Characterization of titanium nitride films deposited by cathodic arc plasma technique on copper substrates

TiN films were deposited directly on Cu substrates by a cathodic arc plasma deposition technique. The films were then characterized by X-ray diffraction (XRD), grazing incidence X-ray diffraction (GID), (TEM), Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS). The preferred orientation of the film changed from (200) to (111) with increasing film thickness. Analyses of both the XRD and GID results showed that in the highly (111) textured grains, the (111) plane was approximately parallel to the film surface, while in the (200) textured grains, the (200) plane was tilted away from the film surface. Small-elongated crystallites with a large aspect ratio and textured grains were found on the TiN surface. AES, which was employed to examine the concentration depth profile, showed no apparent interdiffusion between Cu and TiN during the growth of the film. XPS results showed that amorphous TiO₂, as well as titanium oxynitride, was present on the TiN surface. The spectra of Ti-2p, N-1s, O-1s and Cu-2p before and after the film being sputter etched through the entire film region were also discussed.     

Properties of doped ZnO transparent conductive thin films deposited by RF magnetron sputtering using a series of high quality ceramic targets

To obtain high transmittance and low resistivity ZnO transparent conductive thin films,a series of ZnO ceramic targets (ZnOAl,ZnO(Al,Dy),ZnO(Al,Gd),ZnO(Al,Zr),ZnO(Al,Nb),and ZnO(Al,W)) were fabricated and used to deposit thin films onto glass substrates by radio frequency (RF) magnetron sputtering.X-ray diffraction (XRD) analysis shows that the films are polyerystalline fitting well with hexagonal wurtzite structure and have a preferred orientation of the (002) plane.The transmittance of above 86% as well as the lowest resistivity of 8.43 x 10-3 Ω·cm was obtained.     

声表面波器件用SiO2/ZnO/金刚石/Si多层结构制备

为获得高频、高性能金刚石声表面波器件的多层结构,在金刚石/Si衬底使用磁控溅射方法优化ZnO与SiO₂薄膜沉积工艺参数,制备了具有正负温度系数组合的SiO₂/ZnO/金刚石/Si多层结构,并对多层结构进行表征。结果表明:随着氩氧比增加,ZnO薄膜的沉积速率不断加快,薄膜的表面粗糙度不断增大;ZnO薄膜中的原子摩尔分数比随O₂输入量的减少而逐渐接近理想的1∶1。不同氩氧比下制备的ZnO薄膜均呈(002) 面择优取向生长,其中在氩氧比7∶1时,获得了具有细小柱状晶特征、C轴择优取向程度较高的ZnO薄膜。采用最优的ZnO和SiO₂薄膜沉积工艺,在金刚石/Si衬底获得了具有清晰界面的SiO₂/ZnO/金刚石/Si多层结构。      

Effect of ammonia solution on properties of sprayed ZnO thin films consisting of nano-pyramids

Hexagonal wurtzite zinc oxide (ZnO) thin films were deposited at substrate temperatures from 300 to 500 °C with surfactant of ammonia solution. The effect of ammonia on the structural, surface morphology, compositional, optical and electrical properties of ZnO thin films was studied. X-ray diffraction shows that the all films are polycrystalline in nature and have a hexagonal wurtzite structure with a high preferential orientation (002) plane for ammonia solution. High-resolution SEM studies reveal the formation of ZnO films consisting of nano-pyramids with uniformly distributed grains over the entire surface of the substrates. Photoluminescence studies indicate the presence of two emission peaks: (a) a sharp ultra-violet near band edge ～392 nm, (b) a sharp visible deep-level green emission peak ～564 nm. The optical properties show that the direct band gap energy values increase with increasing substrate temperatures.     

