Microstructure evolution and mechanical properties of Ti-B-N coatings deposited by plasma-enhanced chemical vapor deposition

Ternary Ti-B-N coatings were synthesized on AISI 304 and Si wafer by plasma-enhanced chemical vapor deposition (PECVD) technique using a gaseous mixture of TiCl4,BCl3,H2,N2,and Ar.By virtue of X-ray diffraction analysis,X-ray photoelectron spectroscopy,scanning electron microscope,and high-resolution transmission electron microscope,the influences of B content on the microstructure and properties of Ti B N coatings were investigated systematically.The results indicated that the microstructure and mechanical properties of Ti-B-N coatings largely depend on the transformation from FCC-TiN phase to HCP-TiB2 phase.With increasing B content and decreasing N content in the coatings,the coating microstructure evolves gradually from FCC-TiN/a-BN to HCP-TiB2 /a-BN via FCC-TiN+HCP-TiB2/a-BN.The highest microhardness of about 34 GPa is achieved,which corresponds to the nanocomposite Ti-63%B-N (mole fraction) coating consisting of the HCP-TiB2 nano-crystallites and amorphous BN phase.The lowest friction-coefficient was observed for the nanocomposite Ti-41%B-N (mole fraction) coating consisting of the FCC-TiN nanocrystallites and amorphous BN

Microwave Plasma Chemical Vapor Deposition of Diamond Films on Silicon From Ethanol and Hydrogen

Diamond films with very smooth surface and good optical quality have been deposited onto silicon substrate using microwave plasma chemical vapor deposition (MPCVD) from a gas mixture of ethanol and hydrogen at a low substrate temperature of 450 ℃. The effects of the substrate temperature on the diamond nucleation and the morphology of the diamond film have been investigated and observed with scanning electron microscopy (SEM). The microstructure and the phase of the film have been characterized using Raman spectroscopy and X-ray diffraction (XRD). The diamond nucleation density significantly decreases with the increasing of the substrate temperature. There are only sparse nuclei when the substrate temperature is higher than 800 ℃ although the ethanol concentration in hydrogen is very high. That the characteristic diamond peak in the Raman spectrum of a diamond film prepared at a low substrate temperature of 450 ℃ extends into broadband indicates that the film is of nanophase. No graphite peak appeare

Nanocrystalline Diamond Films Grown by Microwave Plasma Chemical Vapor Deposition and Its Biocompatible Property

Due to its unique properties such as high hardness, light transmittance, thermal conductance, chemical stability and corrosion resistance, diamond has drawn tremendous attention in last two decades. These specific properties made diamond film a promising material for cutting tools, microwave windows, heat sinks for electronic devices and diamond electrodes. However, the diamond film with grain sizes at microscale usually exhibits high surface roughness and hinders its applications in the microelectro mechanical system (MEMS) and biological field because it is difficult to be polished by mechanical and chemical methods. With the development of the chemical vapor deposition, the nanocrystalline diamond (NCD) film has been fabricated and found new applications. The grain size of NCD film is in the range of 10 to 100 nm, which inherits the properties of the diamond and possesses the unique properties of the nanoscale materials, and the morphology of the NCD film is granular or needle-like structure. The microwave plasma chemical vapor deposition (MPCVD) has been regarded as the most promising method to deposit NCD film at low temperature. Compared to the hot filament CVD, MPCVD can grow high quality NCD film avoiding of the contamination from the filament materials. The MPCVD technique has high plasma density to activate carbonaceous compound and grow NCD film in high growth rate and low substrate temperature. The unique properties of NCD film, such as the superior electrical, mechanical and biological properties facilitate their application in various fields. The biological application, especially as a biocompatible coating, mainly includes the joint replacement implants and protective coatings and the ophthalmological prosthesis.

Growth of Aligned Carbon Nanotubes through Microwave Plasma Chemical Vapor Deposition

Aligned carbon nanotubes (CNTs) were synthesized on glass by microwave plasma chemical vapor deposition (MWPCVD) with a mixture of methane and hydrogen gases at the low temperature of 550 ℃. The experimental results show that both the self-bias potential and the density of the catalyst particles are responsible for the alignment of CNTs. When the catalyst particle density is high enough, strong interactions among the CNTs can inhibit CNTs from growing randomly and result in parallel alignment.

