化学气相沉积法制备超纳米金刚石薄膜

采用微波等离子体化学气相沉积法,利用CH4、SiO2和Ar的混合气体在单晶硅片基底上制备出高质量的超纳米金刚石薄膜.表征结果显示,制备的薄膜致密而均匀,晶粒平均尺寸约7.47nm,表面粗糙度约15.72nm,并且其金刚石相的物相纯度相对较高,是质量优异的超纳米金刚石薄膜材料.     

用氢气/甲醇混合气体在微波等离子体CVD中合成纳米晶粒金刚石膜

用微波等离子体增强化学气相沉积方法(MPECVD),利用氢气和甲醇的混合气体,在硅片上沉积出纳米晶粒的金刚石薄膜.用扫描电子显微镜(SEM)、拉曼光谱(Raman)、原子力显微镜(AFM)及扫描隧道显微镜(STM)对薄膜的晶粒平面平整性及纯度进行了表征.通过SEM发现,提高甲醇浓度或降低沉积温度可以减小金刚石膜的晶粒尺寸.拉曼光谱显示薄膜中确实存在纳米晶粒的金刚石,并且薄膜的主要成分为金刚石.用AFM测得薄膜表面的粗糙度Rms＜80m,STM观测晶粒的平均尺寸在10～20m之间.研究结果表明,用MPECVD方法,利用氢气和甲醇的混合气体是制备纳米晶粒金刚石膜的一种理想方法.     

晶粒尺寸对CVD金刚石膜电学特性的影响

通过改变生长参数,采用热丝化学气相沉积(HFCVD)法制备了从10μm到90nm四种晶粒尺寸的金刚石膜,并制作了三明治结构的光电导探测器.采用原子力显微镜和拉曼光谱仪研究了薄膜的结构和表面形貌:表面粗糙度从423nm变化到15nm;晶粒越大,金刚石膜的质量越好.I-V特性测试结果表明随着晶粒尺寸的减小,金刚石膜的电阻率从1011Ω·cm减小到106Ω·cm.在5.9 keV的55Fe X射线辐照下,随着晶粒尺寸的减小,探测器的信噪比(SNR)呈减小趋势.     

双偏压辅助HF-PECVD沉积纳米金刚石薄膜工艺参数的AFM分析

采用双偏压辅助热丝一等离子增强化学沉积系统制备了纳米金刚石薄膜.采用AFM、SEM、Raman等考察了不同工艺条件对纳米金刚石薄膜形貌、粗糙度、内部结构等的影响.结果表明,热丝温度降低,所形成薄膜的晶粒尺寸变大,薄膜表面高低起伏较大,粗糙度也随之增大;随着射频输出功率的增大,等离子体轰击基底的能力增强,但过大的功率会使构成薄膜的晶粒变大;随着偏压的不断增大,氢离子体对薄膜表面的刻蚀程度逐渐增大,从而有利于形成纳米金刚石薄膜.     

沉积参数对化学气相沉积纳米金刚石薄膜的影响

用强电流直流伸展电弧化学气相沉积金刚石薄膜装置,在CH4-Ar和CH4-H2-Ar气氛中沉积了纳米金刚石薄膜,研究了沉积气氛中H2加入量和沉积压力对金刚石薄膜显微组织和生长机制的影响.沉积气氛中H2含量对金刚石薄膜的表面形貌、晶粒尺寸和生长速度有显著影响,随着H2含量增加,金刚石晶粒尺寸增大,薄膜生长速度提高.在1%CH4-Ar气氛中沉积的纳米金刚石薄膜,晶粒尺寸细小,薄膜表面形貌光滑平整.在1%CH4-少量H2-Ar气氛中沉积的金刚石薄膜,晶粒尺寸小于100nm,薄膜表面形貌较平整.随着沉积压力提高,金刚石薄膜的生长速度增大.用激光Ram an对金刚石薄膜进行了表征.     

多层金刚石薄膜的制备研究

利用微波等离子体化学气相沉积法,以H_2/CH_4/CO_2为混合气源,在Si基底上分别沉积了单层微米、纳米以及三层(膜层结构为微米层(MCD)/纳米层(NCD)/微米层(MCD))金刚石薄膜。利用Raman光谱、扫描电子显微镜(SEM)和X射线衍射(XRD)表征金刚石膜,以得到样品质量、表面形貌、晶粒尺寸等信息。结果表明:微米金刚石晶薄膜粒粗大,表面粗糙,纳米金刚石薄膜晶粒细小,表面平整,生长过程中控制反应参数,可以制备出多层金刚石膜,三层结构的引入,可以明显降低表面粗糙度。     

