Comparative study of zinc oxide and aluminum doped zinc oxide transparent thin films grown by direct current magnetron sputtering

Pure and aluminum (Al) doped zinc oxide (ZnO and ZAO) thin films have been grown using direct current (dc) magnetron sputtering from pure metallic Zn and ceramic ZnO targets, as well as from Al-doped metallic ZnAl2at.% and ceramic ZnAl2at.%O targets at room temperature (RT). The effects of target composition on the film's surface topology, crystallinity, and optical transmission have been investigated for various oxygen partial pressures in the sputtering atmosphere. It has been shown that Al-doped ZnO films sputtered from either metallic or ceramic targets exhibit different surface morphology than the undoped ZnO films, while their preferential crystalline growth orientation revealed by X-ray diffraction remains always the (002). More significantly, Al-doping leads to a larger increase of the optical transmission and energy gap (E_g) of the metallic than of the ceramic target prepared films.     

Nitrogen incorporation into titanium diboride films deposited by dc magnetron sputtering: Structural modifications

This work reports a study of titanium boron nitride (Ti-B-N) films deposited at room temperature by dc magnetron sputtering using a TiB₂ target in different Ar-N₂ gas mixture atmospheres. The influence of the nitrogen partial pressure on the structural, mechanical and tribological properties of these films has been studied. The films were analyzed by Rutherford backscattering spectrometry in order to determine their chemical composition and atomic density. X-ray diffraction (XRD) was used to probe the film microstructure and X-ray photoelectron spectroscopy (XPS) for the chemical characterization of the film surface. An atomic force microscope (AFM) was used to analyze the surface topography and, when operating in the lateral force mode, for the friction characterization of the films. The XPS results showed that the surface of the films deposited in pure argon atmosphere was composed essentially by Ti and B oxides, while TiB₂, TiB, TiN and BN phases were present in the sputtered Ti-B-N films. Characterization by XRD determined the nanocrystalline nature of the films structure. While internal stress and friction increase upon the nitrogen incorporation, AFM measurements reveal a strong reduction of the surface roughness.     

BST/BZT/BST多层薄膜结构与性能研究

利用脉冲激光沉积法在LaNiO3/LaAlO3(001)基片上生长了Ba0.6Sr0.4TiO3(BST)和Ba(Zr0.2Ti0.8)O3(BZT)单层薄膜,以及Ba(Zr0.2Ti0.8)O3/Ba0.6Sr0.4TiO3/Ba(Zr0.2Ti0.8)O3(BZT/BST/BZT)多层薄膜.X射线衍射(XRD)分析发现,BST、BZT和LNO薄膜都具有高度的(00l)取向.原子力显微镜(AFM)显示三种样品表面光滑无裂纹,晶粒尺寸和表面粗糙度相当.电容测试表明,相对BST、BZT单层薄膜,多层薄膜具有最大的品质因数42.07.表明多层薄膜在微波应用中具有很大的潜力.     

Investigation of Pb-Mg-Nb-O pyrochlore thin films for tunable material

PMN thin films have been investigated as a feasible material for tunable microwave applications. PMN thin films were deposited by RF magnetron sputtering from Pb₆MgNb₆O₂₂ ceramic target on platinized Si substrates. The crystallinity, thickness, surface morphology, dielectric property, and voltage tunable properties of thin films were investigated by means of X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), and an impedance analyzer. The influences of sputtering substrate temperature and post-annealing on the tunable dielectric properties of thin films were investigated. Increasing the sputtering substrate temperature and annealing temperature can significantly increase tunability; however, these relations had the limitation that overly annealing temperature degraded the tunability of the thin film. A tunability of 38% at 1100 kV/cm of dc bias field under 1 MHz was achieved for a sample sputtered at 550 °C and annealed at 700 °C.     

Modulation of the structural and optical properties of sputtering-derived HfO2 films by deposition power

High-k gate dielectric HfO₂ thin films have been deposited on Si and quartz substrate by radio frequency magnetron sputtering. The structural and optical properties of HfO₂ thin films related to deposition power are investigated by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), ultraviolet–visible spectroscopy (UV–Vis), and spectroscopic ellipsometry (SE). Results confirmed by XRD have shown that the as-deposited HfO₂ thin films are not amorphous state but in monoclinic phase, regardless of deposition power. Analysis from FTIR indicates that an interfacial layer has been formed between the Si substrate and the HfO₂ thin film during deposition. AFM measurements illustrate that the root mean square (RMS) of the as-deposited HfO₂ thin films’ surface demonstrates an apparent reduction with the increase of deposition. Combined with UV–Vis and SE measurements, it can be noted reduction in band gap with an increase in power has been observed. Additionally, increase in refractive index (n) has been confirmed by SE.     

