Structure of diamond nanoparticles grown by chemical vapor deposition

We studied the structure of diamond nanoparticles grown by chemical vapor deposition. SEM images show that the material contains cubic, hexagonal, and possibly icosahedral structures ranging in size from 10 to 200 nm. Raman spectroscopy shows bands, which are characteristic of crystalline diamond, E_2g mode of hexagonal diamond, a-C, and graphite.     

微波化学气相沉积中气压对金刚石薄膜生长速率和质量的影响

研究了微波化学气相沉积中沉积气压对金刚石薄膜生长速率和质量的影响.研究表明，金刚石薄膜的生长速率随沉积气压的提高而增大，生长速率与沉积气压为线性关系.在高沉积气压下生长的金刚石薄膜晶形完整，拉曼谱测量可得到锐利的金刚石相的峰，但电压-电流测量表明，随着制备时沉积气压的提高，金刚石薄膜的暗电流增大，膜的电学质量下降. 关键词： 金刚石薄膜 生长速率 沉积气压     

同质与异质外延掺杂CVD金刚石薄膜的结构与性能

采用化学气相沉积(CVD)技术,以高温高压(HTHP)合成的(100)金刚石和p型(100)Si为衬底制备了硫掺杂和硼-硫共掺杂金刚石薄膜,利用原子力显微镜(AFM)、扫描隧道显微镜(STM)及隧道电流谱(CITS)等手段分析同质和异质外延CVD掺杂金刚石薄膜的结构和性能.结果表明:异Si衬底上CVD金刚石的形核密度低,薄膜表面比较粗糙,粗糙度达到18.5nm;同质HTHP金刚石衬底上CVD金刚石薄膜晶粒尺寸约为10—50nm,表面平整,表面粗糙度为1.8nm.拉曼测试和电阻测量的结果显示,在HTHP金刚 关键词： 金刚石 掺杂 外延     

Response of chemical vapor deposition diamond detectors to X-ray

The outstanding properties of diamond, such as radiation hardness, high carrier mobility, high band gap and breakdown field, distinguish it as a good candidate for radiation detectors. The detector's performance is strongly limited by the concentration of defects (grain boundaries and/or impurities) in chemical vapor deposition (CVD) diamond. We report the response of free-standing CVD diamond with a thickness of 300 μm and area of 2×2 cm², synthesized by a hot filament chemical vapor deposition (HFCVD) technique, to 5.9 keV X-ray radiation from a ⁵⁵Fe source. The linear I-V characteristics indicate that CVD diamond has good ohmic contacts. This detector also shows good results such as dark-current of 10⁻⁸ A, photocurrent of 10⁻⁶ A, energy resolution <0.4%, and a high ratio of signal to noise.     

Atmospheric pressure plasma treatment on graphene grown by chemical vapor deposition

We demonstrate the surface treatment of graphene using an atmospheric pressure plasma jet (APPJ) system. The graphene was synthesized by a thermal chemical vapor deposition with methane gas. A Mo foil and a SiO₂ wafer covered by Ni films were employed to synthesize monolayer and mixed-layered graphene, respectively. The home-built APPJ system was ignited using nitrogen gas to functionalize the graphene surface, and we studied the effect of different treatment times and interdistance between the plasma jet and the graphene surface. After the APPJ treatment, the hydrophobic character of graphene surface changed to hydrophilic. We found that the change is due to the formation of functionalities such as hydroxyl and carboxyl groups. Furthermore, it is worth noting that the nitrogen plasma treatment induced charge doping on graphene, and the pyridinic nitrogen component in the X-ray photoelectron spectroscopy spectrum was significantly enhanced. We conclude that the atmospheric pressure plasma treatment enables controlling the graphene properties without introducing surface defects.     

CVD金刚石膜的结构分析

利用x射线广角衍射和低角掠入射散射谱、正电子湮没谱、定性分析软件和Positronfit程序，研究了生长在Si（100）基底上的金刚石膜微结构.研究发现，在样品邻近基底区域为纳米 多晶结构，具有弱的［111］织构；在邻近表面区域为微米多晶结构，具有强的［220］织构 .金刚石膜样品有空位、空位团和空洞3种缺陷，其中主要缺陷是大约10个空位形成的空位团 . 关键词： 金刚石膜 化学气相沉积 x射线掠入射 正电子湮没谱     

激光轴向偏焦法平整化CVD金刚石膜

利用Nd:YAG型金刚石精密激光切割机,采用激光轴向偏焦法对化学气相沉积（CVD）法制备的金刚石膜表面进行扫描式平整化处理,利用扫描电子显微镜（SEM）、粗糙度仪和金相显微镜对平整化后的金刚石表面进行表征,研究了激光充电电压和焦点位置对扫描凹槽宽度和深度的影响,以及扫描间距对平整化效果的影响。研究结果表明:扫描凹槽宽度随激光充电电压的升高而增大;凹槽深度随激光充电电压的升高而增大,随偏焦量的增大而增大。激光轴向偏焦法对CVD金刚石膜进行平整化处理后,其粗糙度显著减小,利用氢等离子体对其表面进行刻蚀处理,能够有效去除表层石墨,从而达到理想的平整化效果。     

