负偏压对磁控溅射Ti膜沉积速率和表面形貌的影响

 采用直流磁控溅射加负偏压的方法制备了Ti膜,研究了不同偏压条件对Ti膜沉积速率、密度、生长方式及表面形貌的影响。随着偏压逐渐增大,Ti膜沉积速率分三个阶段变化:0~ -40 V之间沉积速率基本不变; -40~ -80 V之间沉积速率迅速降低;超过-80 V后沉积速率随偏压的下降速度又放缓。Ti膜密度随偏压增加而增大,负偏压为-119.1 V时开始饱和并趋于块体Ti材密度。加负偏压能够抑制Ti膜的柱状生长方式;偏压可以改善Ti膜的表面形貌,对于40 W和100 W的溅射功率,负偏压分别在-100 V和-80 V左右时制备出表面光洁性能较佳的Ti膜。     

Thermal and complex impedance analysis of amorphous and crystalline lithium salt mixtures

Amorphous electrolytes consisting of the lithium salts, Li[R-NSO₂CF₃] were prepared and the attendant low ionic conductivities of the lithium salt mixtures (1×10⁻⁶ S cm⁻¹ at room temperature) are attributed to high glass transition temperatures. An example is the novel amorphous salt, Li[18-C-6NSO₂CF₃] which produces an amorphous salt mixture with Li[N(SO₂CF₃)₂] (LiTFSI).     

磁控溅射制备微球表面金属Mo涂层的研究

利用磁控溅射制备了各种工艺参数不同的微球表面金属Mo涂层样品,并通过白光干涉仪和扫描电子显微镜对样品的表面及剖面进行了系统的测试分析。分别探究了溅射工作气压和沉积制备时间对微球表面Mo涂层表面形貌以及结晶质量的影响规律。结果表明通过优化工艺参数可制备微球直径约为800μm、涂层厚度为3.5μm到14.1μm、厚度均匀性良好的微球表面Mo涂层。Mo涂层中的晶粒呈现出柱状结构致密堆积在一起,且随涂层的厚度增加晶粒间空隙增大。     

AlN/Al dual protective coatings on NdFeB by DC magnetron sputtering

AlN/Al dual protective coatings were prepared on NdFeB by DC magnetron sputtering in a home-made industrial apparatus. Comparing with Al coating, AlN/Al coatings have a denser structure of an outmost AlN amorphous layer following an inner Al columnar crystal layer. The coatings and NdFeB substrate combine well, and moreover, there is occurrence of metallurgy bonding in the interface layer. Both Al and AlN/Al coatings have a good protective ability to NdFeB. Especially, the corrosion resistance of AlN/Al coated NdFeB is improved largely. AlN/Al and Al protective coatings not only do not deteriorate the magnetic properties of NdFeB, but contribute to their slight increase.     

Room temperature deposition of crystalline indium tin oxide films by cesium-assisted magnetron sputtering

Indium tin oxide (ITO) films were deposited on a Si (1 0 0) substrate at room temperature by cesium-assisted magnetron sputtering. Including plasma characteristics, the structural, electrical, and optical properties of deposited films were investigated as a function of cesium partial vapor pressure controlled by cesium reservoir temperature. We calculated the cesium coverage on the target surface showing maximum formation efficiency of negative ions by means of the theoretical model. Cesium addition promotes the formation efficiency of negative ions, which plays important role in enhancing the crystallinity of ITO films. In particular, the plasma density was linearly increased with cesium concentrations. The resultant decrease in specific resistivity and increase in transmittance (82% in the visible region) at optimum cesium concentration (4.24 × 10⁻⁴ Ω cm at 80 °C of reservoir temperature) may be due to enhanced crystallinity of ITO films. Excess cesium incorporation into ITO films resulted in amorphization of its microstructure leading to degradation of ITO crystallinity. We discuss the cesium effects based on the growth mechanism of ITO films and the plasma density.     

Deposition of nanostructured crystalline and corrosion resistant alumina film on bell metal at low temperature by rf magnetron sputtering

Aluminium oxide films deposited by rf magnetron sputtering for protective coatings have been investigated. The alumina films are found to exhibit grainy surface microstructure. The grain size, structure and density depend on different system parameters such as argon and/or oxygen flow rate and applied rf power etc. The effect of transition of the discharge from metallic to reactive mode on the surface characteristics of the alumina film is studied. X-ray diffractometry reveals that in poisoned mode of sputtering and under optimized power and pressure, crystalline alumina film can be grown. Different system conditions are optimized for corrosion resistant aluminium oxide films with good adhesion properties. Nanostructured alumina film is obtained at lower pressure (8 × 10⁻⁴ to 9 × 10⁻⁴ Torr) by rf reactive magnetron sputtering.     