Synthesis and characterization of CrZrAlN films using unbalanced magnetron sputtering with segment targets

In this work, CrZrAlN thin films with various Al contents were synthesized with an unbalanced magnetron sputtering technique using segment targets. Microstructure, surface morphology, and film hardness were investigated as functions of the Al content; X-ray diffraction, atomic force microscopy, and a microhardness tester were used to carry out the investigations. The thermal stability of the films as a function of the Al content was evaluated by annealing the films at temperatures up to 500 °C for 30 min in air. The synthesized CrZrAlN thin films with Al content from 0 to 12.9 at.% consisted mainly of the crystalline NaCl B1 fcc solid solution phase. With the addition of Al to the CrZrN thin film, the microstructure of the film changed from dense and compact to a columnar structure, and the preferred orientation of the films changed from (111) to (200) plane. The hardness of the film decreased slightly as the Al content increased, and the thermal stability of the CrZrAlN thin films deteriorated. The columnar microstructure in the CrZrAlN thin film is believed to provide a fast route for oxygen to diffuse, resulting in a poor oxidation resistance of the film. Contrary to expectations, the addition of Al to the CrZrN thin film did not improve the oxidation resistance of the film. A way to break the columnar microstructure of the CrZrAlN thin film should be developed in order to improve the oxidation resistance of the film.     

Zn靶与掺铝ZnO靶共溅射制备ZnO:Al薄膜及其性能

采用Zn靶和ZnO(掺2%Al2O3(质量分数))陶瓷靶在玻璃衬底上共溅射沉积Al掺杂ZnO薄膜,即ZnO:Al透明导电薄膜,研究Zn靶溅射功率(0～90 W)和衬底温度(室温、100℃和200℃)对薄膜结构、形貌、光学和电学性能的影响。结果表明:按双靶共溅射工艺制备的ZnO:Al薄膜的晶体结构均为六角纤锌矿结构,且随着Zn靶溅射功率的增加,薄膜的结晶质量呈现出先改善后变差的规律,薄膜中的载流子浓度逐渐升高,电阻率逐渐降低,而薄膜的光学性能受其影响不大;随着衬底温度的升高,薄膜的结晶性能得到改善,薄膜的可见光透过率增强,电阻率降低。     

Fabrication of YBCO films on Ag substrate by TFA-MOD method

Biaxial aligned YBCO films have been successfully deposited on Ag { 110 } (110) textured polycrystalline substrates by metal-organic decomposition (MOD) method using Trifluoroacetate Salt (TFA). The influence of firing temperature and Ag surface defects on phase purity and texture, surface morphology of YBCO films was studied. Holding temperature at 900℃ for 30 rain benefits to improve orientation and connectivity of YBCO films. The surface of YBCO films deposited on unpolished Ag substrate has many holes and stripes, which are parallel to the rolling stripe on Ag substrates. To eliminate the rolling stripe on the Ag surface, Ag substrates were polished prior to films deposition. The film grown on polished Ag substrates has a smooth surface and good connectivity of grains without parallel stripes. The YBCO films have an onset of transition around 90K and critical current densities of 15000 A/cm^2.     

Effect of substrate bias voltage on the texture and microstructure of Cu thin films deposited by ion beam deposition

Cu thin films deposited by non-mass separated ion beam deposition under various substrate bias voltages were investigated. The film textures and microstructure were analyzed by X-ray diffraction and field emission scanning electron microscopy, and the resistivity of the film was measured with the Van der Pauw method. It was found that the optimum negative substrate bias voltage for Cu films was −50 V. The Cu films deposited without substrate bias voltage showed a columnar grain structure with small grains and random orientation. However, when a substrate bias voltage of −50 V was applied, the Cu films had a non-columnar structure with a strong (111) texture and large grains. The electrical resistivity of the Cu films decreased remarkably with increasing negative substrate bias voltage, and reaching a minimum value of 1.8±0.13 μΩ cm at the substrate bias voltage of −50V.     

The effect of substrate bias voltage on PbTe films deposited by magnetron sputtering

The PbTe films were deposited onto ITO glass substrate by radio frequency magnetron sputtering. Effect of external direct current electrical field applied between substrate and target on the quality of films was investigated. Stylus surface profile, X-ray diffraction (XRD), atomic force microscope (AFM) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the films. The film thickness was measured by a conventional stylus surface profile. The crystal structure and lattice parameters of films were determined by using XRD. The surface morphology of the films was measured by AFM. The absorption coefficients and optical band gaps of films were found from FTIR. The sheet resistance of the samples was measured with a four-point probe and the resistivity of the film was calculated. All the obtained films were highly textured with a strong (2 0 0) orientation. With increasing bias voltage to −30 V, the property of crystal structure, surface morphology and absorption coefficients and resistivity were improved. However, further increase of substrate bias leads to transformation of the property.     

