石英玻璃上生长表面光滑高光透射率的金刚石膜

石英玻璃衬底在金刚石粉和丙酮形成的悬浮液中超声波预处理,有效提高了金刚石成核密度.在最佳预处理和热丝化学气相沉积条件下,成核密度高达1010 cm-2以上.采用HFCVD中四步法生长工艺,制备出了表面粗糙度小于10 nm、膜厚300 nm、晶粒直径100 nm～150 nm、致密、均匀、高质量和高光透射率的金刚石膜,其1 μm～5 μm波段的光透射率达74%～85%.金刚石膜与石英玻璃衬底结合牢固,膜中无裂纹.     

硫化锌窗口上CVD法制备金刚石膜的研究进展

金刚石具有优异的红外透过性能,可作为硫化锌红外窗口的保护膜。但由于CVD金刚石的沉积过程会刻蚀硫化锌衬底,导致在窗口表面直接生长金刚石膜比较困难。本文主要综述了近年来通过添加过渡层沉积金刚石薄膜的方法和光学焊接金刚石厚膜的方法来增强硫化锌窗口的性能,并介绍了CVD金刚石膜的光学应用及其目前所存在的问题,最后对未来CVD金刚石膜发展的方向作出了展望。     

金刚石膜红外光学性质的研究

采用热灯丝化学气相沉积(CVD)方法,通过独特的衬底表面预处理工艺及控制沉积参数,制备出了晶粒细、表面光滑的单片金刚石膜样品。采用SEM观察了样品生长面的表面形貌,通过激光Raman对样品进行了金刚石结构的确认。在450～4000cm~(-1)范围测试了金刚石膜样品的红外光学透过谱,通过分析认为:平均透过率随波长减小而衰减主要是由于金刚石膜生长面的表面粗糙度引起光谱散射造成的。     

端部霍尔等离子体源沉积类金刚石膜的研究

本文通过对端部霍尔离子源特性的研究 ,采用自行研制的用于离子束辅助沉积的端部霍尔离子源成功镀制了类金刚石膜 ,并对采用该离子源制备类金刚石膜的工艺进行了研究和分析。实验结果表明 ,采用端部霍尔离子源镀制类金刚石膜不仅操作简单、可实现大面积沉积 ,而且类金刚石膜的沉积速率较大 ,最大可达 0 .8nm s,其折射率依不同工艺在 1.8～ 2 .2之间可调。并对不同工艺条件下制备的类金刚石膜的硬度进行了测试和分析。     

非平衡磁控溅射无氢DLC增透膜的研制

非平衡磁控溅射(UBMS)技术近年来得到了广泛地应用.采用该技术制备的类金刚石薄膜(DLC)具有许多独特的性质.本文利用正交实验方法,对非平衡磁控溅射技术制备无氢DLC膜增透膜进行了研究,得到了影响薄膜光学性能的主要因素和最佳的制备工艺.结果表明,非平衡磁控溅射制备的无氢DLC膜具有较宽的光谱透明区,锗基底单面沉积DLC膜,其峰值透射率达到61.4%,接近理论值.     

工艺条件对热丝 CVD金刚石薄膜电学性能的影响

采用不同的沉积条件,通过HFCVD方法制备了四种不同质量、不同取向的CVD金刚石薄膜．讨论了薄膜退火前后的介电性能．研究了不同沉积条件和退火工艺与介电性能之间的联系．通过扫描电镜SEM、Raman光谱、XRD、I-V特性曲线以及阻抗分析仪表征CVD金刚石薄膜的特性．结果表明,退火工艺减少了薄膜吸附的氢杂质,改善了薄膜质量．获得的高质量CVD金刚石薄膜具有好的电学性能,在50V偏压条件下电阻率为1．2×1011Ω·cm,频率在2MHz条件下介电常数为5．73,介电损耗为0．02．     

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。     

大面积光学级金刚石自支撑膜制备、加工及应用

大面积光学级金刚石自支撑膜的制备和加工是近年来在CVD金刚石研究领域的最重要的技术进展之一.在军事和民用光学领域有非常重要的应用前景.本文综述了北京科技大学近年来在CVD金刚石膜光学应用领域的研究进展.给出了采用高功率直流电弧等离子体喷射(DC Arc Plasma Jet)CVD工艺制备大面积光学级金刚石自支撑膜的研究结果,并报导了对所制备的光学级金刚石自支撑膜的光学、力学(机械)、热学、微波介电性能和抗激光损伤等方面的最新研究结果.     

