Growth of Free-standing Diamond Films on Graphite Substrates with Ti Interlayers

Free-standing diamond films, deposited using DC Arc Plasma Jet CVD method onto graphite substrates with titanium interlayers, have been investigated. The Ti interlayers were deposited by arc ion plating equipments. The thickness, morphology and composite phase of Ti interlayers were examined by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The titanium carbide (TiC) was detected in both sides of the interlayers, which played an important role with respect to reasonable adhesion with film and diamond nucleation. The semi-translucent diamond films were characterized by SEM and Raman spectrum. The sharp diamond peak with low intensity of amorphous carbon shows that diamond films have very high quality. The overall results suggest that plating Ti interlayer on graphite substrate is an effective way to obtain optical grade free-standing diamond films.

A review on polishing technology of large area free-standing CVD diamond films

Recently,with the rapid development of chemical vapor deposition(CVD)technology,large area free-standing CVD diamond films have been produced successfully.However,the coarse grain size on the surface and the non-uniform thickness of unprocessed CVD diamond films make it difficult to meet the application requirement.The current study evaluates several existing polishing methods for CVD diamond films,including mechanical polishing,chemical mechanical polishing and tribochemical polishing technology.

Preparation of free-standing diamond films for high frequency SAW devices

Free-standing diamond films were prepared by hot filament chemical vapor deposition (HFCVD) method under different conditions. Inter-digital transducers (IDTs) were formed on the nucleation sides of free-standing diamond films by photolithography technique. Then piezoelectric ZnO films were deposited by radio-frequency(RF) reactive magnetron sputtering to obtain the ZnO/diamond film structures. Surface morphologies of the nucleation sides and the IDTs were characterized by means of scanning electron microscopy (SEM), atomic force microscope (AFM) and optical microscopy. The results indicate that the surfaces of nucleation sides are very smooth and the IDTs are of high quality without discontinuity and short circuit phenomenon. Raman spectra show the sharp diamond feature peak at about 1 334 cm?1 and the small amount of non-diamond carbon in the nucleation side. X-ray diffraction (XRD) patterns of the structure of ZnO/diamond films show a strong diffraction peak of ZnO (002), which indicates that as-sputtered ZnO films are highly c-axis oriented.

Growth of Free-Standing Diamond Films on Stainless Steel

Free-standing diamond films have been successfully deposited on stainless steel substrates using microwave plasma-assisted chemical vapor deposition. Although iron, which is the main element of stainless steel, is known to inhibit the nucleation of diamond and enhance the formation of graphite, we were able to grow relatively thick films （-1.2 mm）. The films were easily detachable from the substrates. The poor adhesion made it possible to obtain free-standing diamond films without chemical etching. Raman spectroscopy showed the 1332 cm^-1 characteristic Raman peak of diamond and the 1580 cm^-1, 1350 cm^-1 bands of graphite on the growth surface and backside of the films, respectively. By energy dispersive X-ray spectroscopy it was only possible to detect iron on the back of the films, but not on the surface. The role of iron in the film growth is discussed.

Preparation of ZnO Thin Films on Free-Standing Diamond Substrates

Highly c-axis-oriented ZnO films were deposited successfully on the nucleation sides of free-standing diamond （FD） films by the direct current （DC） magnetron sputtering method. The effect of the sputtering parameters, such as power, gas pressure and sputtering plasma composition of Ar-to-O2, on the properties of ZnO thin films was investigated in detail. X-ray diffraction （XRD） measurements showed that, at a sputtering power of 200 W, gas pressure of 0.5 Pa and an Ar-to- O2 composition of 1：1, a higher intensity of the （002） diffraction peak and a narrower full width at half maximum （FWHM） were detected which meant high c-axis orientation and high quality of the ZnO films. To improve the quality of the ZnO film, a thin ZnO layer was pre-grown as a homo-buffer layer. XRD measurements showed that this buffer layer had a beneficial effect on the structural and morphological properties of the post-grown ZnO film.

