蓝宝石衬底上生长的Ga2+xO3-x薄膜的结构分析

利用卢瑟夫背散射/沟道技术和金属有机化学气相沉积方法, 对蓝宝石衬底上 在不同温度、压强下生长的Ga_2+xO_3-x薄膜进行结构和结晶品质的测量与分析; 并结合高分辨X射线衍射分析技术, 通过对其对称(402)面的θ–2θ及ω扫描, 确定了其结构类型及结晶品质. 实验表明: 在相同的生长温度(500 ℃)下, 结晶品质随压强的下降而变好, 生长压强为15 Torr (1 Torr=133.322 Pa)的样品其结晶品质最好, 沿轴入射之比χ_min值为14.5%; 在相同的生长压强(15 Torr)下, 结晶品质受生长温度的影响不大, 所以, 生长温度不是改变结晶品质的主要因素; 此外, 在相同的生长条件下制备的样品, 分别经过700, 800和900 ℃退火后, 其结晶品质随退火温度的变化而变化. 退火温度为800 ℃的样品的结晶品质最好, χ_min值为11.1%; 当退火温度达到900 ℃时, 样品部分分解; 经热处理的样品其X射线衍射谱中有一个强的Ga₂O₃ (402)面衍射峰, 其半峰全宽为0.5°, 表明该Ga₂O₃外延膜是(402)择优取向. 关键词： 氧化镓 卢瑟夫背散射 X射线衍射 结晶品质     

沉积工艺条件对金刚石薄膜红外椭偏光学性质的影响

采用红外椭圆偏振光谱仪对不同工艺条件下制备的CVD金刚石薄膜在红外波长范围内的光学参量进行了测量，分析了工艺条件对金刚石薄膜红外光学性质的影响.获得了最佳的沉积工艺参数，优化了薄膜的制备工艺.结果表明薄膜的折射率和消光系数与薄膜质量密切相关，当温度为750℃，碳源浓度为0.9%和压强为4.0 kPa时，金刚石薄膜的红外椭偏光学性质最佳，折射率平均值为2.385，消光系数在10^-4范围内，在红外波段具有良好的透过性. 关键词： 薄膜光学 红外光学性质 工艺条件 金刚石薄膜     

环境气体对激光诱导Al等离子体光谱的影响

调QNd:YAG脉冲激光(波长1.06μm,脉冲宽度10ns,能量42mj/pulse)烧蚀平面Al靶,在垂直靶面方向,利用光学多道分析系统(OMA),测量了激光诱导产生的等离子体发射光谱分别在环境气体为Air,N2和Ar,气压范围分别在10-2Torr,152Torr,304Torr,532Torr和760Torr下的空间分布。实验表明,随着环境气体压强的增大,光谱的空间分布被压缩,且谱线强度的峰值向靶面方向移动;在相同的气压下,Ar环境下产生的光谱强度明显大于在Air和N2环境下产生的光谱强度;在气压为152Torr的不同环境气体下,均发现光谱在离靶面很近的地方(约0.5mm～1.0mm)减小,甚至消失;在Ar环境气体下,谱线396.1nmAlⅠ的空间分布随着与靶面距离的增大,谱线位置向短波方向有约0.03nm(对应OMA探头的一个二极管阵列)的移动,而谱线394.4nmAlⅠ的移动不太明显。     