High rate reactive magnetron sputtering of ZnO:Al films from rotating metallic targets

Aluminum doped zinc oxide (ZnO:Al) films were reactively sputtered at a high discharge power from dual rotating metallic targets (Zn:Al = 99.5:0.5 wt.%). Deposition conditions like substrate temperature and working points were varied in order to prepare high quality ZnO:Al films. The influences on electrical and optical ZnO:Al thin film properties and surface texture before and after chemical etching in diluted HCl were studied in order to achieve light scattering films as front contact for solar cells. High dynamic deposition rate close to 90 nm m/min and high Hall mobility of up to 47 cm²/Vs were obtained. Transmission of more than 85% in the visible spectral range is obtained for all ZnO:Al films in this study. In addition, the absorption in near infrared region is low due to low doping. Surface texture after etching is usually much rougher than before. However, some films reveal after etching small surface features that are similar to initial surface features. We propose a relationship between initial and post-etched surface textures.     

气压对离子源增强磁控溅射制备氮化铝薄膜的影响

目的 制备性能优异的氮化铝薄膜.方法 采用射频感应耦合离子源辅助直流磁控溅射的方法 制备氮化铝薄膜,在不同的气压下,在Si(100)基片和普通玻璃上生长了不同晶面取向的氮化铝薄膜.使用X射线衍射仪(XRD)、场发射扫描电镜(FESEM)、原子力显微镜(AFM)分析氮化铝薄膜的结构、晶面取向、表面形貌及薄膜表面粗糙度,使用紫外可见分光光度计测定薄膜的透过率,并计算薄膜的禁带宽度.研究气压的大小对磁控溅射制备氮化铝薄膜微观结构的影响.结果 在各气压下,薄膜生长以(100)面取向为主.在0.7Pa前,(100)面的衍射峰强度逐渐增强,0.7 Pa之后减弱.(002)面衍射峰强度在0.6Pa之前较大,0.6Pa之后变小.各气压下薄膜表面均方根粗糙度均小于3nm,且随着气压的增大先增大后减小,0.7 Pa时最大达到2.678nm.各气压下所制备薄膜的透过率均大于60%,0.7Pa时薄膜的禁带宽度为5.4eV.结论 较高气压有利于(100)晶面的生长,较低气压有利于(002)晶面的生长;(100)面衍射峰强度在0.7 Pa时达到最大;随气压的增大,薄膜表面粗糙度先增大后减小;所制备的薄膜为直接带隙半导体薄膜.     

低模量Ti6Al4V表面Ti(Al/Pt)N薄膜强化改性

为解决硬质薄膜因与软基体硬度和模量差较大导致的薄膜失效问题,提高硬质薄膜在Ti6Al4V(TC4)钛合金基体上的适应性,使用掺杂氮化钛（TiN）陶瓷薄膜对低模量Ti6Al4V合金表面强化。采用热丝增强等离子体磁控溅射技术在Ti6Al4V合金表面制备Ti(Al/Pt)N薄膜：包括本征TiN、Al&Pt掺杂TiAlN和TiAl(Pt)N薄膜。采用扫描电子显微镜、X-射线衍射仪、纳米压痕仪、洛氏硬度计和摩擦磨损测试仪分别表征三种薄膜组织形貌、能谱分析、相结构和内应力、纳米硬度和模量及耐磨性。结果表明：Al元素掺杂使TiN薄膜柱状晶细化,截面形貌柱状晶更致密;同时微量Pt掺杂后,截面断口呈韧性撕裂。本征TiN和TiAlN薄膜衍射峰图谱呈现TiN(111)取向,TiAl(Pt)N薄膜的衍射峰呈TiN(200)主峰位。Al元素掺杂使TiN薄膜晶格畸变增多,内应力从-13 MPa增大到-115 MPa,导致膜-基结合力恶化,洛氏压痕和摩擦磨损实验中均出现薄膜剥落。Pt掺杂后薄膜内应力降低到-66 MPa,在洛氏压痕试验中TiAl(Pt)N薄膜与基体结合良好,仅有少许环形裂纹。摩擦磨损试验中本...     