Deposition and characterization of reactive magnetron sputtered aluminum nitride thin films for film bulk acoustic wave resonator

This work studies the relationship between the deposition process parameters and the properties of sputtered c-axis-oriented aluminum nitride (AlN) thin films. AlN films were deposited on a Pt electrode by reactive magnetron sputtering under various deposition conditions. The films were characterized by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FESEM). A polycrystalline AlN film with highly c-axis-preferred orientation was achieved. The XRD rocking curve was 2.7°. The FESEM photographs also show that the AlN film has a dense hexagonal surface texture with uniform grain size and a highly ordered column structure.     

WO3 thin film prepared by PECVD technique and its gas sensing properties to NO2

Tungsten oxide films have been successfully fabricated from tungsten oxychloride (WOCl₄) precursor by using plasma enhanced vapor deposition (PECVD) technique. The films were deposited onto silicon substrates and ceramic tubes maintained at 100°C under a constant operating pressure of He-O₂ gas mixtures. The compositions and the structures of the thin films have been investigated by means of anaysis methods, such as XRD, XPS, UV and IR. The as-deposited WO₃ thin films were amorphous state and became crystalline after annealing above 400°C. The surface analysis of the films indicates that stoichiometry O/W is 2.77 : 1. The gas sensing measurements of the WO₃ thin film sensors indicate that these sensors have a high sensitivity, excellent selectivity and quick response behavior to NO₂.     

Annealing effects on the structural, electrical and H2 sensing properties of transparent ZnO thin films, grown by pulsed laser deposition

Transparent zinc oxide thin films were grown by reactive pulsed laser deposition on glass substrates. The substrates were kept at 200 °C constant temperature. Post-deposition heat treatment, applied to further promote crystallization and overcome any oxygen deficiency, yielded transparent thin films. Structural investigations carried out by atomic force microscopy (AFM) and X-ray diffraction (XRD), have shown a strong influence of deposition technique parameters and post-annealing on the crystallinity of the zinc oxide films. The gas sensing characteristics of these films were investigated towards different hydrogen concentrations (5000-30,000 ppm) at a selected operating temperature within the 150-230 °C range.     

Thin film deposition for permeability increase of gas being implanted (theoretical consideration)

A theoretical model has been developed for diffusive permeation of gas injected by ion bombardment through thin metallic targets, including membranes with thin films deposited onto the surface. The film material differs from the substrate material. Calculations for gas atom distribution in the film and substrate have been carried out, as well as gas fluxes to the source and sink sides in such a system in a quasi-stationary régime. The possibility of a permeability increase is revealed under implantation of gas ions both with low (～ keV) and higher energies (of the order of tens of keV) by deposition onto an irradiated target surface having a film of material with a lower diffusion coefficient for the gas being implanted than the substrate material itself. It has been shown that the most significant effect may be obtained under relatively high energy implantation for deposited film thicknesses markedly less than the mean ion range, and where the film permeability (diffusion coefficient and/or gas solubility) is much smaller than that of the substrate material itself. Periodic or simultaneous with implantation film renewal on the target surface has been suggested to compensate for sputtering.     

Effect of thickness on nanostructured SnO2 thin films by spray pyrolysis as highly sensitive H2S gas sensor

Nanostructured SnO2 thin films were prepared by spray pyrolysis technique onto glass substrates with different thickness by varying quantity of precursor solution. The structural, optical and electrical properties of these films have been studied. The crystallographic structure of the films was studied by X-ray diffraction (XRD). It is found that the films are tetragonal with (110) orientation. The grain size increases with thickness. Atomic Force Microscopy (AFM) showed that the nanocrystalline nature of the films with porous nature. The grain size increased 14 to 29 nm with increase in film thickness. The studies on the optical properties show that the direct band gap value decreases from 3.75 to 3.50 eV. The temperature dependence of the electrical conductivity was studied. The activation energies of the films are calculated from the conductance temperature characteristics. The nanostructured SnO2 thin films were used as sensing layers for resistive gas sensors. The dependence of gas sensing properties on the thickness of SnO2 thin films was investigated. The gas response of the SnO2 thin films towards the H2S gas was determined at an operating temperature of 150 degrees C. The sensitivity towards H2S gas is strongly depending on surface morphology of the SnO2 thin films.     