Synthesis of Fe-based amorphous composite coatings with low purity materials by laser cladding

Amorphous composite coatings Fe₃₈Ni_30−XSi₁₆B₁₄V₂M_X (X = 0, 1, 2) (M contains Al, Ti, Mo, and C) were prepared with low purity of raw materials by laser cladding. X-ray diffraction and transmission electron microscopy results show that the coating have an amorphous structure with a few crystalline phase on it. The amorphous phase is the primary phase. The glass forming ability as well as the microhardness of the Fe-based alloy made from low purity raw materials can be much enhanced by adding small amount of multi-components. However, the elements addition has its optimal quantity. When X is equal to 1, the microstructure of the coating contains 97.93% amorphous phase and 2.07% crystalline phase on it. As a result, the microhardness of the coating reaches maximum. With further increasing of the additions, the amorphous phase in the coating lessens instead of augment and the crystalline phase begins to accumulate, which result in the decrease of the microhardness.     

Study of hydrogenated amorphous silicon nitride films prepared by RF magnetron sputtering

Hydrogenated amorphous silicon nitride films have been deposited by the rf magnetron sputtering method with non-stoichiometric and stoichiometric compositions using a poly-Si target and a mixture of Ar, H₂ and N₂ as the sputtering gas. Data on optical and infrared absorption, electrical conductivity, breakdown voltage, capacitance measurements and thermal evolution of hydrogen have been presented as a function of nitrogen concentration in the films, especially in the stoichiometric region of composition. Attempts have been made to identify the roles of hydrogen and nitrogen in determining the electrical and optical properties and thermal stability exhibited by the films. Properties relevant for device application of the material have been shown to be comparable to those obtained by glow discharge or electron cyclotron resonance plasma chemical vapour deposition methods of deposition. RF magnetron sputtering has therefore been suggested as a viable alternative to the more widely adopted CVD methods for device applications of silicon nitride, where the use of hazardous process gases can be avoided.     

Development of protective metal coatings on aluminum by magnetron sputtering

Depositions of copper and titanium coatings on aluminum foils and polished aluminum plates for thier protection against corrosion in alkaline media were performed. The coatings were deposited in three different types of magnetron sputtering systems: a direct current (DC) magnetron discharge, a high current impulse magnetron discharge, and a DC magnetron discharge with melted cathode. Only aluminum foils coated with copper films obtained by combined ion-plasma technology, which included preliminarily sputtering of the aluminum surface with an ion beam, deposition of a dense interlayer in the DC magnetron discharge with ion assistance of initial stage of deposition, and deposition of additional layer in the magnetron discharge with melted cathode, were resistant against 30 wt % NaOH solution.     

Effects of Cr doping on physical properties of amorphous In-Ga-Zn-O films

Amorphous thin films of InGaZnO₄ (a-IGZO) doped with Cr have been fabricated by using pulsed-laser deposition (PLD). The electrical, optical and magnetic properties of Cr-doped a-IGZO films grown at 25 °C and 150 °C were investigated. The conductivity, optical transmission and band gap of films are remarkably enhanced by increasing the growth temperature. Conductivity, carrier concentration and mobility decrease with increasing the Cr content. However, the optical transmission and band gap are not significantly affected by Cr doping. Moreover, all Cr-doped films exhibit room-temperature ferromagnetism.     

Structural and tribological properties of CrTiAlN coatings on Mg alloy by closed-field unbalanced magnetron sputtering ion plating

In this paper, a series of multi-layer hard coating system of CrTiAlN has been prepared by closed-field unbalanced magnetron sputtering ion plating (CFUBMSIP) technique in a gas mixture of Ar + N₂. The coatings were deposited onto AZ31 Mg alloy substrates. During deposition step, technological temperature and metallic atom concentration of coatings were controlled by adjusting the currents of different metal magnetron targets. The nitrogen level was varied by using the feedback control of plasma optical emission monitor (OEM). The structural, mechanical and tribological properties of coatings were characterized by means of X-ray photoelectron spectrometry, high-resolution transmission electron microscope, field emission scanning electron microscope (FESEM), micro-hardness tester, and scratch and ball-on-disc tester. The experimental results show that the N atomic concentration increases and the oxide on the top of coatings decreases; furthermore the modulation period and the friction coefficient decrease with the N₂ level increasing. The outstanding mechanical property can be acquired at medium N₂ level, and the CrTiAlN coatings on AZ31 Mg alloy substrates outperform the uncoated M42 high speed steel (HSS) and the uncoated 316 stainless steel (SS).     