氦气对MPCVD沉积金刚石的影响

为了确定添加氦气对微波等离子体化学气相沉积(MPCVD)金刚石膜的影响,采用发射光谱法(OES)在线诊断了CH₄-H₂-He等离子体的发射光谱特性,研究了He对等离子体内基团空间分布的影响;并利用扫描电子显微镜(SEM)和拉曼(Raman)光谱对不同He体积分数下沉积出的金刚石膜进行了表征。结果表明：随着He体积分数的增加,等离子体内H_α, H_β, H_γ, CH和C₂基团的谱线强度均呈上升趋势,其中H_α基团的谱线强度增加最大。光谱空间诊断发现He的加入导致等离子体中各基团的空间分布均匀性变差,造成沉积出的金刚石膜厚度极不均匀。沉积速率测试表明,He的加入导致碳源基团相对浓度增加,有利于提高薄膜的沉积速率,当He体积分数由0 vol.%增加至4.7 vol.%时,沉积速率提高了24%。SEM测试结果表明,随着He体积分数的增加,金刚石膜表面形貌由(111)晶面取向向晶面取向混杂转变,孪晶生长明显。高He(4.7 vol.%)体积分数下由于C₂基团的相对浓度较高,导致二次形核密度增加。此外,由于基片台受到等离子体的刻蚀和溅射作用,导致薄膜沉积过程中引入了金属杂质原子。二次形核和杂质原子的存在使得孪晶大量的产生,薄膜呈现出压应力。     

掺杂CVD金刚石薄膜的应力分析

在不同实验条件下，用微波等离子体化学气相沉积(MPCVD)技术在Si基体上制备了S掺杂和B-S共掺杂CVD金刚石薄膜，利用X射线衍射仪和拉曼光谱仪研究掺杂对CVD金刚石薄膜的应力影响.研究结果发现，随着S掺杂浓度的增加，薄膜中sp²杂化碳含量和缺陷增多，CVD金刚石薄膜压应力增加；小尺寸的B原子与大尺寸的S原子共掺杂时，微量B的加入改变了CVD金刚石薄膜的应力状态，共掺杂形成B-S复合体进入金刚石晶体后降低金刚石晶体的晶格畸变程度，减少S原子在晶界上偏聚数量和晶体中非金刚石结构相含量，降低由于杂质、缺陷及sp²杂化碳含量产生的晶格畸变和薄膜压应力，提高晶格完整性. 关键词： 金刚石薄膜 掺杂 应力     

等离子体活化硒对电沉积Cu-In-Ga金属预制层硒化的影响

使用等离子体活化硒源对电沉积制备的Cu-In-Ga金属预制层进行了硒化处理时, 发现等离子体功率对Cu(In_1-xGa_x)Se₂(CIGS)晶粒的生长有重要影响, 当等离子体功率为75 W时, 制备出单一Cu(In_0.7Ga_0.3)Se₂相的CIGS薄膜. 通过对不同衬底温度的等离子体活化硒源硒化的CIGS 薄膜进行了研究与分析, 并与普通硒化后的薄膜进行对比, 发现高活性硒在低温下会促进Ga-Se二元相的生成, 从而有利于Cu(In_0.7Ga_0.3)Se₂单相的生长. 对等离子体硒化后的CIGS薄膜进行了电池制备, 发现单相CIGS薄膜没有显著提高电池性能. 通过优化工艺, 所制备的CIGS电池效率达到了9.4%. 关键词： 0.7Ga_0.3)Se₂')" href="#">Cu(In_0.7Ga_0.3)Se₂ 电沉积 Cu-In-Ga金属预制层 等离子体活化硒     

石英衬底上生长的高光学质量的纳米金刚石薄膜

采用射频等离子体增强的热丝化学气相沉积(RFHFCVD)技术在石英玻璃衬底上制备了表面光滑、晶粒致密均匀的纳米金刚石薄膜.用扫描电子显微镜(SEM)和台阶仪观测薄膜的表面形貌和粗糙度,x射线衍射(XRD)和Raman光谱表征膜层的结构,并用紫外可见近红外光谱仪测量其光透过率.实验结果表明,衬底温度、反应气压及射频功率对金刚石膜的结晶习性、表面粗糙度及光透过率均有很大程度的影响,其最佳值分别为700℃,2×133Pa和200W.在该最佳参量下经1h的生长即获得连续、平滑的纳米金刚石膜,其平均晶粒尺寸为约25 关键词： 纳米金刚石薄膜 射频等离子体增强热丝化学气相沉积 光透过率     