Atomic force microscopy and X-ray photoelectron spectroscopy evaluation of adhesion and nanostructure of thin Cr films

Chromium (Cr) thin films were deposited on float glass using electron beam (e-beam) physical vapor deposition and radio frequency (RF) magnetron sputtering techniques. Surface morphology of these Cr films was studied using atomic force microscopy (AFM). The e-beam deposited Cr films consisted of isolated surface mounds while in RF sputtered samples, these mounds combined to form larger islands. Lower surface adhesive properties were observed for e-beam deposited films, as determined from AFM force-distance curves, presumably due to the nanostructural differences. Similar amounts of adsorbed atmospheric carbonaceous contaminants and water vapor were detected on samples deposited using both methods with e-beam deposited samples having additional carbide species, as determined by X-ray photoelectron spectroscopy data. The dominant crystallographic plane in both e-beam deposited and RF sputtered Cr thin films was (110) of body-centered cubic Cr metal structure as determined from X-ray diffraction data. Weak (211) reflection was also observed in RF sputtered samples and was attributed to a different thin Cr film condensation and growth mechanism which resulted in nanostructural differences between films deposited using two different methods.     

快速热处理对(Ba,Sr)TiO3薄膜晶化行为的影响

采用射频溅射法在Si(111)基片上制备了(Ba,Sr)TiO3(BST)薄膜,并对制备的薄膜进行了快速退火热处理.采用X射线衍射和原子力显微镜分析了退火温度、退火时间和加热速度对BST薄膜晶化行为的影响.研究结果表明,BST薄膜的晶化行为强烈依赖于退火温度、退火时间和加热速度.BST薄膜的结晶度随退火温度的升高而提高.适当的热处理可降低BST薄膜的表面粗糙度,BST薄膜的表面粗糙度随退火温度的升高经历了一个先降低后增大的过程,但退火后BST薄膜的表面粗糙度都小于制备态薄膜的表面粗糙度.BST薄膜的晶粒尺寸随退火温度的升高经历了一个先增大后减小的过程.随退火时间的延长,BST薄膜的特征衍射峰越来越强,薄膜的晶化程度越来越高.随退火时问的延长,BST薄膜的晶粒尺寸和表面粗糙度也经历了一个先增大后减小的过程.BST薄膜的晶粒大小主要由退火温度决定.高的升温速率可获得较小的晶粒.     

硅衬底上高增透金刚石膜的制备研究

采用甲烷和氢气作为工作气体,在热丝化学气相沉积(HFCVD)设备上采用五段式沉积法制备了金刚石薄膜,用扫描电子显微镜(SEM)、激光拉曼光谱仪、X射线衍射仪(XRD)、原子力显微镜(AFM)以及傅立叶红外光谱仪研究了金刚石膜的结构和性质.结果表明,采用五段式沉积法可以得到晶粒大小达到纳米级的、表面粗糙度较小、金刚石纯度较高的金刚石膜,其最大增透率超过70%,能满足作为光学窗口增透膜的应用要求.     

Substrate dependent structural and magnetic properties of pulsed laser deposited Fe3O4 thin films

Nanocrystalline iron oxide thin films have been deposited on various substrates such as quartz, MgO(100), and Si(100) by pulsed laser deposition technique using excimer KrF laser (248 nm). The orientations, crystallite size and lattice parameters were studied using X-ray diffraction. The XRD results show that the films deposited on MgO and Si substrates are highly oriented and show only (400) and (311) reflections respectively. On the other hand, the orientation of the films deposited on quarts substrate changed from (311) to (400) with an increase in the substrate temperature from 400 degrees C to 600 degrees C, indicating thereby that the film growth direction is highly affected with nature of substrate and substrate temperature. The surface morphology of the deposited films was studied using Atomic Force Microscopy (AFM) and spherical ball like regular features of nanometer size grains were obtained. The magnetic properties were studied by Superconducting Quantum Interference Device (SQUID) magnetometer in the magnetic field +/- 6 Tesla. The magnetic field dependent magnetization (M-H) curves of all the Fe3O4 thin films measured at 5 K and 300 K show the ferrimagnetic nature. The electrochemical sensing of dopamine studied for these films shows that the film deposited on MgO substrate can be used as a sensing electrode.     

Preparation of crystalline TiC thin films grown by pulsed Nd:YAG laser deposition using Ti target in methane gas

Titanium carbide (TiC) thin films that are smooth and pinhole-free have been synthesized on Si(100) substrates by a pulsed neodymium:yttrium–aluminum–garnet (Nd:YAG) laser deposition method using titanium and TiC targets in methane gas. Glancing angle X-ray diffraction (GXRD) showed that polycrystalline films with components of TiC and Ti can be prepared using a Ti target. Single-phase TiC films can be synthesized using a TiC target. It was found that the methane gas pressure can control the crystallinity and composition. The root-mean-square (RMS) roughness of the film, as measured by an atomic force microscope (AFM), was lower than 2 nm in all the deposition areas. The film thickness, measured by α-step, was about 92 nm and the growth rate was approximately 3.1 nm/min. Measurements of optical emission spectra were performed to estimate the processing plasma state.     

