Edge effect during microwave plasma chemical vapor deposition diamond-film:Multiphysics simulation and experimental verification

This study focused on the investigation of the edge effect of diamond films deposited by microwave plasma chemical vapor de-position.Substrate bulge height△h is a factor that affects the edge effect,and it was used to simulate plasma and guide the diamond-film deposition experiments.Finite-element software COMSOL Multiphysics was used to construct a multiphysics(electromagnetic,plasma,and fluid heat transfer fields)coupling model based on electron collision reaction.Raman spectroscopy and scanning electron microscopy were performed to characterize the experimental growth and validate the model.The simulation results reflected the experimental trends observed.Plasma discharge at the edge of the substrate accelerated due to the increase in△h(△h=0-3 mm),and the values of electron density(n_(c)),molar concentration of H(C_(H)),and molar concentration of CH_(3)(C_(CH_(3)))doubled at the edge(for the special concave sample with△h=−1 mm,the active chemical groups exhibited a decreased molar concentration at the edge of the substrate).At=0-3 mm,a high diamond growth rate and a large diamond grain size were observed at the edge of the substrate,and their values increased with.The uniformity of film thickness decreased with.The Raman spectra of all samples revealed the first-order characteristic peak of dia-mond near 1332 cm^(−1).When△h=−1 mm,tensile stress occurred in all regions of the film.When△h=1-3 mm,all areas in the film ex-hibited compressive stress.

SYNTHESIS OF PPCuPc FILM BY MICROWAVE PLASMA CHEMICAL VAPORIZATION DEPOSITION(MPCVD)

Using a low power microwave generator(W_(max)=100W) and a Surfatron discharge device, Plasma-polymerized copper phthalocyanine (PPCuPc) film was synthesised from monomer copper phthalocyanine(CuPc) by microwave plasma chemical vaporization deposition(MPCVD) with Ar as incorporation gas. The film was characterized by FTIR and ESCA. The role of dissociation of chemical bond in the polymerization process and the influence of substrate temperature and material on deposition were investigated in some detail.

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 appeared in the XRD pattern confirms that the film is mainly composed of SP3 carbon. The diamond peak in the XRD pattern also broadens due to the nanocrystalline of the film.

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

Fabrication and characterization of iron and iron carbide thin films by plasma enhanced pulsed chemical vapor deposition

A new pulsed chemical vapor deposition（PCVD） process has been developed to fabricate iron（Fe） and iron carbide(Fe1-xCx) thin films at low temperature range from 150 ℃ to 230 ℃.The process employs bis（1,4-di-tert-butyl-1,3-diazabutadienyl）iron（Ⅱ） as iron source and hydrogen gas or hydrogen plasma as the coreactant.The films deposited with hydrogen gas are demonstrated polycrystalline with body-centered cubic Fe.However,for the films deposited with hydrogen plasma,the amorphous phase of iron carbide is obtained.The influence of the deposition temperature on iron and iron carbide characteristics have been investigated.

Effective parameters on diameter of carbon nanotubes by plasma enhanced chemical vapor deposition

The effective parameters on the diameter of carbon nanotubes (CNTs) by plasma enhanced chemical vapor deposition (PECVD) were presented.Among lots of influential parameters,the effects of the catalytic film thickness and the pretreatment plasma power on the growth of CNTs were investigated.The results show that the size of catalytic islands increases by increasing the thickness of catalytic layer,but the density of CNTs decreases.The pretreatment duration time of 30 s is the optimal condition for growing CNTs with about 50 nm in diameter.By increasing the pretreatment plasma power,the diameter of CNTs decreases gradually.However,the diameter of CNTs does not change drastically from 80 to 120 W.The uniformly grown CNTs with the diameter of 50 nm are obtained at the pretreatment plasma power of 100 W.

Characterization of Crystalline Nanoparticles/Nanorods Synthesized by Atmospheric Plasma Enhanced Chemical Vapor Deposition of Perfluorohexane

A mass of nanoparticles/nanorods were formed on a simultaneously deposited gran- ular film by plasma enhanced chemical vapor deposition （PECVD） of perfluorohexane at atmo- spheric pressure without any catalysts or templates. Scanning electron microscopy （SEM） and X-ray photoelectron spectroscopy （XPS） were used to characterize the morphology and the chem- ical compositions of nanoparticles. The average size of particles is about 100 nm and the length of synthesized nanorods is between 1 μm and 2.5/tm. The analyses of transmission electron microscopy （TEM）, high-resolution transmission electron microscopy （HRTEM）, selected area electron diffraction（SAED） and X-ray diffraction （XRD） reveals that the nanoparticles and nanorods are crystalline.

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.

Characteristics and Electrical Properties of SiNx:H Films Fabricated by Plasma-Enhanced Chemical Vapor Deposition

SiNx：H films with different N/Si ratios are synthesized by plasma-enhanced chemical vapor deposition （PECVD）. Composition and structure characteristics are detected by Fourier transform infrared spectroscopy （FTIR） and X-ray photoelectron spectroscopy （XPS）. It indicates that Si-N bonds increase with increased NH3/SiH4 ratio. Electrical property investigations by I-V measurements show that the prepared films offer higher resistivity and less leakage current with increased N/Si ratio and exhibit entirely insulating properties when N/Si ratio reaches 0.9, which is ascribed to increased Si-N bonds achieved.

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.