Effect of working pressure and temperature on ZnO film deposited on free-standing diamond substrates

The structure characteristic and electric performance of ZnO film deposited on nucleation side of free-standing diamond substrates under different heating temperatures (Th) of substrate and working pressures (p) were studied. The structure of the ZnO films tested by X-ray diffraction shows that ZnO film of high c-axis orientation is deposited on the nucleation side of free-standing diamond substrate which is extremely smooth when Th=250 ℃ and p=0.4 Pa. After annealing at 480 ℃ in N2 atmosphere, the SEM and the AFM analyses demonstrate that the c-axis orientation of ZnO film is obviously enhanced. The resistivity of ZnO films also increases up to 8×105 ■·cm which is observed by I?V test.

Numerical Analysis of Nd:YAG Pulsed Laser Polishing CVD Self-standing Diamond Film

Chemical vapor deposited （CVD） diamond film has broad application foreground in high-tech fields. But polycrystalline CVD self-standing diamond thick film has rough surface and non-uniform thickness that adversely affect its extensive applications. Laser polishing is a useful method to smooth self-standing diamond film. At present, attentions have been focused on experimental research on laser polishing, but the revealing of theoretical model and the forecast of polishing process are vacant. The paper presents a finite element model to simulate and analyze the mechanism of laser polishing diamond based on laser thermal conduction theory. The experimental investigation is also carried out on Nd：YAG pulsed laser smoothing diamond thick film. The simulation results have good accordance with the results of experimental results. The temperature and thermal stress fields are investigated at different incidence angles and parameters of Nd：YAG pulsed laser. The pyramidal-like roughness of diamond thick film leads to the non-homogeneous temperature fields. The temperature at the peak of diamond film is much higher than that in the valley, which leads to the smoothing of diamond thick film. The effect of laser parameters on the surface roughness and thickness of graphite transition layer is also carried out. The results show that high power density laser makes the diamond surface rapid heating, evaporation and sublimation after its graphitization. It is also found that the good polish quality of diamond thick film can be obtained by a combination of large incident angle, moderate laser pulsed energy, large repetition rate and moderate laser pulse width. The results obtained here provide the theoretical basis for laser polishing diamond film with high efficiency and high quality.

Preparation and Characterization of High Quality Diamond Films by DC ArcPlasma Jet CVD Method

Under optimal conditions free-standing high quality diamond films were prepared by DC arc plasma jet CVD method at a growth rate of 7-10 Pm/h. Surface and cross section morphologies of the diamond films were observed by SEM. Raman spectrometer wasused to characterize the quality of diamond films. The IR transmittivity measured by IR spectrometer is close to the theoretical value ofabout 71% in the far infrared band. The thermal conductivity measured by photothermal deflection exceeds 18 W/cm' K. <l 10> is thepreferential growth orientation of the films detected by X-ray diffractometer. As s result, the extremely high temperature of DC arc plasma jet can produce supersaturated atomic hydrogen, which played an important role in the process for the deposition of high quality diamond films.

Fabrication of Diamond Microstructures by Using Dry and Wet Etching Methods

Diamond films have great potential for micro-electro-mechanical system（MEMS） application.For device realization,precise patterning of diamond films at micrometer scale is indispensable.In this paper,simple and facile methods will be demonstrated for smart patterning of diamond films,in which two etching techniques,i.e.,plasma dry etching and chemical wet etching（including isotropic-etching and anisotropic-etching） have been developed for obtaining diamond microstructures with different morphology demands.Free-standing diamond micro-gears and micro-combs were achieved as examples by using the experimental procedures.It is confirmed that as-designed diamond structures with a straight side wall and a distinct boundary can be fabricated effectively and efficiently by using such methods.