激光轴向偏焦法平整化CVD金刚石膜

利用Nd：YAG型金刚石精密激光切割机,采用激光轴向偏焦法对化学气相沉积（CVD）法制备的金刚石膜表面进行扫描式平整化处理,利用扫描电子显微镜（SEM）、粗糙度仪和金相显微镜对平整化后的金刚石表面进行表征,研究了激光充电电压和焦点位置对扫描凹槽宽度和深度的影响,以及扫描间距对平整化效果的影响。研究结果表明：扫描凹槽宽度随激光充电电压的升高而增大;凹槽深度随激光充电电压的升高而增大,随偏焦量的增大而增大。激光轴向偏焦法对CVD金刚石膜进行平整化处理后,其粗糙度显著减小,利用氢等离子体对其表面进行刻蚀处理,能够有效去除表层石墨,从而达到理想的平整化效果。     

Enhanced field emission characteristics of boron doped diamond films grown by microwave plasma assisted chemical vapor deposition

Boron doped diamond films were synthesized on silicon substrates by microwave plasma chemical vapor deposition (MPCVD) technique. The effect of B₂O₃ concentration varied from 1000 to 5000 ppm on the field emission characteristics was examined. The surface morphology and quality of films were characterized by scanning electron microscope (SEM) and Raman spectroscopy. The surface morphology obtained by SEM showed variation from facetted microcrystal covered with nanometric grains to cauliflower of nanocrystalline diamond (NCD) particles with increasing B₂O₃ concentration. The Raman spectra confirm the formation of NCD films. The field emission properties of NCD films were observed to improve upon increasing boron concentration. The values of the onset field and threshold field are observed to be as low as 0.36 and 0.08 V/μm, respectively. The field emission current stability investigated at the preset value of ∼1 μA is observed to be good, in each case. The enhanced field emission properties are attributed to the better electrical conductivity coupled with the nanometric features of the diamond films.     

Boron-doped diamond synthesized by chemical vapor deposition as a heating element in a multi-anvil apparatus

ABSTRACT

We tested boron-doped diamond (BDD) synthesized by chemical vapor deposition (CVD) as a heating element in a multi-anvil apparatus. We succeeded in manufacturing BDD into a tubular shape by laser cutting and electric discharging machining. The BDD tube shaped by the electric discharging machining was contaminated by discharging electrode materials (Mo and W), which affected the heating performance. The laser-cut BDD tube has a clean surface and, therefore, had a good heating performance. We succeeded in generating temperature as high as 2670?K at a pressure around 30?GPa with laser-cut heater. Heating reproducibility was confirmed through repeated heating and cooling cycles. The recovered sample shows that a higher temperature generation above 2670?K was prevented by eutectic melting of ZrO₂ thermal insulator and Al₂O₃ sample. Owing to the commercial availability with a reasonable price, CVD–BDD heaters are more practical than a high-pressure synthesized BDD heaters for wide applications.     

化学气相沉积金刚石探测器测量辐射驱动内爆的硬X射线

金刚石探测器具有响应快、灵敏度高、动态范围大、平响应、击穿电压高、抗辐射等优点, 广泛运用于X射线测量. 利用化学气相沉积方法制备的光学级金刚石, 采用金属-金刚石-金属结构研制了X射线金刚石探测器. 在8ps激光器上的探测器响应性能考核表明, 整个探测器系统的响应时间为444 ps, 上升时间为175 ps, 载流子寿命为285 ps. 将探测器应用于神光Ⅲ原型装置的内爆物理实验硬X射线测量, 分别测量得到以注入黑腔的激光转化为主和靶丸内爆产生为主的硬X射线能流, 测得的峰值信号分别正比于激光总能量和反比于靶丸CH层厚度. 关键词： CVD金刚石探测器 硬X射线 激光能量     

化学气相沉积金刚石X射线探测器相对标定

利用神光Ⅱ激光装置,开展了化学气相沉积金刚石X射线探测器的相对标定技术研究。实验得到了金刚石X射线探测器与已绝对标定的平响应X射线二极管对X射线辐射的测量结果,计算得到金刚石X射线探测器平均灵敏度为1.19610-5 C/J,不同发次得到的灵敏度与平均值之间的偏差不大于13%。     

Bolometric detector embedded in a polycrystalline diamond grown by chemical vapor deposition

A fast bolometric detector embedded in a plate of chemical-vapor-deposited polycrystalline diamond was developed and fabricated. The working element of the bolometer is a buried graphitized layer (with temperature-sensitive resistance) fabricated in the bulk of a diamond by C⁺ ion implantation followed by annealing. The kinetics of the response of the structure to irradiation with light from an LGI-21 pulsed nitrogen laser (λ = 337 nm, τ_P ～ 8 ns) were studied. The room-temperature response width at half-maximum is ～ 20 ns. Using the space-time distribution of responses of the structure, thermal (bolometric) signals were resolved from signals of different nature (photoconductivity or photovoltage).     

