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利用微波等离子体化学气相沉积(MPCVD)技术,采用偏压增加成核(BEN)、两步生长的方法在一氧化碳(CO)和氢气(H2)的环境下制备了金刚石薄膜. 利用扫描电子显微镜(SEM)、Raman光谱仪和透射电子显微镜(TEM)对金刚石薄膜的形貌和结构进行了分析. 研究发现金刚石晶粒在第一步成核及生长的过程中产生了层错和孪晶,而在第二步的生长过程中产生的层错和孪晶很少,最终形成的金刚石晶粒外表面比较光滑,包含有近五次对称或者平行的片状的孪晶,并可以观察到少量的位错. 而在样品的边缘由于等离子体的不均匀产生了比样品中心成核密度低的区域. 在这个区域中,发现了一个新的非金刚石的碳结构. 相似文献
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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 相似文献
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Results of experiments dedicated to the study of the structure under high pressure of amorphous Ge (a-Ge) and crystalline Ge (c-Ge) are reported. Energy-dispersive X-ray diffraction measurements of c-Ge have been collected at the DW11A beamline (DCI, LURE) using a heatable diamond anvil cell as pressure device up to 500?K. The a-Ge measurements have been performed at the ESRF, using the advanced set-up available at the BM29 beamline, which allows the simultaneous collection of X-ray absorption spectroscopy data and diffraction patterns used to monitor pressure and crystallization of a sample in a Paris–Edinburgh large-volume cell. The new structural data allowed us to obtain a reliable determination of the lattice parameters as a function of pressure and temperature in c-Ge and of the first-neighbor distance distribution in a-Ge. 相似文献
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Amorphous carbon films (ACFs) have recently emerged as one of the best candidates for etching-resistant hardmask materials in advanced semiconductor manufacturing processes. Etching resistivity of ACFs is known to be improved by controlling the relative abundance between sp2 and sp3 bonds. We have investigated the relative abundance between sp2 and sp3 bonds in several ACFs, fabricated by plasma-enhanced chemical vapor deposition at different temperatures, which were analyzed by using X-ray photoemission spectroscopy, Raman spectroscopy, and transmission electron microscopy. We found that the relative abundance of sp2 bond increased as the growth temperature was raised. Furthermore, the ACFs eventually evolved into nano-crystalline graphite with increasing growth temperature. 相似文献
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Intergrowth microstructures of MnF2 subjected to shock compression at 4.4, 9.0 and 21.6 GPa were examined using transmission electron microscopy (TEM). Intergrowth microstructures consisting of rutile- and α-PbO2-type phases were observed in samples shock-loaded to 4.4 and 9 GPa. The sample subjected to 21.6 GPa consisted of a twin structure with stacking faults, with a rutile-type but not the α-PbO2-type phase. In the 9.0-GPa shocked sample, the phase ledge structure originating from a phase transition is directly captured by high-resolution transmission electron microscopy. 相似文献
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A novel form of hexagonal diamond containing Li atoms in the open rooms surrounded by sp3-bonded carbon atoms was successfully synthesized from a Li graphite intercalation compound under high pressure, as had been predicted by theoretical studies. High-pressure experiments with LiC6 were performed in the pressure range from 0.1 MPa to 43 GPa using a diamond-anvil cell. In situ X-ray diffractometry and optical microscopy revealed that LiC6 was transformed to a hexagonal-diamond form without losing Li atoms. The c-axis of the hexagonal-diamond form was considerably longer than that of the hexagonal diamond transformed from pure graphite, which was consistent with the predicted structure of the endohedral Li diamond. The observed high-pressure form exhibited a golden metallic gloss, which was also consistent with the calculated metallic band structure. 相似文献
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Atsushi Kubo Yanbin Wang Takeyuki Uchida Norimasa Nishiyama Thomas S. Duffy 《Journal of Physics and Chemistry of Solids》2008,69(9):2255-2260
The melting curve of silicon has been determined up to 15 GPa using a miniaturized Kawai-type apparatus with second-stage cubic anvils made of X-ray transparent sintered diamond. Our results are in good agreement with the melting curve determined by electrical resistivity measurements [V.V. Brazhkin, A.G. Lyapin, S.V. Popova, R.N. Voloshin, Nonequilibrium phase transitions and amorphization in Si, Si/GaAs, Ge, and Ge/GaSb at the decompression of high-pressure phases, Phys. Rev. B 51 (1995) 7549] up to the phase I (diamond structure)—phase II (β-tin structure)—liquid triple point. The triple point of phase XI (orthorhombic, Imma)—phase V (simple hexagonal)—liquid has been constrained to be at 14.4(4) GPa and 1010(5) K. These results demonstrate that the combination of X-ray transparent anvils and monochromatic diffraction with area detectors offers a reliable technique to detect melting at high pressures in the multianvil press. 相似文献