Structural evolution and optical characterization in argon diluted Si:H thin films obtained by plasma enhanced chemical vapor deposition

The structural evolution and optical characterization of hydrogenated silicon(Si:H) thin films obtained by conventional radio frequency(RF) plasma enhanced chemical vapor deposition(PECVD) through decomposition of silane diluted with argon were studied by X-ray diffractometry(XRD),Fourier transform infrared(FTIR) spectroscopy,Raman spectroscopy,transmission electron microscopy(TEM),and ultraviolet and visible(UV-vis) spectroscopy,respectively.The influence of argon dilution on the optical properties of the thin films was also studied.It is found that argon as dilution gas plays a significant role in the growth of nano-crystal grains and amorphous network in Si:H thin films.The structural evolution of the thin films with different argon dilution ratios is observed and it is suggested that argon plasma leads to the nanocrystallization in the thin films during the deposition process.The nanocrystallization initiating at a relatively low dilution ratio is also observed.With the increase of argon portion in the mixed precursor gases,nano-crystal grains in the thin films evolve regularly.The structural evolution is explained by a proposed model based on the energy exchange between the argon plasma constituted with Ar* and Ar+ radicals and the growth regions of the thin films.It is observed that both the absorption of UV-vis light and the optical gap decrease with the increase of dilution ratio.

A perspective of microplasma oxidation (MPO) and vapor deposition coatings in surface engineering of aluminum alloys

Over the past years, great achievements have been made in the development of coating technologies for surface improvement of aluminum alloys. Despite these achievements, the role in the market strongly depends on the ability of surface coating technology under technical and economic considerations to meet the increased demands for heavy tribological applications of aluminum alloys. Microplasma oxidation (MPO) technology has recently been studied as a novel and effective means to provide thick and hard ceramic coating with improved properties such as excellent load-bearing and wear resistance properties on aluminum alloys. The present work covers the evaluation of the performances of current single and duplex coatings combining MPO, physical vapor deposition (PVD), and plasma assisted chemical vapor deposition (PACVD) coatings on aluminum alloys. It suggests that the MPO coating is a promising candidate for design engineers to apply aluminum alloys to heavy load-bearing applications. The prospective future for the research on MPO coatings is introduced as well.

Diagnosis of gas phase near the substrate surface in diamond film deposition by high-power DC arc plasma jet CVD

Optical emission spectroscopy （OES） was used to study the gas phase composition near the substrate surface during diamond deposition by high-power DC arc plasma jet chemical vapor deposition （CVD）. C2 radical was determined as the main carbon radical in this plasma atmosphere. The deposition parameters, such as substrate temperature, anode-substrate distance, methane concentration, and gas flow rate, were inspected to find out the influence on the gas phase. A strong dependence of the concentrations and distribution of radicals on substrate temperature was confirmed by the design of experiments （DOE）. An explanation for this dependence could be that radicals near the substrate surface may have additional ionization or dissociation and also have recombination, or are consumed on the substrate surface where chemical reactions occur.

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。

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。

Preparation of TiO2/MCM-41 by plasma enhanced chemical vapor deposition method and its photocatalytic activity

Titanium dioxide is coated on the surface of MCM-41 wafer through the plasma enhanced chemical vapor deposition （PECVD） method using titanium isopropoxide （TTIP） as a precursor. Annealing temperature is a key factor affecting crystal phase of titanium dioxide. It will transform an amorphous structure to a polycrystalline structure by increasing temperature. The optimum anatase phase of TiO2 which can acquire the best methanol conversion under UV-light irradiation is obtained under an annealing temperature of 700℃ for 2 h, substrate tem- perature of 500~C, 70 mL. min1 of oxygen flow rate, and 100W of plasma power. In addition, the films are composed of an anatase-rutile mixed phase, and the ratio of anatase to rutile varies with substrate temperature and oxygen flow rate. The particle sizes of titanium dioxide are between 30.3 nm and 59.9nm by the calculation of Scherrer equation. Under the reaction conditions of ll6.8mg.L-1 methanol, 2.9mg.L-1 moisture, and 75~C of reaction temperature, the best conversion of methanol with UV-light is 48.2% by using the anatase-rutile （91.3/ 8.7） mixed phase TiO2 in a batch reactor for 60 min. While under fluorescent light irradiation, the best photoactivity appears by using the anatase-rutile （55.4/44.6） mixed phase TiO2 with a conversion of 40.0%.

Deposition of ZnO Films on Freestanding CVD Thick Diamond Films

For ZnO/diamond structured surface acoustic wave （SAW） filters, performance is sensitively dependent on the quality of the ZnO films. In this paper, we prepare highly-oriented and fine grained polycrystalline ZnO thin films with excellent surface smoothness on the smooth nucleation surfaces of freestanding CVD diamond films by metal organic chemical vapour deposition （MOCVD）. The properties of the ZnO films are characterized by x-ray diffraction （XRD）, scanning electron microscopy （SEM）, and photoluminescence （PL） spectrum. The influences of the deposition conditions on the quality of ZnO films are discussed briefly. ZnO/freestanding thick-diamond-film layered SAW devices with high response frequencies are expected to be developed.

High rate deposition of microcrystalline silicon films by high-pressure radio frequency plasma enhanced chemical vapor deposition (PECVD)

Hydrogenated microcrystalline silicon (μc-Si:H) thin films were prepared by high- pressure radio-frequency (13.56 MHz) plasma enhanced chemical vapor deposition (rf-PECVD) with a screened plasma. The deposition rate and crystallinity varying with the deposition pressure, rf power, hydrogen dilution ratio and electrodes distance were systematically studied. By optimizing the deposition parameters the device quality μc-Si:H films have been achieved with a high deposition rate of 7.8 /s at a high pressure. The Voc of 560 mV and the FF of 0.70 have been achieved for a single-junction μc-Si:H p-i-n solar cell at a deposition rate of 7.8 /s.

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℃.