微波等离子体化学气相沉积合成掺氮金刚石薄膜的缺陷和结构特征及其生长行为

Diamond film was deposited in CH₄ and H₂ gas mixture with a small amount of N₂ by microwave plasma assisted chemical vapor deposition (MPCVD). Scanning electron microscopy, Raman spectroscopy and transmission electron microscopy were applied to characterize the film. The results showed that the growth of grains are different the central region and the edge. In the central region, diamond grains nucleated with a density as high as 4.8×10⁸ cm^-2 and were preferential in 〈001〉 orientation. The inner grains formed an area without stacking faults,which was surrounded by a rim with a high density of stacking faults. A growth model was suggested to interpret the morphological feature and the behavior of preferential growth. At the edge, the grains were identified to be 6H polytypes of diamond and a new twin relationship of grains was found. Besides, the effect of the N dopant on the growth behavior of the diamond film deposited by MPCVD was discussed in connection with the growth rate of the film. 关键词： 金刚石 结构表征 透射电子显微镜 多型金刚石     

High pressure sintering behavior of polycrystalline diamond with tungsten

Polycrystalline diamond was investigated under high pressure and high temperature of 5.0 GPa and 1100–1500 °C in the presence of tungsten. In situ resistance measurements indicated that reactions between diamond and tungsten happened at about 960 °C. Phase analysis demonstrated that WC increased and meta-stability of W₂C decreased clearly at the higher temperature. It is clear from the characterization of the sintered body that the electrical resistance decreased and the density of specimens increased as the sintering temperature rose. The specimen sintered at 1500 °C has a homogeneous microstructure and good conductivity.     

Large single crystal diamond grown in FeNiMnCo-S-C system under high pressure and high temperature conditions

Large diamonds have successfully been synthesized from FeNiMnCo-S-C system at temperatures of 1255-1393 ℃and pressures of 5.3-5.5 GPa.Because of the presence of sulfur additive,the morphology and color of the large diamond crystals change obviously.The content and shape of inclusions change with increasing sulfur additive.It is found that the pressure and temperature conditions required for the synthesis decrease to some extent with the increase of S additive,which results in left down of the V-shape region.The Raman spectra show that the introduction of additive sulfur reduces the quality of the large diamond crystals.The x-ray photoelectron spectroscopy(XPS) spectra show the presence of S in the diamonds.Furthermore,the electrical properties of the large diamond crystals are tested by a four-point probe and the Hall effect method.When sulfur in the cell of diamond is up to 4.0 wt.%,the resistance of the diamond is 9.628×10~5 Ω·cm.It is shown that the large single crystal samples are n type semiconductors.This work is helpful for the further research and application of sulfur-doped semiconductor large diamond.     

High pressure generation in the Kawai-type multianvil apparatus equipped with sintered diamond anvils

ABSTRACT

Generation of high pressure is a key to the investigation of the interior of the Earth. The Kawai-type multianvil apparatus (KMA) has been widely used in the fields of Earth science and material science. In conventional KMA, tungsten carbide (WC) has been used as the second stage anvil material. However, attainable pressure is limited to ～70?GPa even if newly developed WC is used. Recently, on the other hand, second stage anvils of sintered diamond that is much harder than WC have enabled us to extend the pressure range of KMA up to 120?GPa, corresponding to the pressure of the D” layer in the Earth’s mantle. It is evident that our development of pressure generation facilitates the investigation of the structure and dynamics of the deep mantle of the Earth.     

High-energy X-ray diffraction of a hydrous silicate liquid under conditions of high pressure and temperature in a modified hydrothermal diamond anvil cell

In situ high-energy X-ray diffraction measurements were made for the first time on a water-saturated silicate melt at high pressure and temperature. A modified hydrothermal diamond anvil cell (HDAC), designed to minimize the path length of the X-ray beam within a diamond anvil and to increase the solid angle of the diffracted beam, was used to reduce high background contributions and extend X-ray diffraction data collection in Q space. Quantitative differential pair distribution function (PDF) analysis of X-ray diffraction data show that the first measurable (Si–O) peak is 0.095 Å greater in length in the hydrous melt than in the starting glass. Contributions from the H₂O O–O correlations, as well as from the second nearest neighbor O–O correlations within the silicate melt, are evident within the second peak of the differential PDF. The procedure described opens new opportunities to directly investigate volatile-rich melts at high pressure and temperature.     

Investigation of optical emission spectroscopy in diamond chemical vapor deposition by Monte Carlo simulation

The optical emission spectra(atomic hydrogen(Hα,Hβ,Hγ),atomic carbon C(2p3s→2p2:λ=165.7 nm) and radical CH(A2△→X2П:λ=420-440 nm))in the gas phase process of the diamond film growth from a gas mixture of CH4 and H2 by the technology of electron-assisted chemical vapor deposition (EACVD)have been investigated by using Monte Carlo simulation.The results show that the growth rate may be enhanced by the substrate bias due to the increase of atomic hydrogen concentration and the mean temperature of electrons.And a method of determining the mean temperature of electrons in the plasma in-situ iS given.The strong dependence on substrate temperature of the quality of diamond film mainly attributes to the change of gas phase process near the substrate surface.