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The evolution of the microstructure of a granular Cu80Fe10Ni10 (at%) melt-spun ribbon is studied by transmission electron microscopy (TEM), energy-filtered transmission electron microscopy (EFTEM) and X-ray diffraction. This system is interesting as large giant magnetoresistance (GMR) values have been measured for this composition. We have shown the presence of two face-centred cubic phases, an (Fe,Ni)-rich phase and a Cu-rich phase. The lattice parameters of these two phases are close and no diffraction or elastic contrast is involved in displaying the two phases in TEM bright-field mode. With EFTEM imaging, we have shown the presence of a fine-scale (Fe,Ni)-rich precipitation inside the Cu-rich fcc matrix. The precipitates are 2–4 nm in the as-spun state and 4–6 nm after annealing for 2 h at 400°C. The lattice parameter of the Cu-rich phase in the as-spun sample is 0.3608 nm and 0.3610 nm for the (Fe,Ni)-rich phase. After a 24-h annealing treatment at 600°C, the mean diameter of the particle is 20 nm and the lattice parameter of the (Fe,Ni)-rich phase has decreased to 0.3600 nm, while that of the Cu-rich phase has increased to 0.3613 nm, which is consistent with a segregation of Fe and Ni in the precipitates. The composition and volume fraction of the two phases measured for this annealed sample are in good agreement with the Thermocalc® predictions. 相似文献
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Diamond-like carbon (DLC) films were fabricated by pulsed laser ablation of a liquid target. During deposition process the growing films were exited by a laser beam irradiation. The films were deposited onto the fused silica using 248 nm KrF eximer laser at room temperature and 10−3 mbar pressure. Film irradiation was carried out by the same KrF laser operating periodically between the deposition and excitation regimes. Deposited DLC films were characterized by Raman scattering spectroscopy. The results obtained suggested that laser irradiation intensity has noticeable influence on the structure and hybridization of carbon atoms deposited. For materials deposited at moderate irradiation intensities a very high and sharp peak appeared at 1332 cm−1, characteristic of diamond crystals. At higher irradiation intensities the graphitization of the amorphous films was observed. Thus, at optimal energy density the individual sp3-hybridized carbon phase was deposited inside the amorphous carbon structure. Surface morphology for DLC has been analyzed using atomic force microscopy (AFM) indicating that more regular diamond cluster formation at optimal additional laser illumination conditions (∼20 mJ per impulse) is possible. 相似文献
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Maxime Noël Sergey Ananev Mattias Mases Xavier Devaux Juhan Lee Ivan Evdokimov Manuel Dossot Edward McRae Alexander V. Soldatov 《固体物理学:研究快报》2014,8(11):935-938
We report on a first study of single walled carbon nanotubes (SWCNTs) after application of dynamic (shock) compression. The experiments were conducted at 19 GPa and 36 GPa in a recovery assembly. For comparison, an experiment at a static pressure of 36 GPa was performed on the material from the same batch in a diamond anvil cell (DAC). After the high pressure treatment the samples were characterized by Raman spectroscopy and transmission electron microscopy (TEM). After exposure to 19 GPa of shock compression the CNT material exhibited substantial structural damage such as CNT wall disruption, opening of the tube along its axis (“unzipping”) and tube shortening (“cutting”). Dynamic compression to 36 GPa resulted in essentially complete CNT destruction whereas at least a fraction of the nanotubes was recovered after 36 GPa of static compression though severely damaged. The results of these shock wave experiments underline the prospect of using SWCNTs as reinforcing units in material WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim) 相似文献
