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本文利用六面顶压机,在5.6 GPa, 1250—1450℃的高压高温条件下,分别选用FeNiCo和NiMnCo触媒合金开展了金刚石大单晶的生长实验,系统地考察了触媒组分对金刚石单晶裂纹缺陷的影响.首先,通过对两种组分触媒晶体生长实验对比发现,金刚石大单晶裂纹缺陷出现的概率与触媒组分相关联.同NiMnCo触媒相比, FeNiCo触媒生长的金刚石单晶更容易出现生长裂纹.我们认为,这与FeNiCo触媒黏度高、流动性差、碳素输运能力差、生长中晶体比表面积大,进而导致其对生长条件稳定性的要求较高有关.其次,两种触媒极限增重速度和生长时间的关系曲线表明,相同生长时间条件下, NiMnCo触媒生长金刚石单晶的极限增重速度相对较大.再次,扫描电子显微镜测试结果表明,裂纹缺陷的出现与否同晶体表面平整度的高低无必然联系,表面平整度高的金刚石单晶内部也可能存在裂纹缺陷.最后,经对金刚石单晶傅里叶微区红外测试结果进行分析,得出了氮杂质含量的高低与金刚石单晶裂纹缺陷的出现与否无内在关联性的研究结论. 相似文献
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在铁基触媒原材料中添加不同含量的六方氮化硼,采用粉末冶金方法制备片状触媒,在六面顶压机上合成出含硼金刚石单晶。用体视显微镜对金刚石单晶的结构、形貌进行观察,并用电子探针(EPMA)和波谱仪(WDS)分析了金刚石(111)晶面的硼含量,发现金刚石表面有硼元素存在,且其含量随着触媒中掺硼量的增加而变化。在测定了含硼金刚石单晶的静压强度的基础上,采用冲击韧性测定仪和差热分析仪对不同掺硼量触媒合成出的金刚石单晶在空气中的热稳定性进行了系统的对比研究。结果表明,触媒掺硼量对金刚石的机械强度和热稳定性有重要影响,随着掺硼量的变化,其机械强度和热稳定性均存在一个最佳值。 相似文献
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在25MN合成工艺的基础上成功开发出30MN金刚石合成工艺。30MN合成工艺的成功将有助于提高金刚石质量,开发附加值更高的超硬材料产品。30MN两面顶压机合成工艺研究包含片状触媒合成工艺研究和粉末触媒合成工艺研究两个方面。片状触媒合成工艺研究进行了传压密封介质研究和优化腔体结构的研究,为了提高密封压力,在密封碗里增加内摩擦系数大的材料,解决了合成的可靠性,使30MN片状触媒合成工艺水平实现了单产80~90克拉,高品级金刚石的所占比率达到40%,其性能见表1。 相似文献
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利用FeMn粉末触媒在国产六面顶压机上进行了合成金刚石单晶的实验,研究了高温高压条件下(5.7 GPa、1 550 ℃),石墨-FeMn粉末触媒体系中金刚石单晶的生长特性。通过光学成像显微镜观测表明:合成出的金刚石单晶呈浅黄色,晶形完整,且都是八面体,晶体里含有白色物质,粒度集中在0.3~0.5 mm;通过扫描电镜观测了晶体的表面形貌,表面有熔坑;通过穆斯堡尔谱,发现粉末触媒里主要是FeMn合金和独立状态的Fe,金刚石内部主要是Fe和Fe3C;利用X射线荧光光谱,检测出样品里有Fe和Mn元素。 相似文献
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选用不同形状的{100}金刚石籽晶面,以NiMnCo合金为触媒,利用温度梯度法在压力为5.5 GPa、温度为1260~1300℃的条件下,合成Ib型金刚石大单晶。通过光学显微镜和电子显微镜对晶体的形貌进行表征。研究发现,将合成籽晶的{100}晶面切割成不同形状,只会令晶体的长宽比发生改变,晶体并不会因籽晶形状的改变而偏离{100}晶体的正常形貌。晶体的合成质量受到籽晶长宽比的影响:在籽晶长宽比较小的情况下,晶体的合成质量能够得到保证;但当籽晶长宽比过大时,合成晶体的下表面出现较多缺陷。关于籽晶形状对晶体生长情况影响的研究,揭示了籽晶形状与合成晶体形貌之间的关系,有利于更深入理解晶体的生长过程和外延生长机理,对于今后合成不同形貌的金刚石具有借鉴意义。同时此项研究有助于扩大籽晶的选取范围,降低籽晶的选择难度,提升工业级金刚石的利用率,为合成金刚石大单晶的籽晶选取提供了技术支持。 相似文献
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选用Ni-Mn-C粉末触媒,在国产DS6×800A型铰链式六面顶压机上实现了高石墨转化率的金刚石合成,其石墨转化率可达90%以上。高石墨转化率金刚石的合成,不仅有助于提高金刚石的效率,而且还可以减化提纯后处理工序。 相似文献
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本文就年轮型高压装置,对福长修的平板模型作了改进,即在式中引入了压砧的半顶角θ,计算了封垫中的压力及封垫对于压砧的支撑力,计算结果基本上和实验结果符合。就年轮型及立方六面顶型高压装置讨论了高压室和封垫的压力增量之间的匹配问题,还就卸压问题介绍了Murnaghan方程的应用。 相似文献
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以有限元法为理论基础,通过运行大型有限元软件,成功构建了铰链式六面顶压机配套顶锤的有限元理论模型,并确立了碳化钨顶锤的破裂判据。模拟结果表明:以小斜边末尾处为应力参考点,依据第四强度理论,能够对碳化钨顶锤的性能进行更加合理的数值分析。依据此判据可知:在顶锤锤面及小斜边附近,裂纹高发区分布在小斜边附近;在顶锤轴向上,裂纹高发区分布在距离顶锤锤面30 mm处。铰链式六面顶压机配套碳化钨顶锤的有限元模型以及碳化钨顶锤破裂判据的成功构建,为实现新型碳化钨顶锤的设计与研究奠定了基础,对促进实现铰链式六面顶压机腔体大型化具有现实意义。 相似文献