MPCVD制备纳米金刚石真空窗口的研究

微波等离子体化学气相沉积装置用于制备纳米金刚石膜和纳米金刚石真空窗口,气源为H2、CH4、Ar和少量O2。扫描电镜、拉曼光谱、X射线衍射仪、原子力显微镜用于表征和分析纳米金刚石膜,自制的漏气率测量装置测出纳米金刚石真空窗口漏气率。结果表明:金刚石膜厚20μm、表面平均粗糙度Ra=34. 6 nm,平均晶粒尺寸35 nm,金刚石窗口漏气率为2. 78×10-9Pa·m3/s。     

掺氮纳米金刚石膜的制备和性能

以Ar、CH4和CO2为反应气源,以三聚氰胺的甲醇饱和溶液为掺杂源,用微波等离子体化学气相沉积法在单晶硅基体上制备了掺氮的金刚石薄膜;用原子力显微镜,拉曼光谱以及霍尔效应测试仪等手段表征了膜的组成结构和半导体特性.结果表明:掺氮的金刚石薄膜晶粒平均尺寸约为20 nm,表面粗糙度约为8.935 nm,其拉曼光谱为典型的纳...     

单双层加热结构对纳米金刚石膜形貌及摩擦性能的影响

采用热丝化学气相沉积方法研究了CH4/H2体系不同沉积气压以及不同加热结构对金刚石薄膜组成及形貌的影响,并对其摩擦磨损性能进行了检测。结果表明:通过降低反应气体的压力和选择适当的碳源浓度的方法,可以获得纳米金刚石薄膜;采用双层丝加热,可以使颗粒尺寸及表面粗糙度控制在12 nm左右,并具有更低的摩擦系数,更好的耐磨性能。     

富氮N_2/CH_4/H_2体系中金刚石纳米线的制备研究

使用微波等离子体化学气相沉积(MPCVD)法在富氮N_2/CH_4/H_2体系中纳米金刚石膜沉积进行研究。使用扫描电子显微镜对纳米金刚石膜的表面形貌进行测试,使用光射线光电子能谱(XPS)和拉曼光谱对纳米金刚石膜的表面化学结构进行表征。结果表明,氮气浓度的改变对纳米金刚石膜的表面形貌和晶粒尺寸都有明显影响。在氮气浓度为85%时,纳米金刚石膜的表面由平均长度为2.5μm金刚石纳米线组成,晶粒尺寸在85%最低,为8 nm。纳米金刚石膜氮元素含量随氮气浓度上升而上升在95%为2.68%。晶粒尺寸下降,晶界含量上升,C=C键含量上升;晶粒尺寸上升,晶界含量下降,C=C含量下降。C-C键含量随着晶粒尺寸下降而下降,随晶粒尺寸上升而上升,同时C-C峰的FWHM值在氮气浓度为85%时最低为1.16 e V。     

Ultra-smooth nanostructured diamond films deposited from He/H2/CH4/N2 microwave plasmas

Addition of He to a high CH4 content (10.7 vol%) H2/CH4/N2 feedgas mixture for microwave plasma chemical vapor deposition produced hard (58-72 GPa), ultra-smooth nanostructured diamond films on Ti-6AI-4V alloy substrates. Upon increase in He content up to 71 vol%, root mean squared (RMS) surface roughness of the film decreased to 9-10 nm and average diamond grain size to 5-6 nm. Our studies show that increased nanocrystallinity with He addition in plasma is related to plasma dilution, enhanced fragmentation of carbon containing species, and enhanced formation of CN radical.     

Low-temperature growth of nanostructured diamond films

Nanostructured diamond films are grown on a titanium alloy substrate using a two-step deposition process. The first step is performed at elevated temperature (820 degrees C) for 30 min using a H2/CH4/N2 gas mixture to grow a thin (approximately 600 nm) nanostructured diamond layer and to improve film adhesion. The remainder of the deposition involves growth at low temperature (< 600 degrees C) in a H2/CH4/O2 gas mixture. The continuation of the smooth nanostructured diamond film growth during low-temperature deposition is confirmed by in situ laser reflectance interferometry, atomic force microscopy, micro-Raman spectroscopy, and surface profilometry. Similar experiments performed without the initial nanostructured diamond layer resulted in poorly adhered films with a more crystalline appearance and a higher surface roughness. This low-temperature deposition of nanostructured diamond films on metals offers advantages in cases where high residual thermal stress leads to delamination at high temperatures.     

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.     