Enhancement of the crystalline quality of reactively sputtered yttria-stabilized zirconia by oxidation of the metallic target surface

Yttria-stabilized zirconia (YSZ) thin films were fabricated on glass substrates by direct current magnetron reactive sputtering. We found out that the crystalline quality of the YSZ film was improved by an oxidation process of the metallic target surface prior to the sputtering deposition process. It is speculated that, at the initial stage of the sputtering, the sputtered particles from the oxidized target surface form a layer with higher degree of crystallization on the substrate, compared with those particles from the metallic target surface. This crystallized layer can enhance the crystallization of the film deposited subsequently. Other sputtering conditions such as sputtering pressure, oxygen flow rate, substrate temperature, and Y₂O₃ content in the film were investigated, for optimization of the crystalline quality of the deposited YSZ film.     

射频磁控反应溅射制备Al2O3薄膜的工艺研究

采用射频磁控反应溅射法,以高纯Al为靶材,高纯O2为反应气体,在不锈钢和单晶Si基片上成功地制备了氧化铝(Al2O3)薄膜,并对氧化铝薄膜的沉积速率、结构和表面形貌进行了研究.结果表明,沉积速率随着射频功率的增大先几乎呈线性增大而后缓慢增大;随着溅射气压的增加,沉积速率先增大,在一定气压时达到峰值后继续随气压增大而减小,同时随着靶基距的增大而减小;随着氧气流量的不断增加,靶面溅射的物质从金属态过渡到氧化物态,沉积速率也随之不断降低.X射线衍射图谱表明薄膜结构为非晶态;用原子力显微镜对薄膜表面形貌观察,薄膜微结构为柱状.     

Influence of deposition conditions on optical properties of aluminum nitride (AlN) thin films prepared by DC-reactive magnetron sputtering

Aluminum nitride (AlN) films have been prepared by DC-reactive magnetron sputtering technique. The optical properties of the films have been studied by optical spectroscopy with an incoherent light source. For the first time, it is demonstrated that for certain deposition conditions, the film may behave as a metallic thin film. In this case, there are strongly enhanced reflection peaks in the optical spectrum and the peaks may red-shift according to the degree of the metallization. The microscopic structures of the films have also been studied with scanning electron microscopy (SEM) and X-ray diffraction (XRD). It turns out that the orientation of the crystallites in the film determines whether the film remains dielectric or becomes metallic. It is found that the degree of the metallization depends on the proportion of (1000) preferred orientation in the film. In the deposition process, various deposition parameters have been experimented and a close relation between the deposition parameters and the status of the films is established. The most influential deposition conditions are as follows: the substrate temperature in a range from 200 to 700 °C, the gas composition ratio of Ar/N₂ from 20/80 to 60/40 and the plasma current from 0.2 to 0.45 A.     

On the characterization of Al-0.11 wt.%Sc alloy thin film

The characterizations (i.e., film adhesion, optical reflectivity, illumination aging and anti-corrosion behavior) should be considered for the metallic thin film served as a candidate of autolamp materials. The characterizations of three candidates (i.e., sputtered Al-0.11 wt.% Sc, sputtered pure Al, and thermally evaporated pure Al) have been investigated and compared. The sputtered Al-0.11 wt.% Sc film performed much better than any of the other two regarding the characterizations concerned. Examining through AFM, the sputtered Al-0.11 wt.% Sc revealed better surface property (including flatness and smoothness) than the others. Excellence in surface properties and optical reflectivity for the Al-0.11 wt.% Sc may arise from grain refinement in the film. Under long-term illumination, the films led to grain growth and hillocks formation. This illumination aging degraded the surface properties and optical reflectivity of the films, especially for the pure Al films. The sputtered Al-0.11wt.%Sc revealed more corrosion-resistance than the other films in 5% NaCl solution regardless whether or not under illumination aging.     

Growth of titanium dioxide films by cluster supersonic beams for VOC sensing applications

We developed and tested gas sensing devices based on TiO/sub 2/ nano-crystalline films produced at room temperature by the novel growth method of cluster beam deposition. The devices show a very good response to ethanol, methanol, and propanol and an overall performance comparable or better to the best devices reported in literature, based on films grown with other techniques. The major advantage of our growth method is that there is no need of the thermal annealing or doping processes usually required to improve sensitivity and reliability of gas sensing devices based on nanostructured thin film. The sensors dynamic response gives a maximum sensitivity for ethanol at about 250/spl deg/C. As the morphological (AFM) and structural (XRD) characterizations of the films show, the high performance of our sensors could only be achieved because their nano-crystalline structure was well controlled by the properties of the cluster precursors in the supersonic beam. We envisage possible further developments in terms of sensitivity and selectivity of gas sensing devices based on films grown by cluster beam deposition.