基体温度对磁控溅射TiN薄膜电化学性能的影响

采用直流反应磁控溅射方法在AISI 304不锈钢和Si(100)表面沉积了TiN薄膜,利用场发射扫描电镜、X射线衍射仪和电化学技术研究了基体温度对TiN薄膜结构与电化学性能的影响。结果表明:TiN薄膜为柱状结构,表面平整、致密,但基体温度高于300℃时膜表面存在微裂纹。薄膜为面心立方结构δ-TiN并存在择优取向,室温和150℃时的薄膜择优取向为(111)晶面,300℃和450℃时为(200)晶面;基体为室温时薄膜厚度为0.63μm,温度提高到150℃后膜厚增加到1μm左右,但继续升温对膜厚影响并不明显。薄膜在NaCl溶液中的腐蚀为点蚀,基体温度为150℃时的TiN薄膜具有最高的开路电位和点蚀电位以及最低的腐蚀速率,因此具有最佳的耐蚀性。     

Anisotropy and texture in thin copper films—an elasto-plastic analysis

The role of elastic anisotropy on the stress inhomogeneity and effective behavior of columnar grained textured Cu thin films have been analyzed within a continuum framework. The analysis is based on a three-dimensional model of a film/substrate system. The film exhibits a fiber texture with (111), (001) and randomly oriented grains. Mainly two load cases have been considered. Biaxial loading of a film deposited on a silicon substrate and tensile loading of a film deposited on a polyimide substrate. The stress distributions in the (111) and (001) grains were generally found to be very different when subjected to biaxial loading and quite similar when subjected to tensile loading. When plastic behavior is invoked, a structural hardening effect is observed. The plastic behavior differs significantly between biaxial and tensile cyclic loading respectively. A new orientation dependent hardening law is proposed. This hardening law causes the plastic hardening behavior to be orientation dependent and scale with elastic anisotropy. The newly proposed hardening law is demonstrated on a film with small grain aspect ratio.     

MICROSTRUCTURE AND PROPERTIES OF ANNEALED ZnO THIN FILMS DEPOSITED BY MAGNETRON SPUTTERING

1.IntroductionZnO especially in the form ofthin film shasbeen attracting attention because ofits m any applica-tions,such astransparentelectrodes,varistors,phosphors,gassensors,surface acousticw ave devicesandpiezoelectric actuators[1,2].M ore recently,re…     

Spray deposited superhydrophobic ZnO coatings via seed assisted growth

Superhydrophobic zinc oxide (ZnO) coatings were synthesized by a simple and cost-effective spray pyrolysis technique (SPT) via seed assisted growth onto the glass substrates at 723 K from an aqueous zinc acetate precursor solution. Initially, the ZnO seeds were synthesized from an aqueous 0.4 M zinc acetate solution onto the glass substrates at 723 K. For the seed assisted growth of ZnO, the solution concentrations (0.1 M to 0.4 M) were used and its effect on structural, morphological, optical and wettability properties of ZnO thin films was investigated. The synthesized films were found to be polycrystalline, with preferential growth along c-axis. Scanning electron microscopy (SEM) images show the uniform distribution of spherical grains of about 60-80 nm grain size. After seed assisted growth, film surface becomes very rough. The films were specular and transmittance of thin films decreases as the concentration of the precursor solution increases. The optical absorption spectrum shows a sharp absorption band-edge at 381 nm, corresponding to optical gap energy (Eg) of 3.25 eV. All samples are superhydrophobic in nature. The Zn4 sample shows the superhydrophobicity with highest value of the contact angle (CA) i.e. 165°. Such a superhydrophobic coatings can be useful in the anti-snow, anti-fog and self cleaning surfaces.     