Preparation of Nano-Crystalline Diamond Films on Poly-Crystalline Diamond Thick Films by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond （NCD） films were prepared on poly-crystalline diamond （PCD） thick flims by the microwave plasma enhanced chemical vapor deposition （MPCVD） method. Free standing PCD thick film （50 mm in diameter） with a thickness of 413 μm was deposited in CHn/H2 plasma. It was then abraded for 2 hours and finally cut into pieces in a size of 10×10 mm^2 by pulse laser. NCD fihns were deposited on the thick film substrates by introducing a micro-crystalline diamond （MCD） interlayer. Results showed that a higher carbon concentration （5%） and a lower substrate temperature （650℃） were feasible to obtain a highly smooth interlayer, and the appropriate addition of oxygen （2%） into the gas mixture was conducive to obtaining a smooth nano-crystalline diamond film with a tiny grain size.

Two‑Dimensional Cr_(5)Te_(8)@Graphite Heterostructure for Efficient Electromagnetic Microwave Absorption

Two-dimensional(2D)transition metal chalcogenides(TMCs)hold great promise as novel microwave absorption materials owing to their interlayer interactions and unique magnetoelectric properties.However,overcoming the impedance mismatch at the low loading is still a challenge for TMCs due to the restricted loss pathways caused by their high-density characteristic.Here,an interface engineering based on the heterostructure of 2D Cr_(5)Te_(8) and graphite is in situ constructed via a one-step chemical vapor deposit to modulate impedance matching and introduce multiple attenuation mechanisms.Intriguingly,the Cr_(5)Te_(8)@EG(ECT)heterostructure exhibits a minimum reflection loss of up to−57.6 dB at 15.4 GHz with a thin thickness of only 1.4 mm under a low filling rate of 10%.The density functional theory calculations confirm that the splendid performance of ECT heterostructure primarily derives from charge redistribution at the abundant intimate interfaces,thereby reinforcing interfacial polarization loss.Furthermore,the ECT coating displays a remarkable radar cross section reduction of 31.9 dB m^(2),demonstrating a great radar microwave scattering ability.This work sheds light on the interfacial coupled stimulus response mechanism of TMC-based heterogeneous structures and provides a feasible strategy to manipulate high-quality TMCs for excellent microwave absorbers.

Effects of various substrate materials on structural and optical properties of amorphous silicon nitride thin films deposited by plasma-enhanced chemical vapor deposition

The plasma-enhanced chemical vapor deposition(PECVD)technique is well suited for fabricating optical filters with continuously variable refractive index profiles;however,it is not clear how the optical and structural properties of thin films differ when deposited on different substrates.Herein,silicon nitride films were deposited on silicon,fused silica,and glass substrates by PECVD,using silane and ammonia,to investigate the effects of the substrate used on the optical properties and structures of the films.All of the deposited films were amorphous.Further,the types and amounts of Si-centered tetrahedral Si–SivN4-v bonds formed were based upon the substrates used;Si–N4 bonds with higher elemental nitrogen content were formed on Si substrates,which lead to obtaining higher refractive indices,and the Si–SiN3 bonds were mainly formed on glass and fused silica substrates.The refractive indices of the films formed on the different substrates had a maximum difference of0.05(at 550 nm),the refractive index of SiNx films formed on silicon substrates was 1.83,and the refractive indices of films formed on glass were very close to those formed on fused silica.The deposition rates of these SiNx films are similar,and the extinction coefficients of all the films were lower than 10-4.

Synthesis of LiFePO_4 in situ vapor-grown carbon fiber (VGCF) composite cathode material via microwave pyrolysis chemical vapor deposition

One of the most important factors that limits the use of LiFePO 4 as cathode material for lithium ion batteries is its low electronic conductivity.In order to solve this problem,LiFePO 4 in situ vapor-grown carbon fiber (VGCF) composite cathode material has been prepared in a single step through microwave pyrolysis chemical vapor deposition.The phase,microstructure,and electrochemical performance of the composites were investigated.Compared with the cathodes without in situ VGCF,the initial discharge capacity of the composite electrode increases from 109 to 144 mA h g-1 at a 0.5-C rate,and the total electric resistance decreases from 538 to 66.The possible reasons for these effects are proposed.