用压痕试验法研究CVD金刚石膜的粘附性能

在观察与分析压入过程中CVD金刚石膜开裂方式的基础上,初步探讨了用压痕试验法评定CVD金刚石膜粘附性能的可行性．采用反映膜／基粘附性能的临界开裂或剥落载荷P_er和抗裂性参数dP／dX两指标评定了硬质合金基体表面经不同预处理方法和沉积工艺参数合成的金刚石膜的粘附性能;研究了粘附性能指标与沉积工艺参数（如甲烷浓度、沉积气压、沉积功率）之间的关系．适当的表面预处理、适中的甲烷浓度、较低的沉积气压、较高的沉积功率均有利于改善金刚石膜的粘附性能．     

由红外透过谱确定金刚石膜的光学常数及相关因素

结合金刚石膜的具体情况,考虑到色散效应、膜的微结构、表面粗糙度及样品中自由载流子和C-H的吸收等多种因素对红外透过谱的影响,在无吸收单层膜透过率模型的基础上进行了修正,给出了自支撑金刚石薄膜透过率的数学模型.并对不同制备方法和工艺参数下沉积的金刚石膜的红外透过谱用Levenberg-Mar-quardt算法进行非线性最小二乘拟合,从而确定出样品的红外光学常数和其它影响透过率的因素.这些结果对正确分析金刚石薄膜的红外光学性质是很重要的.     

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

采用微波PCVD方法制备出直径50mm膜厚300um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红外波段范同内红外透过率达到70%,但是其生长速率只有1um/h-2um/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7um/h～8um/h,经过两面抛光之后膜厚为260um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.     

Study of the moderate-temperature growth process of optical quality synthetic diamond films on quartz substrates

Growth of undoped and boron-doped diamond films on quartz substrates at moderate temperature of 500 °C by microwave plasma chemical vapor deposition method was studied in terms of growth rate, surface roughness and optical transmittance. Similar density of diamond seed particles on quartz surfaces seeded mechanically before the deposition process and diamond grains within diamond films grown on those substrates is observed. The growth rate is found similar to that reported for diamond deposited on silicon substrates in the same plasma deposition system, although with substantially higher activation energy. Furthermore, increased level of dopant concentration in the gas mixture resulted in a decrease of the growth rate, while a gradual reduction of the surface roughness occurred at high dopant levels. Overall, the highest measured regular optical transmittance of the undoped diamond film on quartz was 45% at 1100 nm (including quartz absorption), whereas that of boron-doped diamond peaked 5% at 700 nm (tail absorption of boron centers).     

化学气相沉积金刚石薄膜生长的原位反射率测量

报道了化学气相沉积金刚石薄膜生长的原位反射率测量,提出了监控金刚石薄膜生长的激光反射多光束干涉的数学模型。通过原位反射率的测量,精确监控了金刚石薄膜的生长厚度,成功地制备了红外增透增,这种方法的测量装置简单、紧凑而且可靠。     

红外光学材料硫化锌衬底上沉积金刚石膜的研究

采用微波等离子体化学气相沉积法,在预镀陶瓷过渡层的硫化锌衬底上沉积金刚石膜。在以前的实验中,我们发现在陶瓷过渡层上沉积金刚石膜极其困难,但采用金刚石诱导形核方法后,我们已经在过渡层／硫化锌试样表面获得了很小面积（约1mm宽的环状区域）的金刚石形核。本文对前期的诱导形核工作进行了一定改进,目前已经使形核生长范围大大增加,沉积面积超过原来10倍。此外,本文对金刚石／过渡层／硫化锌试样的红外透过特性以及金刚石膜质量等进行了评价。     

