 4.0 × 10⁻² Ω cm. According to the result from room temperature photoluminescence spectra measurement, the luminescent bands also depend on the oxygen supply.     

Characterization of TiO2/Au/TiO2 films deposited by magnetron sputtering on polycarbonate substrates

Transparent and conducting TiO₂/Au/TiO₂ (TAuT) films were deposited by reactive magnetron sputtering on polycarbonate substrates to investigate the effect of the Au interlayer on the optical, electrical, and structural properties of the films. In TAuT films, the Au interlayer thickness was kept at 5 nm. Although total thickness was maintained at 100 nm, the stack structure was varied as 50/5/45, 70/5/25, and 90/5/5 nm.In XRD pattern, the intermediate Au films were crystallized, while all TAuT films did not show any diffraction peaks for TiO₂ films with regardless of stack structure. The optical and electrical properties were dependent on the stack structure of the films. The lowest sheet resistance of 23 Ω/□ and highest optical transmittance of 76% at 550 nm were obtained from TiO₂ 90 nm/Au 5 nm/TiO₂ 5 nm films. The work function was dependent on the film stack. The highest work function (4.8 eV) was observed with the TiO₂ 90 nm/Au 5 nm/TiO₂ 5 nm film stack. The TAuT film stack of TiO₂ 90 nm/Au 5 nm/TiO₂ 5 nm films is an optimized stack that may be an alternative candidate for transparent electrodes in flat panel displays.