磁控反应溅射法制备渐变折射率薄膜的模型分析

阐述了磁控反应溅射法制备渐变折射率薄膜的机理;探讨了磁控反应溅射法制备渐变折射率薄膜的理论模型,给出了渐变折射率薄膜的折射率与反应气体分压的关系,在一定的沉积参数下,由要得到的膜层折射率随膜层几何厚度的变化规律可推导出反应气体分压比随时间的变化规律;最后以制备折射率线性变化的薄膜为例说明了如何推导得到反应气体分压比随时间的变化规律. 关键词： 渐变折射率 磁控反应溅射 模型     

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利用在线椭偏仪对非晶碳氢膜进行了光学常数、沉积率和刻蚀率的测量。在无直流负偏压或偏压较小时,薄膜呈现聚合物结构,折射率和消光系数较小;当增加直流负偏压时,薄膜的折射率和消光系数显著提高,所成膜为硬质非晶碳氢膜。在以CH4作为气源进行沉积时,随着偏压的增加,沉积率先升高再降低,在偏压为-100V时,沉积率为最大。H2/N2(30%N2)的混合气体的刻蚀率要比单独用H2作为刻蚀气体的刻蚀率要大。对于CH4/N2(30%N2),在偏压从0V增加到300V过程中,在大约50V时,基底上的薄膜有一个从沉积到刻蚀的转化过程。     

Aluminium-induced crystallization of amorphous silicon films deposited by DC magnetron sputtering on glasses

Amorphous silicon (a-Si) and hydrogenated amorphous silicon (a-Si:H) films were deposited by DC magnetron sputtering technique with argon and hydrogen plasma mixture on Al deposited by thermal evaporation on glass substrates. The a-Si/Al and a-Si:H/Al thin films were annealed at different temperatures ranging from 250 to 550 °C during 4 h in vacuum-sealed bulb. The effects of annealing temperature on optical, structural and morphological properties of as-grown as well as the vacuum-annealed a-Si/Al and a-Si:H/Al thin films are presented in this contribution. The averaged transmittance of a-Si:H/Al film increases upon increasing the annealing temperature. XRD measurements clearly evidence that crystallization is initiated at 450 °C. The number and intensity of diffraction peaks appearing in the diffraction patterns are more important in a-Si:H/Al than that in a-Si/Al layers. Results show that a-Si:H films deposited on Al/glass crystallize above 450 °C and present better crystallization than the a-Si layers. The presence of hydrogen induces an improvement of structural properties of poly-Si prepared by aluminium-induced crystallization (AIC).     

Color and optical characteristics of carbon coatings produced by magnetron sputtering

The color parameters of carbon coatings deposited by magnetron sputtering of a graphite target onto substrates of stainless steel without a sublayer and with a titanium sublayer are calculated. By numerical modeling, the refractive indices and extinction coefficients for the titanium sublayer and carboniferous film as well as the volume content of titanium dioxide in the sublayer are determined. Physico-Technical Institute of the Academy of Sciences of Belarus, 4, Zhodinskaya St., Minsk, 220141, Belarus. Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 64, No. 3, pp. 374–385, May–June, 1997.     

脉冲磁控溅射法制备单斜相氧化铒涂层

用中频脉冲反应磁控溅射法,在溅射功率为78 W,93 W和124 W以及衬底温度分别为室温,500 ℃及677 ℃下制备了氧化铒涂层.采用原子力显微镜、纳米压痕、X射线衍射和掠入射X射线衍射法研究了涂层的形貌、力学性能及物相结构.测量了涂层的电学性能.结果显示,脉冲磁控溅射沉积氧化铒涂层具有较高的沉积速率.实验制备得到了单斜相结构的氧化铒涂层.提高溅射功率时,沉积速率从28 nm/min增大至68 nm/min,涂层的结晶质量显著下降.提高衬底温度至500 ℃和677 ℃时,单斜相衍射峰强度下降.分析认为 关键词： 氧化铒 脉冲磁控溅射 单斜晶相     