Diamond and diamond-like carbon films

Polycrystalline diamond films are grown from low pressure gas mixtures, the deposition techniques are Microwave Plasma Chemical Vapour Deposition and Hot filament Chemical Vapour Deposition, in both techniques the deposition temperature is close to 900°C. The film growth process is strongly dominated by the initial nucleation stage, after this stage, the film grows at a rate of one micron per hour. The carbon atoms in the diamond film are fully fourfold (sp³) co-ordinated and the film properties are close to those of single crystalline diamond: extremely hard, resistant and transparent from UV to IR.Diamond-like carbon (DLC) films are amorphous and contain a variable amount of hydrogen in their structure, the carbon atoms are partially threefold (sp²) co-ordinated. Films are obtained at temperatures below 250°C and deposited on almost any substrate. Film composition, structure and functional properties are strongly dependent on the level of ionic bombardment of the film during growth. DLC films are very hard, have a low friction coefficient and good wear resistance, are chemically inert and are transparent in the IR.     

Optimization of chemical vapor deposition diamond films growth on steel: correlation between mechanical properties, structure, and composition

In the present work we perform optimization of mechanical and crystalline properties of CVD microcrystalline diamond films grown on steel substrates. A chromium-nitride (Cr-N) interlayer had been previously proposed to serve as a buffer for carbon and iron inter-diffusion and as a matching layer for the widely differing expansion coefficients of diamond and steel. However, adhesion and wear as well as crystalline perfection of diamond films are strongly affected by conditions of both Cr-N interlayer preparation and CVD diamond deposition. In this work we assess the effects of two parameters. The first one is the temperature of the Cr-N interlayer preparation: temperatures in the range of 500 degrees C-800 degrees C were used. The second one is diamond film thickness in the 0.5 microm-2 microm range monitored through variation of the deposition time from approximately 30 min to 2 hours. The mechanical properties of so deposited diamond films were investigated. For this purpose, scratch tests were performed at different indentation loads. The friction coefficient and wear loss were assessed. The mechanical and tribological properties were related to structure, composition, and crystalline perfection of diamond films which were extensively analyzed using different microscopic and spectroscopic techniques. It was found that relatively thick diamond film deposited on the Cr-N interlayer prepared at the temperature similar to that of the CVD process has the best mechanical and adhesion strength. This film was stable without visible cracks around the wear track during all scratch tests with different indentation loads. In other cases, cracking and delamination of the films took place at low to moderate indentation loads.     

热阴极辉光放电对金刚石膜沉积的影响

研究了在热阴极辉光放电等离子体化学气相沉积金刚石膜过程中，热阴极辉光放电特性与金刚石膜沉积工艺的关系．结果表明，适当的阴极温度是保证大电流、高气压辉光放电的必要条件．阴极的温度影响辉光放电阴极位降区的放电性质．金刚石膜的沉积速率随着气体压力(16～20kPa)的升高而上升，在18.6kPa左右出现最高值，而阳极位降区电场强度的降低使膜品质下降．放电电流(8～12A)对沉积速率的影响与气体压力的影响具有相似的规律．     

微波等离子体化学气相沉积技术制备金刚石薄膜的研究

介绍了微波等离子体化学气相沉积法（MPCVD）制备金刚石薄膜的研究情况，重点论述了该法的制备工艺对金刚石薄膜质量的影响及其制备金刚石薄膜的应用前景。     

直流热阴极PCVD法间歇生长模式制备金刚石膜

采用直流热阴极PCVD(Plasma chemical vapor deposition)法间歇生长模式制备金刚石膜,通过加入周期性的刻蚀阶段清除金刚石膜在一定生长期中形成的石墨和非晶碳等杂质,实现了金刚石膜生长的质量调控。间歇式生长过程分为沉积阶段和刻蚀阶段,两个阶段交替进行。采用Raman光谱、SEM和XRD对所制金刚石膜的品质进行了表征,并与同样生长条件下连续生长模式制备的金刚石膜样品进行了比较。结果表明,当单个生长周期为30 min(沉积时间为20 min、刻蚀时间为10 min)时,直流热阴极PCVD法间歇生长模式制备的金刚石膜中的非金刚石相杂质含量低于连续间歇生长模式制备的金刚石膜。     

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.