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We propose a design and operation of a hybrid-toroidal anvil used for the large volume cubic high pressure apparatus (LV-CHPA), such that it is possible to obtain a higher sintered quality, less weight and cost of tungsten carbide (WC) anvil than the conventional anvil. We use the finite element simulations to show the distributions of the stress on the surface and in the bulk of the WC anvils, and conclude that, for a given load on the hybrid-toroidal anvil, the volume of the compressed press medium has increased by 4.88%, and the rate of the transmitted pressure has increased by 6.72% compared with the conventional anvil. Furthermore, the advantages of the hybrid-toroidal anvil are that the movement of anvils increases by 37.14% and the growth rate of the fatigue crack decreases by 40%. This has been proved by the high pressure experiments. This work gives an approach to optimize the WC anvils used for the LV-CHPA and presents a simple method to achieve the higher sample pressure and the larger sample volume. 相似文献
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The Bridgman anvil technique offers a simple and versatile means of generating very high pressures required in solid state
studies. The opposed anvil technique is based on the principle of massive support. The practical case of a gasketted anvil
is considered, and an expression for the maximum pressure generated under massive support is derived in terms of the geometric
parameters, the strength of the anvil material and the gasket properties. In particular, for a given maximum pressure, it
is possible to calculate the taper angle, the taper height and the gasket thickness from this expression. The anvil is assumed
to be in the elastic region under load. Good agreement is obtained between the calculated and the experimental values for
the massive support factor (msf) for various taper angles. By choosing the proper geometry, it is possible to achieve a pressure as high as 130 kbar in an
alloy steel anvil. It has been clearly found that the straight portion, where the taper ends, does not really take any part
in changing the stress pattern. Thus the minimum straight portion can serve the purpose, and will result in material saving.