Boron and fluorine doped ZnO films obtained from zinc chloride precursor via chemical spray pyrolysis

Both boron (1, 2 and 3 at %) and fluorine (1, 3, 5 and 7 at %) doped zinc oxide thin films (ZnO:B:F) were fabricated using zinc chloride precursor by airbrush spray pyrolysis technique on glass substrates. X-ray diffraction (XRD) measurements show that all ZnO:B:F films have hexagonal wurtzite structure with a preferential growth along the [0 0 2] direction on glass substrates. Scanning electron microscope (SEM) results show that the morphologies of all doped films have a regular hexagonal shape. The optical measurements reveal that ZnO:B:F films have a direct band gap and optical energy gaps are increasing with boron and fluorine concentration. The optical transmittance of B and F doped ZnO films is measured very low due to columnar structure of prepared films. Moreover, it has been observed that the doping of ZnO films with boron and fluorine decreases the electrical resistance, and the lowest resistances of films were observed at 1%B–3%F and 2%B–3%F concentrations.     

Study on nanocrystalline Cr2O3 films deposited by arc ion plating: I. composition, morphology, and microstructure analysis

Nanocrystalline Cr₂O₃ thin films were deposited on silicon wafers with (100) orientation by arc ion plating (AIP) technique at various negative bias voltages. By virtue of X-ray diffraction analysis, scanning electron microscope, and high-resolution transmission electron microscope, the influence of substrate bias voltage on the film growth process, microstructure, and characteristics was investigated systematically, including the phase constituents, grain size, lattice constant, chemical compositions, as well as surface and cross-section morphologies. With increasing the bias voltage, the grain size and lattice constant of AIP Cr₂O₃ films first decreased slightly, and then increased gradually again. Both reached the minimum (35 nm and 13.57 Å) when the bias voltage was − 100 V. However, the bias voltage had little effect on the phase constituents and chemical compositions of AIP Cr₂O₃ films. During the film growth process, the surfaces of Cr₂O₃ films were getting smoother with the negative bias voltage increase, in the meantime, their microstructures evolved from coarse columnar grains to fine columnar grains, short columnar recrystallized grains, and fine columnar grains again.     

Influence of post-grown treatments on CuInS2 thin films prepared by sulphurization of Cu-In films

Polycrystalline CuInS2 (CIS) films were prepared by sulphurization of Cu-In films.The surface morphology and phase composition of the as-grown film,the KCN-etched film,and the annealed KCN-etched film were investigated.During the sulphurization,the secondary CuχS phase segregated on the surface of the as-grown films.To improve the crystalline quality of CulnS2 films,a series of post-grown treatments,such as KCN-etching and vacuum annealing KCN-etched films,were performed on the as-grown films.Both as-grown and post-treated films were characterized by X-ray diffraction (XRD),scanning electron microscopy (SEM),and energy dispersive spectroscopy (EDS).The results indicated that a CuχS secondary phase segregated on the surface of the as-grown film,which could be removed effectively by KCN etching.After the vacuum annealing treatment,the KCN-etched film had a sphalerite structure with (112) preferred orientation.Meanwhile,the crstalline quality of the CIS film was significantly improved,which provided a novel method to improve the performance of thin film solar cells.     

Site-specific synthesis of ZnO nanocrystalline networks via a hydrothermal method

ZnO nanocrystalline networks (NCNWs) consisting of percolating nanocrystals with irregular shape and size were synthesized using Al seed layers in a hydrothermal process. Various thicknesses of Al films were used to assess the effects of film thickness on the formation of ZnO NCNWs; the coverage and size of the ZnO nanocrystals increased with an increasing Al film thickness. In addition, by exploiting the seed layer-dependent crystal growth behaviors, two distinctly different ZnO nanostructures, nanorods on ZnO seed and NCNWs on Al seed, could be selectively achieved on the same substrate under the same growth conditions. Spectrally- and spatially-resolved investigations of these two ZnO nanostructures were performed using cathodoluminescence, which provided a significant opportunity to study the effect of the nanostructures on the luminescent characteristics. The ZnO NCNWs have an extremely high surface to volume ratio and sufficient inter-space, which enabled the conversion of the surface property from hydrophilic to superhydrophobic.