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     

Strength and equation of state of molybdenum triboride under 80 GPa pressure,using radial X-ray diffraction

The strength and equation of state of molybdenum triboride have been determined under nonhydrostatic compression up to 80?GPa, using an angle-dispersive radial X-ray diffraction technique in a diamond anvil cell (DAC). The RXD data yield a bulk modulus and its pressure derivative as K_0?=?342(6)?GPa with K₀′?=?2.11(17) at ψ?=?54.7°. Analysis of diffraction data using the strain theory indicates that the ratio of differential stress to shear modulus (t/G) ranges from 0.002 to 0.050 at pressures of 4–80?GPa. Together with theoretical results on the high pressure shear modulus, our results here show that molybdenum triboride sample under uniaxial compression can support a differential stress of ～10?GPa when it started to yield with plastic deformation at ～30?GPa. In addition, we draw a conclusion that MoB₃ is not a superhard material but a hard material.     

用显微金刚石池测试高分子弹性材料的红外光谱

本文论述了用显微金刚石池研究高分子弹性材料，方法简便、快速和精确。     

Ruby fluorescence pressure scale： Revisited

Effect of non-hydrostatic stress on X-ray diffraction in a diamond anvil cell (DAC) is studied. The pressure gradient in the sample chamber leads to the broadening of the diffraction peaks, which increase with the hkl index of the crystal. It is found that the difference between the determined d-spacing compressive ratio d/d0 and the real d-spacing compressive ratio dr/d0 is determined by the yield stress of the pressure transmitting media (if used) and the shear modulus of the sample. On the basis of the corrected experiment data of Mao et al. (MXB86), which was used to calibrate the most widely used ruby fluorescence scale, a new relationship of ruby fluorescence pressure scale is corrected, i.e., P = (1904/9.827)[(1+λ/λ0)9.827-1].     

Fracture of diamond coatings by high velocity sand erosion

This paper describes a study of the behaviour of diamond coatings when subjected to solid particle erosion from sand particles. The coatings were deposited by chemical vapour deposition (CVD) onto tungsten substrates and tested using a high velocity air–sand erosion test facility. The erosion tests were conducted using particle impact velocities of between 33 and 268 m/s. Examination of the eroded test specimens showed that the principal damage features were circumferential cracks and pin-holes. Comparison with Hertz impact theory revealed that the measured circumferential crack diameters were more than double the predicted Hertzian contact diameter. Moreover, a trend of increasing circumferential crack diameter with coating thickness, which is not predicted by Hertz, was found. Instead, the crack diameters showed good agreement with those predicted by the theory of stress wave reinforcement, which is more commonly associated with liquid impact damage of brittle materials. During impact, the bulk compression and shear waves are reflected at the rear surface of debonded regions of the coating to return to the front surface and reinforce the Rayleigh surface wave, which generates a tensile stress. Where this stress exceeds the local tensile strength of the coating, a ring of cracks surrounding the area of impact is created. The results from the present study therefore suggest that stress wave reflection is responsible for the formation of the cracks at locally debonded regions of the coating. This hypothesis was supported by images acquired using scanning acoustic microscopy, which showed that circumferential cracks and pin-holes were only found on areas of the coating that had become delaminated by multiple particle impacts during the erosion tests.     

A New Indirect Electroanalytical Method to Monitor the Contamination of Natural Waters with 4‐Nitrophenol Using Multiwall Carbon Nanotubes

The electrochemical detection of the hazardous pollutant 4‐nitrophenol (4‐NP) at low potentials, in order to avoid matrix interferences, is an important research challenge. This study describes the development, electrochemical characterization and utilization of a multiwall carbon nanotube (MWCNT) film electrode for the quantitative determination of 4‐NP in natural water. Electrochemical impedance spectroscopy measurements showed that the modified surface exhibits a decrease of ca. 13 times in the charge transfer resistance when compared with a bare glassy carbon (GC) surface. Voltammetric experiments showed the possibility to oxidize a hydroxylamine layer (produced by the electrochemical reduction of 4‐NP on the GC/MWNCT surface) in a potential region which is approximately 700 mV less positive than that needed to oxidize 4‐NP, thus minimizing the interference of matrix components. The limit of detection for 4‐NP obtained using square‐wave voltammetry (0.12 μmol L^?1) was lower than the value advised by EPA. A natural water sample from a dam located in São Carlos (Brazil) was spiked with 4‐NP and analyzed by the standard addition method using the GC/MWCNT electrode, without any further purification step. The recovery procedure yielded a value of 96.5% for such sample, thus confirming the suitability of the developed method to determine 4‐NP in natural water samples. The electrochemical determination was compared with that obtained by HPLC with UV‐vis detection.     

人造金刚石生长中的温度控制

 本文讨论了与腔体组装方法、温度梯度和边界条件等有关的温度控制问题及其对金刚石生长的影响。     

金刚石近红外增透滤光保护窗口的制备及应用

报道金刚石近红外增透滤光保护窗口的研制及其在工业中的应用。采用热灯丝化学气相沉积方法成功地制备出金刚石近红外增透滤光保护窗口，其工作波长为１．３￣１．８μｍ，具有良好的光学透过性和优良的物理化学性质。该窗口已在上海宝钢获得成功应用。     

Effect of Li2CO3 on formation temperature of hBN by modified O'Connor model

This study is interested in the effect of lithium carbonate on the formation of hexagonal boron nitride (hBN) by means of the available experimental methods including TGA, XRD, FTIR, SEM and HR‐TEM. hBN samples were synthesized at the 1450 °C with different molar ratios of lithium carbonate by modified O'Connor routine. The crystalline hBN formation tended to improve with the increment of the Li₂CO₃ concentration level (especially after more 20 %). The dopant quantity decreased the residual stresses due to the presence of possible relaxation mechanisms along with the nanocrystal structure, even favored by XRD experimental findings regarding the enhancement of crystal plane alignments, crystallite sizes and lattice parameters. As for the FTIR surveys, the Li₂CO₃ foreign impurities strengthened more and more the covalent bonds between boron and nitrogen atoms. At the same time, the samples with 40 % lithium carbonate were annealed at the varied temperatures of 1000, 1150, 1300 and 1450 °C to determine the optimum annealing temperature. The XRD+FTIR investigations indicated that the degree of hexagonality improved with the increased annealing temperature. Similarly, the surface morphology confirmed not only the formation of regularity and flaky hexagonal BN structures, but also the strengthening of covalent bonds between the atoms.