基于玻璃碳基底的超薄自支撑多晶金刚石膜制备

选取Ti、Si、玻璃碳3种基底,采用微波等离子体化学气相沉积技术,以CH_(4)/H_(2)为反应源制备超薄多晶金刚石膜。通过SEM、Raman、台阶仪表征并分析所制备的金刚石薄膜整体形态、表面(断面)形貌、组成、应力状态等。结果表明:仅以玻璃碳为基体生长的金刚石膜能自动剥离形成完整自支撑体,且薄膜表面晶粒的晶面显形清晰,膜厚仅为10μm;Raman光谱表征表明薄膜呈强的尖锐金刚石特征峰,且计算的残余应力最低,仅有−0.2161 GPa。可为超薄自支撑CVD金刚石膜的一步法生长-剥离提供新的技术途径。

微波PCVD法大尺寸透明自支撑金刚石膜的制备及红外透过率(英文)

采用微波PCVD方法制备出直径50mm膜厚300μm的大尺寸透明自支撑金刚石膜。在甲烷体积分数2%的条件下制备的透明自支撑金刚石膜经过两面抛光后在500cm-1~4000cm-1红外波段范围内红外透过率达到70%,但是其生长速率只有1μm/h^2μm/h。在体积分数4%甲烷浓度下制备的自支撑透明金刚石膜,其生长速率达到7μm/h^8μm/h,经过两面抛光之后膜厚为260μm的金刚石膜的在500cm-1~4000cm-1红外波段范围内红外透过率达到60%左右,而且膜中心和边缘区的红外透过率基本相同。这些结果为大尺寸金刚石厚膜在红外窗口上的实际应用奠定了基础。

用人工神经网络预测电铸自支撑金刚石-镍复合膜沉积结果

用人工神经网络预测了电铸自支撑金刚石-镍复合膜中金刚石颗粒的含量、复合膜的厚度和表面微观形貌。结果表明,当阴极电流密度小于1.0A/dm2时,复合膜的表面均匀,无镍瘤;复合膜的沉积速率约为14μm/h。其预测的沉积结果与实际样品测量值接近,相对误差小于9.9%。人工神经网络能够充分体现电镀工艺参数与沉积结果之间的非线性关系和隐含关系,训练精度较高,具有较高的预测能力。

DC Plasma Jet CVD金刚石自支撑膜体结构的控制生长及其表面粗糙度的研究

在 100kW级DCPlasmaJetCVD设备上,采用Ar H2 CH4 混合气体,通过控制工艺参数,在Mo衬底上获得不同占优晶面和应力状态的膜体结构。研究表明:不同取向的晶面在膜体中的分布不同,但各晶面随沉积温度的变化规律是相似的,在 900℃左右容易获得较大的(220)晶面占优的膜体结构;薄膜的内应力沿晶体生长方向逐渐减小,且随沉积温度或甲烷浓度的增大而增大;具有高取向度的膜体将获得较为平整的表面。

金刚石自支撑膜的高温红外透过性能

由于金刚石具有低吸收和优异的力学与导热性能使其成为长波(8~12μm)红外光学窗口材料的重要选择。对于许多极端条件的应用,化学气相沉积(CVD)金刚石自支撑膜的高温光学性质至关重要。应用直流电弧等离子喷射法制备光学级金刚石自支撑膜进行变化温度的红外光学透过性能研究,采用光学显微镜、X射线衍射、激光拉曼和傅里叶变换红外-拉曼光谱仪检测CVD金刚石膜的表面形貌、结构特征和红外光学性能。结果表明:在27℃时金刚石膜长波红外8~12μm之间的平均透过率达到65.95%,在500℃时8~12μm处的平均透过率为52.5%。透过率下降可分为3个阶段。对应于透过率随温度的下降,金刚石膜的吸收系数随温度的升高而增加。金刚石自支撑膜表面状态的变化,对金刚石膜光学性能的影响显著大于内部结构的影响。

光学级金刚石自支撑膜及其镀制Y_2O_3增透膜后的高温抗氧化性

为了提高金刚石膜的红外透过率和高温抗氧化性能,采用纯钇(Y)金属靶,使用直流反应磁控溅射法在光学级金刚石自支撑膜表面制备了Y2O3薄膜。对比研究了光学级金刚石自支撑膜和Y2O3/Diamond/Y2O3复合窗口的高温抗氧化性能,及氧化前后样品表面形貌和红外透过率的变化情况。热分析、扫描电子显微镜和傅立叶变换红外光谱仪的研究结果表明Y2O3薄膜对光学级金刚石膜有非常好的抗氧化防护性能,在高达950℃的温度暴露30s后对光学级金刚石膜表面没有造成明显损伤,且仍能保持良好的增透效果(透过率超过80%)。