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ABSTRACTHere we report a novel route for synthesizing nano-polycrystalline diamond (NPD) using stearic acid (C18H36O2) as a starting material under high pressure and high temperature. The obtained NPD shows a transparent dark-yellowish color similar to the standard NPD synthesized from graphite and consists of extremely fine diamond grains (~10?nm). The temperature required for the present synthesis of pure transparent NPD is as low as 1000°C at 13 and 17?GPa, which is surprisingly lower than that for conventional NPD synthesis (1800–2000°C). The amorphous-like, extremely poorly crystalline graphite produced by the thermal decomposition of stearic acid likely provides preferential nucleation sites for diamond and significantly lower the activation energy. The removal of volatile components such as H2O generated through the decomposition from the system is a key to obtain pore-free transparent NPD. Magnesite, MgCO3 and periclase, MgO can be used as an efficient H2O remover through the hydration reaction. 相似文献
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Yogesh K. Vohra Gopi K. Samudrala Samuel L. Moore Jeffrey M. Montgomery Georgiy M. Tsoi Nenad Velisavljevic 《高压研究》2015,35(3):282-288
Ultra-high static pressures have been achieved in the laboratory using a two-stage micro-ball nanodiamond anvils as well as a two-stage micro-paired diamond anvils machined using a focused ion-beam system. The two-stage diamond anvils’ designs implemented thus far suffer from a limitation of one diamond anvil sliding past another anvil at extreme conditions. We describe a new method of fabricating two-stage diamond micro-anvils using a tungsten mask on a standard diamond anvil followed by microwave plasma chemical vapor deposition (CVD) homoepitaxial diamond growth. A prototype two-stage diamond anvil with 300?µm culet and with a CVD diamond second stage of 50?µm in diameter was fabricated. We have carried out preliminary high pressure X-ray diffraction studies on a sample of rare-earth metal lutetium sample with a copper pressure standard to 86?GPa. The micro-anvil grown by CVD remained intact during indentation of gasket as well as on decompression from the highest pressure of 86?GPa. 相似文献
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Zahra Darvishi 《Applied Surface Science》2010,256(11):3607-9111
Nano-sepiolite with novel morphology has been fabricated by solvothermal method in different conditions. The nano-sepiolite was characterized by X-ray fluorescence analysis, X-ray powder diffraction, thermal gravimetry analysis, differential thermal analysis and infrared spectroscopy. Scanning electron microscopy observations revealed that using of solvothermal route led to nano-wires of sepiolite. The reactions have been performed in several conditions to find out the role of different factors such as the aging time and temperature of the reaction in the solvothermal on the size and morphology of the nano-structures. 相似文献
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T. Suzuki Y. Guo S. Inoue X. Zhao M. Ohkohchi Y. Ando 《Journal of nanoparticle research》2006,8(2):279-285
Uniform cathode deposits (longer than 15 mm), containing multiwalled carbon nanotubes (MWNTs) inside, were produced by dc arc discharge evaporation with a computer-controlled feeder of a pure-carbon electrode without a metal catalyst in a He–H2 gas mixture. The purification of MWNTs was carried out to remove amorphous carbon and carbon nanoparticles. High-resolution transmission electron microscopy observations and Raman scattering studies show that the MWNTs possess a high crystallinity and a mean outermost diameter of ∼
∼10 nm. It has been confirmed that the current density in the electron field emission from a purified MWNT mat can reach 77.92 mA/cm2, indicating that the purified MWNTs are a promising candidate electron source in a super high-luminance light-source tube or a miniature X-ray source. 相似文献
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Nanoparticles of cobalt ferrite prepared by the co-precipitation method with crystallite size varying from 4.7 to 41 nm have been characterized by positron annihilation lifetime spectroscopy. Three lifetime components are fitted to the lifetime data. The shortest lifetime component is attributed to the delocalized positron lifetime shortened by defect trapping. The intermediate lifetime is assigned to the positron annihilation in diffuse vacancy clusters or microvoids at the grain boundaries and at the grain-boundary triple points. The longest component corresponds to the pick-off annihilation of ortho-positronium formed at the larger voids. The variations in these lifetimes and their relative intensities with annealing temperature and crystallite size have been studied in detail. 相似文献