金刚石薄膜的红外椭圆偏振光谱研究

采用红外椭圆偏振光谱对微波等离子体化学气相沉积法（MPCVD）和热丝化学气相沉积法（H-FCVD）制备的金刚石薄膜在红外波长范围（2.5—12.5μm）的光学参数进行了测量.建立了不同的光学模型，且在模型中采用Bruggeman有效介质近似方法综合考虑了薄膜表面和界面的椭偏效应.结果表明，MPCVD金刚石膜的椭偏数据在模型引入了厚度为77.5nm的硅表面氧化层、HFCVD金刚石膜引入879nm粗糙层之后能得到很好的拟合.最后对两种模型下金刚石薄膜的折射率和消光系数进行了计算，表明MPCVD金刚石薄膜的红外 关键词： 金刚石薄膜 红外椭圆偏振光谱 光学参数 有效介质近似     

含氮氟化类金刚石(FN-DLC)薄膜的研究：(Ⅰ) sp结构与化学键分析

以CF₄，CH₄和N₂为源气体，利用射频等离子体增强化学气相沉积法，在不同功率下制备了含氮氟化类金刚石膜.用俄歇电子能谱、拉曼光谱、X射线光电子能谱和傅里叶变换红外光谱对薄膜的电子结构和化学键进行了表征，并结合高斯分峰拟合方法分析了薄膜中sp²，sp³结构比率.结果表明，制备的薄膜属于类金刚石结构，不同沉积功率下，薄膜内的sp²/sp³值在2.0—9.0之间，随着沉积功率的增加薄膜内sp²的相对含量增加.膜内主要有C—F_x(x=1，2)，C—C，C=C和C≡N等化学键.沉积功率增加，C—C基团增加，膜内F的浓度降低，C—F基团减少，薄膜的关联加强，稳定性提高. 关键词： 含氮氟化类金刚石膜 sp结构 化学键结构 射频功率     

高气压MPCVD沉积金刚石的光谱研究

采用微波等离子体化学气相沉积方法(microwave plasma chemical vapor deposition, MPCVD)在高沉积气压(34.5 kPa)下制备多晶金刚石,利用发射光谱(optical emission spectroscopy, OES)在线诊断了CH₄/H₂/O₂等离子体内基团的谱线强度及其空间分布,并利用拉曼(Raman)光谱评价了不同O₂体积分数下沉积出的金刚石膜质量,研究了金刚石膜质量的均匀性分布问题。结果表明：随着O₂体积分数的增加,C₂, CH及H_α基团的谱线强度均呈下降的趋势,而C₂,CH与H_α谱线强度比值也随之下降,表明增加O₂体积分数不仅导致等离子体中碳源基团的绝对浓度下降,而且碳源基团相对于氢原子的相对浓度也降低,使得金刚石的沉积速率下降而沉积质量提高。此外,具有刻蚀作用的OH基团的谱线强度却随着O₂体积分数的增加而上升,这也有利于降低金刚石膜中非晶碳的含量。光谱空间诊断发现高沉积气压下等离子体内基团分布不均匀,特别是中心区域C₂基团聚集造成该区域内非晶碳含量增加,最终导致金刚石膜质量分布的不均匀。     

Microstructure, chemical bonds, and friction properties of nanocrystalline diamond films deposited in two different plasma media

Nanocrystalline diamond films with the properties dependent on the composition of the gaseous medium have been prepared using the microwave plasma enhanced chemical vapor deposition (MPECVD) method. A nanocrystalline film formed in the Ar/CH₄ plasma is characterized by a high crystallinity factor, a small grain size, a large fraction of sp ²-amorphous carbon, and, consequently, by an increase in the hardness and elastic modulus. The low value of the friction coefficient of this film is associated with the small grain size and large fraction of the sp ²-amorphous carbon boundary phase that ensures an easy sliding. The contact angle of the film is small (hydrophilic properties) in the case when the plasma consists of an Ar/CH₄ mixture. It has been shown that the wetting properties of the films are provided by a thin layer of carboxyl and hydroxyl functional groups passivating the dangling bonds at the surface that are responsible for the boundary lubrication mechanism. It has also been found that the friction coefficient of these films is inversely proportional to the contact pressure dependent on the diameter of the sliding counterbody ball.     