无支撑、光学级MPCVD金刚石膜的研制

利用引进的6 kW微波等离子体化学气相沉积设备,进行了无支撑金刚石膜工艺的初步研究。在800~1050℃的基片温度范围内,金刚石膜都呈（111）择优取向;基片相对位置对沉积较大面积、光学级金刚石膜至关重要。制出0.25 mm厚Φ50 mm的无支撑金刚石膜。拉曼光谱和X射线衍射分析表明,合成的金刚石膜晶体结构完整,sp2含量极低;透过率测试结果说明了优良的光学性能：截止波长225 nm,光学透过率（λ≥2.5μm）≥70%。

大面积金刚石自支撑膜机械抛光的优化工艺研究

研究了一种用于抛光等离子体溅射CVD法制备的金刚石自支撑膜的高效安全的抛光工艺。试验探索了转盘转速、金刚石粉颗粒尺寸、磨盘表面形状对金刚石自支撑膜磨抛速率的影响。研究表明:带槽盘对金刚石自支撑膜的粗研磨效果明显,速率较高,平面盘对提高金刚石自支撑膜的表面粗糙度有利;不同颗粒的金刚石粉对应着各自合适的能充分利用其磨削能力的转速,在这个转速下,金刚石自支撑膜的磨抛速率在12μm/h左右。本文通过对新的工艺参数的探索,为金刚石自支撑膜后续加工提供有力的技术支持。

自支撑金刚石厚膜表面外延掺硼金刚石薄膜研究

采用微波等离子体化学气相沉积技术(MPCVD),在抛光厚度0.5 mm的高热导率自支撑金刚石厚膜表面沉积厚度10μm掺硼金刚石薄膜,通过热导率测试仪、扫描电子显微镜、激光拉曼光谱、X射线光电子能谱以及四探针仪等测试手段对材料的热导率、形貌及微观质量、表面键合状态及导电性能等进行分析。结果表明,优化工艺后在自支撑金刚石厚膜表面外延形成了质量优异,结合力佳的掺硼金刚石薄膜,其电阻率最低为1.7×10^(-2)Ω·cm。同时,鉴于界面同质外延特性以及大尺寸晶粒特点,整体材料的热导率可高达1750 W/(m·K),显示这种层状复合材料良好的整体导热性能及表面导电性能。

大面积无衬底自支撑金刚石厚膜沉积

讨论了在采用直流电弧等离子体喷射CVD工艺沉积大面积无衬底自支撑金刚石厚膜时遇到的若干技术问题．在制备过程中经常出现的膜炸裂现象，主要是由于膜和衬底材料线膨胀系数差异引起的巨大热应力，而衬底表面状态的控制、沉积过程中工艺参数的优化和控制也是一个重要的因素．因此，必须对整个金刚石厚膜沉积过程进行严格而系统的控制，才能有效地保证获得无裂纹大面积金刚石自支撑厚膜．

直流电弧等离子体区域电弧分布特征对自支撑金刚石膜性质的影响

直流电弧等离子体喷射法制备自支撑金刚石膜时,电弧区域可分为弧心、弧干和弧边三个区域。本文运用扫描电子显微镜(SEM)、X射线衍射(XRD)、激光Raman光谱、正电子湮没寿命谱(PAL)和力学性能实验机研究了同一块自支撑金刚石膜不同区域的生长面形貌、晶体取向、内应力、空位缺陷和断裂强度。结果表明:随着与直流电弧等离子体弧心距离增加金刚石膜生长更稳定,(220)取向晶粒减少,平均空位缺陷减少,内应力和断裂强度呈现先增大后减小的趋势。