Anvils exhibit yielding at very high pressure. It is also pointed out that a further strengthening of the anvil can extend
the ultimate pressure. Several methods of further strengthening the anvils are discussed. 相似文献
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The absence of in situ optical probes for large volume presses (LVPs) often limits their application to high-pressure materials research. In this article, we present a unique anvil/optical window design for use in LVPs, which consists of an inverted diamond anvil seated in a Bridgman-type anvil. A small cylindrical aperture through the Bridgman anvil ending at the back of diamond anvil allows optical access to the sample chamber and permits direct optical spectroscopy measurements, such as ruby fluorescence (in situ pressure) or Raman spectroscopy. The performance of this anvil design has been demonstrated by loading KBr to a pressure of 14.5 GPa. 相似文献
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Srivastava DN Perkas N Seisenbaeva GA Koltypin Y Kessler VG Gedanken A 《Ultrasonics sonochemistry》2003,10(1):1-9
Porous nickel and cobalt oxides were prepared using their alkoxides as inorganic precursors. The stabilization of the mesostructure is especially critical for divalent elements such as Ni and Co, which do not form any network structure, like silicates. The lack of a network-forming multivalent bond is the probable reason why no stable mesoporous oxides have been synthesized for divalent elements yet. Here we have reported our attempt to synthesize porous oxides of Ni and Co. Octadecylamine has been used as the organic structure-directing agent. The product obtained was put under solvent extraction and calcination at various temperatures to remove the surfactant, followed by characterization using XRD, TEM and BET measurements. The FT/IR and thermal analyses (TGA and DSC) were also carried out for supporting information, such as extent of removal of surfactant from the pores of the metal oxide. A relatively better surface area has been obtained for the Co oxide, but in Ni the surface area found is not as good. A possible reason for that has been discussed. The porous (solvent extracted) cobalt oxide has been used as a catalyst in the oxidation reaction of cyclohexane in mild conditions. The catalyst has shown relatively better conversion of cyclohexane into cyclohexanone and cyclohexanol than the nanostructured cobalt oxide catalyst of regular structure. 相似文献
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以金刚石压腔高压装置为工具,用Ⅱ型金刚石作压砧兼红外窗口,对本征态聚苯胺进行了高压(0~8.4 GPa)就位红外光谱测试。结果表明:在4.8~5.2 GPa压力区间,代表醌环振动的吸收峰相对代表苯环振动的吸收峰变小,表明聚苯胺在此压力区间结构上发生了显著变化,且这种变化是不可逆的。聚苯胺的高压(0~14.5 GPa)电阻测量结果表明:当压力小于7.5 GPa时,电阻随压力升高而显著降低,据此认为聚苯胺为电子性导电物质;在7.5 GPa处电阻出现极小值,然后又缓慢升高,至10 GPa后基本不变。推测聚苯胺电阻极小值是由结构变化引起的。至于红外光谱与电阻测量结果反映聚苯胺结构变化的压力值不一致,可能是由于测试条件不同所致。 相似文献
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Abstract Although potentially extremely important for understanding the high-pressure microscopic behaviour of materials, over the years the area of high-pressure EXAFS in particular using diamond anvil cells has proved to be technically difficult. This has significantly hampered its development. The interference of X-ray dimaction from the diamonds in the diamond anvil cell with the absorption signal has proved to be a challenging problem to tackle, restricting the use of high-pressure EXAFS to energies below about 11 key Below 11 keV however the technique is also limited due to absorption of incident X-rays by the diamonds making it virtually impossible to conduct X-ray absorption experiments below about 9keV In this paper we describe in detail the methodology for scanriirig high-pressure EXAFS in diamond anvil cells and examine the origins of the associated problems and ways of dealing with them. We also demonstrate that it is possible to extend the useful range of studied absorption edges from 7keV up to at least 30keV This brings about new opportunities for high pressure EXAFS using diamond anvil cells. 相似文献
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