Deposition and Boron Doping of Nano-Crystalline Diamond Thin Films on Poly-Crystalline Diamond Thick Films

Boron-doped nano-crystalline diamond （NCD） thin films have been successfully deposited on well-polished poly-crystalline diamond （PCD） thick films in a microwave plasma enhanced chemical vapor deposition （MPCVD） reactor for the first time. Different surface pretreatment techniques are carried out under different gas conditions （CH4, H2, Ar, and CH4/H2） to eliminate the effect of grain boundaries on the growth of a smooth NCD intrinsic layer. Well doped NCD films have been fabricated in CH4/H2/B2H6 plasma by varying the atomic ratio of B/C and the substrate temperature. Atomic force microscopy （AFM） results show that pretreatment in pure CH4 plasma at 1000℃ is most effective for NCD growth, while hydrogen containing plasma is harmful to the surface smoothness of NCD thin fihns. Doping research indicates that the optimum parameters for the boron-doping of high-quality NCD thin films are B/C=300 ppm （10-6） and 800℃.

Synthesis and Temperature-dependent Electrochemical Properties of Boron-doped Diamond Electrodes on Titanium

On the sand-blasting-treated titanium（Ti） substrate, the boron-doped diamond（BDD） electrodes with a wide potential window were prepared by microwave plasma chemical vapor deposition（MPCVD）. The electrochemi- cal oxidation ratios of phenol at BDD/Ti electrodes at elevated temperatures（from 20 ℃ to 80 ℃） were examined by the chemical oxygen demand（COD） of phenol electrolyte during electrolysis. The results show that the COD removal was increased at high temperatures and the optimized temperature for enhancing the electrochemical oxidation ratio of phenol is 60 ℃. The mechanism for the temperature-dependent electrochemical oxidation ratios of phenol at the electrodes was investigated. The study would be favorable for further improving the performance of BDD/Ti elec- trodes, especially working at high temperatures.

SiC基GaN上多晶金刚石散热膜生长及其影响

通过微波等离子体化学气相沉积(MPCVD)法,在SiC基GaN高电子迁移率晶体管(HEMT)异质结构材料上生长多晶金刚石散热膜,采用光学显微镜(OM)、拉曼光谱、非接触霍尔测试系统、X射线衍射(XRD)和扫描电子显微镜(SEM)对生长样品进行表征,研究了生长温度、多晶金刚石散热膜厚度对GaN HEMT异质结构材料性能的影响。测试结果表明,当多晶金刚石生长温度为625℃,散热膜厚度为20μm时,GaN材料载流子迁移率降低9.8%,载流子浓度上升5.3%,(002)衍射峰半高宽增加40%。生长温度越高,金刚石散热膜的生长速率越快。当金刚石散热膜厚度相差不大时,生长温度越高,GaN所受拉应力越大,材料电特性衰退越明显。多晶金刚石高温生长过程中,金刚石引入的应力未对GaN结构产生破坏作用,GaN材料中没有出现孔洞等缺陷。

Effect of trace oxygen on plasma nitriding of titanium foil

Titanium nitride films are prepared by plasma enhanced chemical vapor deposition method on titanium foil using N_(2) as precursor. In order to evaluate the effect of oxygen on the growth of titanium nitride films, a small amount of O_(2) is introduced into the preparation process. The study indicates that trace O_(2) addition into the reaction chamber gives rise to significant changes on the color and micro-morphology of the foil, featuring dense and long nano-wires. The as-synthesized nanostructures are characterized by various methods and identified as TiN, Ti_(2) N, and TiO_(2) respectively. Moreover, the experiment results show that oxide nanowire has a high degree of crystallinity and the nitrides present specific orientation relationships with the titanium matrix.

纳米金刚石膜/{100}晶面多晶金刚石膜台阶法快速生长研究

通过高功率微波等离子体化学气相沉积(MPCVD)以及台阶式基底排列方法,可以在一次沉积过程中同时沉积纳米晶粒及<100>取向的{100}面多晶金刚石薄膜。详细比较在同一次沉积中同时制备的多种不同类别的金刚石产物的生长速率。采用台阶法并添加少量空气,微波功率从2.0k W增加至3.2 kW,在下面大硅片上生长的纳米金刚石膜的平均生长速率可从0.3μm/h增大到3.0μm/h;而在上面小硅片上生长的纳米金刚石膜的平均生长速率从3.8μm/h也增加到11.2μm/h,同时产物也转变为{100}晶面的多晶膜。另外,在上面小硅片上生长的金刚石膜的边角效应明显,在边界生长的金刚石产物的生长速率更高,从17.0μm/h增大到27.1μm/h。该结果表明少量氮气和氧气同时添加对金刚石生长的形貌多样性调节作用和对生长速率的提升作用强烈依赖于生长条件。