Differing morphologies of textured diamond films with electrical properties made with microwave plasma chemical vapor deposition

This study investigates the orientation of textured diamond films produced through microwave plasma chemical vapor deposition (MPCVD) at 1200 W, 110 Torr, CH₄/H₂ = 1/20, with depositions times of 0.5-4.0 h. After a growth period of 2.0-4.0 h, this particular morphology revealed a rectangular structure stacked regularly on the diamond film. The orientation on {1 1 1}-textured diamond films grew a preferred orientation of {1 1 0} on the surface, as measured by XRD. The formation of the diamond epitaxial film formed textured octahedrons in ball shaped (or cauliflower-like) diamonds in the early stages (0.5 h), and the surface of the diamond film extended to pile the rectangular structure at 4.0 h. The width of the tier was approximately 200 nm at the 3.0 h point of deposition, according to TEM images. The results revealed that the textured diamond films showed two different morphological structures (typical ball shaped and rectangular diamonds), at different stages of the deposition period. The I-V characteristics of the oriented diamond films after 4.0 h of deposition time showed good conformity with the ohmic contact.     

Effects of N2 addition on nanocrystalline diamond films by HFCVD in Ar/CH4 gas mixture

Nanocrystalline diamond (NCD) films were grown on silicon substrates by hot filament chemical vapor deposition in Ar/N₂/CH₄ gas mixtures. The effects of seeding process prior to deposition, the total gas pressure, and concentration of nitrogen on the grain size, morphology and bonding nature in HFCVD technique were investigated. The results indicated that a low total gas pressure is favorable for nanosized diamond crystallites. Films micrograph obtained from scanning electron microscopy showed diamond nanograins elongated with the addition of nitrogen in the plasma. Crystal structure investigations were carried out by X-ray diffraction measurements for deposited films. An increase in the size of crystallite is also observed from XRD measurements in NCD film when nitrogen was added in plasma. From Raman spectra, it was observed that the relative intensity of G peak increases indicating more graphite content after nitrogen added in the plasma. The effects of the nitrogen incorporation in nanocrystalline films in HFCVD are discussed.     

Influence of boron carbide on properties of CVD-diamond thin films at various deposition pressures

Microcrystalline boron-doped diamond (BDD) films are synthesized on the silicon substrate by the hot-filament chemical vapor deposition method under the gas mixture of hydrogen and methane in the presence of boron carbide (B₄C) placed in front of filaments. The observed results of scanning electron microscopy, Raman spectroscopy and X-ray diffraction show the morphologies. Microstructures for various deposition pressures of as-grown diamond films are found to be dependent on the change of deposition pressure. These results reveal that with the increase of deposition pressure, resistivity decreases and increase in the grain size is noted in the presence of B₄C. Resistivity shows a sudden fall of about three orders of magnitude by the addition of boron in the diamond films. This is due to the crystal integrity induced by B-atoms in the structure of diamond in the presence of B₄C. These results are also significant for the conventional applications of BDD materials. The effects of deposition pressure on the overall films morphology and the doping level dependence of the diamond films have also been discussed.     

OES study of the gas phase during diamond films deposition in high power DC arc plasma jet CVD system

This paper used optical emission spectroscopy (OES) to study the gas phase in high power DC arc plasma jet chemical vapour deposition (CVD) during diamond films growth processes. The results show that all the deposition parameters (methane concentration, substrate temperature, gas flow rate and ratio of H₂/Ar) could strongly influence the gas phase. C₂ is found to be the most sensitive radical to deposition parameters among the radicals in gas phase. Spatially resolved OES implies that a relative high concentration of atomic H exists near the substrate surface, which is beneficial for diamond film growth. The relatively high concentrations of C₂ and CH are correlated with high deposition rate of diamond. In our high deposition rate system, C₂ is presumed to be the main growth radical, and CH is also believed to contribute the diamond deposition.     