Freestanding ultrananocrystalline diamond films with homojunction insulating layer on conducting layer and their high electron field emission properties

Freestanding ultrananocrystalline diamond (UNCD) films with homojunction insulating layer in situ grown on a conducting layer showed superior electron field emission (EFE) properties. The insulating layer of the films contains large dendrite type grains (400-600 nm in size), whereas the conducting layer contains nanosize equi-axed grains (5-20 nm in size) separated by grain boundaries of about 0.5-1 nm in width. The conducting layer possesses n-type (or semimetallic) conductivity of about 5.6 × 10(-3) (Ω cm)(-1), with sheet carrier concentration of about 1.4 × 10(12) cm(-2), which is ascribed to in situ doping of Li-species from LiNbO(3) substrates during growth of the films. The conducting layer intimately contacts the bottom electrodes (Cu-foil) by without forming the Schottky barrier, form homojunction with the insulating layer that facilitates injection of electrons into conduction band of diamond, and readily field emitted at low applied field. The EFE of freestanding UNCD films could be turned on at a low field of E(0) = 10.0 V/μm, attaining EFE current density of 0.2 mA/cm(2) at an applied field of 18.0 V/μm, which is superior to the EFE properties of UNCD films grown on Si substrates with the same chemical vapor deposition (CVD) process. Such an observation reveals the importance in the formation of homojunction on enhancing the EFE properties of materials. The large grain granular structure of the freestanding UNCD films is more robust against harsh environment and shows high potential toward diamond based electronic applications.     

Growth of nanocrystalline diamond films in CCl4/H2 ambient

We investigated the growth characteristics of the nanocrystalline diamond films using CCl₄/H₂ as gas sources in a hot-filament chemical vapor deposition (CVD) reactor. Successful growth of nanocrystalline diamond at typical growth condition of 1.5-2.5% CCl₄ and 550-730 °C substrate temperature has been demonstrated. Glancing angle X-ray diffraction (XRD) clearly indicated the formation of diamond in the films. Typical root-mean-square surface roughness of 10-15 nm and an optimal root-mean-square surface roughness of 6 nm have been achieved. Transmission electron microscopy (TEM) analyses indicated that nanocrystalline diamond film with an average grain size in the range of 10-20 nm was deposited from 2.5% CCl₄/H₂ at 610 °C. Effects of different source gas composition and substrate temperature on the grain nucleation and grain growth processes, whereby the grain size of the nanocrystalline film could be controlled, were discussed.     

CO2对MPCVD制备金刚石膜的影响研究

应用微波等离子体化学气相沉积（MPCVD）技术,以CH4／H2／N2为主要气源,通过添加CO2辅助气体,并与未添加CO2辅助气体进行对比,进行了金刚石膜沉积。研究了添加不同浓度CO2对生长金刚石膜的影响。结果表明：当CO2流量在0～25cm3／min范围变化时,金刚石膜表面粗糙度分别为8．9nm、6．8nm、9．2nm、9．6nm。表明适量引入CO2可以降低膜面粗糙度,但是进一步提高CO2流量,膜面粗糙度反而上升。同时当CO：流量在0～15cm3／min范围变化时,金刚石膜的品质和生长都表现出上升趋势,但是超过该流量,其品质和生长率都出现下降趋势。另外,当CO2流量为15cm3／min,生长的金刚石膜不仅品质好,而且生长率也较高。     

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).     

Optical and electrochemical properties of optically transparent,boron-doped diamond thin films deposited on quartz

The optical and electrochemical properties of transparent, boron-doped diamond thin film, deposited on quartz, are discussed. The films were deposited by microwave-assisted chemical vapor deposition, for 1-2 h, using a 0.5% CH4/H2 source gas mixture at 45 Torr and 600 W of power. A high rate of diamond nucleation was achieved by mechanically scratching the quartz. This pretreatment leads to the formation of a continuous film, in a short period of time, which consists of nanometer-sized grains of diamond. The thin-film electrode was characterized by cyclic voltammetry, atomic force microscopy, and UV-visible absorption spectrophotometry. The film's electrochemical response was evaluated using Ru(NH3)6(3+/2+) in 1 M KCl, Fe(CN)6(3-/4-) in 1 M KCl, and chlorpromazine (CPZ) in 10 mM HClO4. The film exhibited a low voltammetric background current and a stable and active voltammetric response for all three redox systems. The optical transparency of the polycrystalline film in the visible region was near 50% and fairly constant between 300 and 800 nm. The optical and electrical properties were extremely stable during 48-h exposure tests in various aqueous (HNO3, NaOH) solutions and nonaqueous (e.g., chlorinated) solvents. The properties were also extremely stable during anodic and cathodic potential cycling in harsh aqueous environments. This stability is in stark contrast to what was observed for an indium-doped tin oxide thin film coated on quartz. The spectroelectrochemical response (transmission mode) for CPZ was studied in detail, using a thin-layer spectroelectrochemical cell. Thin-layer voltammetry, potential step/ absorption measurements, and detection analytical figures of merit are presented. The results demonstrate that durable, stable, and optically transparent diamond thin films, with low electrical resistivity (approximately 0.026 omega x cm) laterally through the film, can be deposited on quartz.