SUBSTRATE EFFECT ON HYDROGENATED MICROCRYSTALLINE SILICON FILMS DEPOSITED WITH VHF-PECVD TECHNIQUE

Raman spectra and scanning electron microscope （SEM） techniques were used to determine the structural properties of microcrb＇stalline silicon （μc-Si：H） films deposited on different substrates with the very high frequency plasma-enhanced chemical vapor deposition （VHF-PECVD） technique. Using the Raman spectra, the values of crystalline volume fraction Xc and average grain size d are 86%, 12.3nm; 65%, 5.45nm; and 38%, 4.05nm, for single crystalline silicon wafer, coming 7059 glass, and general optical glass substrates, respectively. The SEM images further demonstrate the substrate effect on the film surface roughness. For the single crystalline silicon wafer and Coming 7059 glass, the surfaces of the μc-Si：H films are fairly smooth because of the homogenous growth or h＇ttle lattice mismatch. But for general optical glass, the surface of the μ-Si： H film is very rough, thus the growing surface roughness affects the crystallization process and determines the average grain size of the deposited material. Moreover, with the measurements of thickness, photo and dark conductivity, photosensitivity and activation energy, the substrate effect on the deposition rate, optical and electrical properties of the μc-Si：H thin films have also been investigated. On the basis of the above results, it can be concluded that the substrates affect the initial growing layers acting as a seed for the formation of a crystalline-like material and then the deposition rates, optical and electrical properties are also strongly influenced, hence, deposition parameter optimization is the key method that can be used to obtain a good initial growing layer, to realize the deposition of μc-Si：H films with device-grade quality on cheap substrates such as general glass.

多晶金刚石对硅基氮化镓材料的影响

氮化镓(GaN)器件的自热问题是目前限制其性能的关键因素,在GaN材料上直接生长多晶金刚石改善器件的自热问题成为研究的热点,多晶金刚石距离GaN器件工作有源区近,散热效率高,但多晶金刚石和GaN材料热失配可能会导致GaN电特性衰退.本文采用微波等离子体化学气相沉积法,在2 in (1 in=2.54 cm)Si基GaN材料上生长多晶金刚石.测试结果显示,多晶金刚石整体均匀一致,生长金刚石厚度为9—81 μm,随着多晶金刚石厚度的增大, GaN (002)衍射峰半高宽增量和电性能衰退逐渐增大.通过激光切割和酸法腐蚀,将Si基GaN材料从多晶金刚石上完整地剥离下来.测试结果表明:金刚石高温生长过程中,氢原子对氮化硅外延层缺陷位置有刻蚀作用形成孔洞区域,刻蚀深度可达本征GaN层;在降温过程,孔洞周围形成裂纹区域.剥离下来的Si基GaN材料拉曼特征峰峰位, XRD的(002)衍射峰半高宽以及电性能均恢复到本征状态,说明多晶金刚石与Si基GaN热失配产生应力,引起GaN晶格畸变,导致GaN材料电特性衰退,这种变化具有可恢复性,而非破坏性.

MPCVD制备金刚石的研究

金刚石在材料家族中是集力、光、电、声、热、磁于一身的最优秀的材料。它不仅在工程领域中得到了广泛应用,而且在功能应用中也是大有作为的材料。因此,吸引着国内外广大科技工作者对其进行研发的极大欲望。文章简要地介绍了多晶金刚石薄膜、大尺寸单晶金刚石(Single Crystal Diamond—SCD)合成过程中的腔体压强大小、基体温度的高低、衬底材质与表面粗糙度等工艺参数以及饰钻培育的形核、生长质量等技术问题的研究结果。通过实践分析得到了高温形核-低温生长的梯度规律和腔体内压强和基体温度低或过高都不利于生长出高质量金刚石薄膜的规律。