Optimization of plasma parameters for high rate deposition of titanium nitride films as protective coating on bell-metal by reactive sputtering in cylindrical magnetron device

Nano-structured titanium nitride (TiN) thin film coating is deposited by reactive sputtering in cylindrical magnetron device in argon and nitrogen gas mixtures at low temperature. This method of deposition using DC cylindrical magnetron configuration provides high uniform yield of film coating over large substrate area of different shapes desirous for various technological applications. The influence of nitrogen gas on the properties of TiN thin film as suitable surface protective coating on bell-metal has been studied. Structural morphological study of the deposited thin film carried out by employing X-ray diffraction exhibits a strong (2 0 0) lattice texture corresponding to TiN in single phase. The surface morphology of the film coating is studied using scanning electron microscope and atomic force microscope techniques. The optimized condition for the deposition of good quality TiN film coating is found to be at Ar:N₂ gas partial pressure ratio of 1:1. This coating of TiN serves a dual purpose of providing an anti-corrosive and hard protective layer over the bell-metal surface which is used for various commercial applications. The TiN film's radiant golden colour at proper deposition condition makes it a very suitable candidate for decorative applications.     

Synthesis of micro- or nano-crystalline diamond films on WC-Co substrates with various pretreatments by hot filament chemical vapor deposition

Diamond films deposited on tungsten carbide can lead to major improvements in the life and performance of cutting tools. However, deposition of diamond onto cemented tungsten carbide (WC-Co) is problematic due to the cobalt binder in the WC. This binder provides additional toughness to the tool but results in poor adhesion and low nucleation density of any diamond film. A two-step chemical etching pretreatment (Murakami reagent and Caro acid, (MC)-pretreatment) and a boronization pretreatment have both been used extensively to improve adhesion of CVD diamond film on WC-Co substrates. Here we discuss the applicability of MC-pretreatment for a range of Co-containing WC-Co substrates, and demonstrate a controlled synthesis process based on liquid boronizing pretreatment for obtaining smooth and dense micro- or nano-crystalline diamond films on high Co-containing WC-Co substrates. Substrate treatments and deposition parameters were found to have major influences on the smoothness, structure and quality of the diamond films. The best quality diamond films were achieved under conditions of relatively high substrate temperature (T_s) and the best adhesion was achieved at T_s = 800 °C.     

Influences of Process Parameters on 111-Oriented CVD Diamond Film Growth Under Two-Step Method

The growth of 111-oriented CVD diamond film under a two-step model was simulated at atomic scale by using revised KMC method. The simulation was conducted at various substrate temperatures (1100 K-1400 K) and CH3 radical concentration (0.01 that: (1) The 111-oriented CVD diamond film growth under the two-step model is superior to that under corresponding single-step model, which is in good agreement with the experimental results. (2) Substrate temperature (T _s) and the concentration of CH₃ ([CH₃]) can produce important effects on the film deposition rate, surface roughness and the concentration of atom H embedded in the film. However, both the T _s and [H] should be controlled to a proper range for high quality films.     

Two-dimensional model of a large area, inductively coupled,rectangular plasma source for chemical vapor deposition

A novel design for an inductively coupled, rectangular plasma source is described. The design encompasses several key issues of large area thin film growth by chemical vapor deposition: structural integrity, electrostatic screening, substrate temperature control and maximal growth surface. A test reactor has been utilized to grow diamond films over ~1800 cm² at 13 MHz and ~1 torr pressure with 45 kW coupled power. The design is readily scalable to larger areas. To analyze the axial plasma uniformity, a two-dimensional (2-D) simulation model is presented. The electromagnetic coupling, nonequilibrium plasma chemistry and multispecies diffusion are self-consistently treated. In this 2-D approach, the slotted Faraday screen behaves as a diamagnetic medium in transmitting the magnetic field. Results are compared with experimental data for the hydrogen plasma extent, electron and gas temperatures. Neutral gas thermal conduction and hydrogen recombination dominate the energy deposition to the wall and in turn govern the plasma length. A tradeoff between quality and growth area is predicted for the reactor as the pressure is decreased