(Ti,Al,Si,C)N nanocomposite coatings synthesized by plasma-enhanced magnetron sputtering

Materials’ surface service property could be enhanced by transition metal nitride hard coatings due to their high hardness, wear and high temperature oxidation resistance, but the higher friction coefficient (0.4-0.9) of which aroused terrible abrasion. In this work, quinternary (Ti,Al,Si,C)N hard coating 3-4 μm was synthesized at 300 °C using plasma enhanced magnetron sputtering system. It was found that the coating's columnar crystals structure was restrained obviously with the increase of C content and a non-columnar crystals growth mode was indicated at the C content of 33.5 at.%. Both the XRD and TEM showed that the (Ti,Al,Si,C)N hard coatings had unique nanocomposite structures composed of nanocrystalline and amorphous nc-(Ti,Al)(C,N)/nc-AlN/a-Si₃N₄/a-Si/a-C. However, the coatings were still super hard with the highest hardness of 41 GPa in spite of the carbon incorporation. That a-C could facilitate the graphitization process during the friction process which could improve the coating's tribological performance. Therefore, that nanocomposite (Ti,Al,Si,C)N coatings with higher hardness (>36 GPa) and a lower friction coefficient (<0.2) could be synthesized and enhance the tribological performance and surface properties profoundly.     

Influence of Cr interlayer on the structure and optical properties of Ag films on glass substrate by magnetron sputtering

Optical properties and microstructure of Ag film on glass substrate with Cr intermediate layer were studied by using spectrophotometer and XRD. The spectra results showed that introducing Cr intermediate layer reduced the surface roughness and promoted the reflectivity of Ag film. The XRD analysis showed that the crystalline grains increased and the stress decreased. The adhesion was also improved by using the tape test method.     

Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems

Solid polymer electrolytes (SPEs) contain amorphous and crystalline regions, each of which have unique contributions to the ¹³C NMR spectrum. Understanding and assigning the ¹³C NMR signals are vital to interpreting the NMR data collected for each phase. The ¹³C CPMAS solid-state NMR spectrum of poly(ethylene oxide), a common polymer electrolyte host material, has superimposed broad and narrow components. Previously, the narrow component has been assigned to the amorphous region and the broad component to the crystalline PEO fraction. These assignments for pure PEO have been applied to various PEO:salt systems. Using lithium triflate salt dissolved in PEO, we revisit the spectral assignments and discover that the narrow component is due to crystalline PEO:LiTf component, which is reversed from the previous pure PEO assignment. This paradigm shift is based on data collected from a 100% crystalline PEO:LiTf with a 3:1 oxygen:lithium ratio sample, which exhibited only the narrow peak. For dilute electrolytes, such as 20:1 PEO:LiTf, the ¹³C CPMAS spectra contain the narrow peak superimposed on a broad peak as seen with pure PEO. As dilute electrolytes are heterogeneous with crystalline and amorphous regions of both pure PEO and PEO:LiTf complex, peak assignments for pure PEO and PEO:LiTf are important. Thus, we reexamine the previous assignment for pure PEO using samples of pure powdered PEO, thermally treated pure powdered PEO, and a thin film PEO cast from an acetonitrile solution. With these different samples, we observed the growth of the narrow peak under conditions that favor crystallization. Therefore, for pure PEO, we have reassigned the narrow peak to the crystalline region and the broad peak to the amorphous region. In light of our observations, previous NMR studies of pure PEO and PEO SPEs should be reinvestigated. We also use rotational echo double resonance (REDOR) to study the 20:1 PEO:LiTf created from 2 and 100 kDa PEO. We find that the lithium environment is similar in the respective microcrystalline domains. However, the 100 kDa samples have a larger fraction of pure crystalline PEO.     

直流磁控溅射制备氧化钒薄膜

讨论了在低温下以高纯金属钒作靶材,用直流磁控溅射的方法制备出了氧化钒薄膜。通过设计正交试验,分析了氩气和氧气的流量比,溅射功率,工作压强,基底温度对氧化钒薄膜沉积速率和电阻温度系数TCR的影响,采用RTP-500型快速热处理机对氧化钒薄膜样品进行了退火热处理,实验结果表明:当Ar与O2的比例为100:4,溅射功率为120W,工作压强为2Pa时,所获得薄膜TCR较大,都在-2%/K附近,最高的可达-3.6%/K。