微波等离子体化学气相沉积法制备大尺寸单晶金刚石的研究进展

金刚石作为一种超宽禁带半导体,是下一代功率电子器件和光电子器件最有潜力的材料之一。然而,高品质、大面积(大于2英寸)单晶衬底的制备仍是金刚石器件产业应用亟待解决的问题。介绍了目前受到广泛关注的微波等离子体化学气相沉积法(MPCVD)获得大尺寸金刚石单晶衬底的技术方案,即单颗金刚石生长、拼接生长以及异质外延生长。综述了大尺寸单晶金刚石外延生长及其在电子器件领域应用的研究进展。总结了大尺寸单晶金刚石制备过程中面临的挑战并提出了潜在的解决方案。

MPCVD高功率外延生长单晶金刚石均匀性研究

目的 为了优化单晶金刚石大批量生长的等离子体环境,开展了高功率微波等离子体环境对单晶金刚石外延生长研究。方法 利用实验室自主研发的915 MHz-MPCVD装置,在15~37 kW的高功率微波馈入的条件下,研究了在高功率微波等离子体环境中CVD单晶金刚石的均匀生长条件,利用光学显微镜及激光拉曼光谱对所生长的单晶金刚石进行了形貌质量表征,利用等离子体发射光谱对高功率微波等离子体环境进行了诊断。结果 在保持甲烷体积分数为5%时,当微波功率为15k W时,等离子体球的尺寸较小,并不能完全覆盖直径150 mm的基片台;将微波功率从28 kW提高到37 kW,肉眼所见的等离子体尺寸变化并不明显,但等离子体的能量分布范围有一定的扩大,这意味着在一定的范围内活性基团的能量分布更均匀。在较高的微波功率下,分布于基片台不同区域的单晶金刚石片均能获得较好的层状生长台阶。随着微波功率的提高以及基片温度的增加,分布于基片台不同区域的微波电磁场强度都有所增强,提高了单晶金刚石的生长速率和质量。结论 在高功率等离子体环境中,通过大幅度的提高微波功率,可以有效地活化含碳基团,在等离子体中产生有利于单晶金刚石高质量高速生长的活性基团。在微波功率为37k W、甲烷体积分数为5%的情况下,将基片温度控制在950℃附近,可以有效地抑制多晶杂质的生成,实现了57片单晶金刚石的批量生长。

单晶金刚石异质外延用铱复合衬底研究现状

金刚石优异的物理性质使其成为下一代最有发展潜力的半导体材料之一。目前来看,基于微波等离子体化学气相沉积的异质外延可能是未来制备大尺寸单晶金刚石的最佳方法。在过去的三十年间,铱复合衬底上异质外延生长单晶金刚石取得了一定进展,特别是近几年实现了2英寸(1英寸=2.54 cm)以上的大尺寸自支撑单晶金刚石的生长。本文总结了金刚石异质外延用的衬底,简要介绍了异质衬底上的偏压增强成核,详细介绍了目前最成功的铱/氧化物、铱/氧化物层/硅复合衬底,最后对金刚石异质衬底和异质外延进行了总结,指出目前存在的问题并给出了一些可能的解决思路。

利用发射光谱探究CO_(2)对MPCVD法生长单晶金刚石质量的影响

等离子体发射光谱作为一种非侵入性等离子体诊断手段能有效探测等离子体内部基团的变化信息,对这些信息的分析可以反映等离子体的特性,从而有助于探究影响单晶金刚石生长结果的原因和机理。CO_(2)是一种比O2更安全的气体,近年来在源气体引入CO_(2)生长高质量单晶金刚石的研究日渐增多。本文利用微波等离子体化学气相沉积法在4.2 kW的微波功率下进行单晶金刚石同质外延生长实验,对生长过程中的CH_(4)/H_(2)/CO_(2)等离子体进行了发射光谱诊断,最后结合光谱信息和拉曼光谱表征研究了CO_(2)体积分数对单晶金刚石生长质量的影响,结果发现CO_(2)浓度增加对C_(2)和CH基团强度抑制作用明显,对C_(2)抑制作用最强,这也是导致生长速率下降的主要原因。I(CH)/I(Hα)比值略有增加,说明CO_(2)增加对金刚石前驱物的沉积有促进作用,这在一定程度上减弱了对生长速率的不利影响。拉曼表征结果说明0~5%CO_(2)浓度下的单晶金刚石质量随CO_(2)浓度上升变好,且浓度为5%时,1420 cm−1杂质峰基本消失。