触媒静压法合成金刚石的机理问题

对太原市晋阳金刚石厂触媒静压法合成金刚石的专用石墨、触媒和合成产物进行了观测。看到有的金刚石生长在石墨中,也有的金刚石生长在触媒上。依照扫描电镜的形貌观察,我们认为,此种材料和工艺生产的金刚石,其形成机理是“直接转化说”、“溶剂说”二者都符合。文章的最后还提出了我们的工艺改进意见。     

多晶石墨材料中的微晶与人造金刚石的合成

本文测量了合成金刚石用的几种多晶石墨材料的微晶尺寸和石墨化程度。结果表明:样品的石墨化程度与微晶尺寸没有直接关系。用透射电镜观测到了人造多晶石墨材料中类金刚石结构的微晶的存在。静压法合成金刚石的结果表明:除去工艺方面的原因外,人工合成金刚石的晶粒大小与石墨材料中微晶的尺寸有关。     

铁基粉末触媒合成金刚石

本文利用六种铁基粉末触媒（FeNiNa,n=0,1,2,3,d,5X。代表Fe在触媒中的含量,Xn〉xn-1）在国产六面顶压机上进行了金刚石单晶的合成实验,研究了高温高压条件下（～6GPa,～1600℃）,铁基粉末触媒随铁含量的改变,石墨碳—铁基触媒体系合成金刚石条件的变化规律以及金刚石单晶的生长特性,利用穆斯堡尔谱对金刚石中铁元素形成的包裹体进行了检测．结果表明,随着铁基粉末触媒中铁含量的增加,合成金刚石的压力和温度条件逐渐增高,金刚石生长的“V形区”上移,同时得出了铁基粉末触媒适合高温区（110）和（111）面生长以及金刚石中铁元素以FeNi和FeyC形式存在的结论．     

高温高压下Fe-Ni-C-B系合成Ⅱb型金刚石单晶

提出了一种在高温高压下利用粉末冶金方法制备的Fe-Ni-C-B系触媒合金生长Ⅱb型金刚石的新方法. 由于硼元素的存在,Ⅱb型金刚石生长所需的温度和压力条件均高于普通的Ⅰb型金刚石,并且合成出的金刚石单晶粒度较粗,晶形稍差,表面结构比较复杂. 通过晶体的颜色、X射线衍射以及Raman光谱可以初步断定合成出的金刚石晶体中确实含有硼元素. 以金刚石在不同温度下的静压强度和冲击韧性以及差热分析和热重分析的结果来表征金刚石的热稳定性. 实验发现,由于硼元素的进入使得Ⅱb型金刚石单晶的热稳定性与采用同种方法合成出的Ⅰb型金刚石相比有了较大程度的提高. 采用自制的夹具通过检测金刚石的电阻温度特性,初步确定了在Fe-Ni-C-B系中生长的Ⅱb型金刚石具有半导体特性. 大量的实验数据充分说明,采用这种方法生产Ⅱb型金刚石具有成本低廉、操作简单、产品质量稳定等优点,具有极高的工业化推广应用的价值.     

Fe-Ni-C粉末触媒体系金刚石的合成与表征

利用FeNi粉末触媒在六面顶压机上进行工业金刚石单晶的合成与表征. 结果表明: 在Fe-Ni-C体系合成了优质的六面体、 六-八面体及八面体金刚石单晶; 金刚石{111}晶面的生长属于二维层状生长机制; 金刚石中的包裹体主要由FeNi合金组成.     

铁镍触媒合成金刚石内部包裹体的研究

分析铁镍触媒合成金刚石内部的包裹体成分及形成原因. 结果表明: 金刚石晶体中的包裹体主要以FeNi合金和Fe₃C形式存在; 随着生长速度加快, 金刚石内部包裹体的点状分布逐渐增多; 在不同温度下, 进入金刚石晶体内部包裹体的方式不同; 随着包裹体的增多, 合成的金刚石晶体硬度降低. 通过调整合成工艺, 合成了包裹体含量极少、 粒度约为0.6~0.7 mm的金刚石单晶.     

电镀晶种法合成金刚石单晶实验研究

目的寻求一种合成金刚石大单晶的有效方法。方法采用在金刚石单晶上面电镀一层金属镍膜作为触媒,镀有镍膜的金刚石晶种被规则地放在石墨片上预先刻好的洞中,每两个洞之间保持相等的间距,然后与其他石墨片交替组装在高温高压下进行实验合成。结果实验结果表明,在合成压力、温度和时间分别~5.8 GPa、~1 460℃和14 min的条件下,合成后的单晶尺寸约是原晶种的3倍。与传统的合成工艺相比较,合成后的金刚石单晶具有较好的形貌与质量。结论采用电镀晶种法合成对高品级金刚石大单晶的合成具有一定参考意义。     

类泡沫触媒合成金刚石的工艺特征

对触媒形状的变化关系与表面问题进行了研究．在制备类泡沫触媒的基础上，总结了类泡沫触媒在国产六面顶压机上合成金刚石的基本工艺规律，并对类泡沫触媒在六面顶压机上合成金刚石的适用范围进行了分析、确定．结果表明，增加石墨与触媒的接触面积或反应面积，是提高合成金刚石转化率的一条重要途径．     

碳加镍锰钴粉末触媒体系中B杂质对金刚石最低成核压力的影响

本文以国产JHY-Ⅲ型六面顶压机为合成设备,以Ni70Mn25Co5粉末触媒作为合成触媒,高纯鳞片石墨粉末做碳源,在合成压力4.6GPa到5.3GPa之间,合成温度1100℃到1200℃之间,合成时间300s的条件下合成金刚石样品。结果表明样品中随着硼含量的增加,金刚石的最低成核压力先降低,当添加0.75%时降至最低,然后随着硼含量的增加最低成核压力又开始升高;同时考察了不同压力、温度值对金刚石样品的影响规律,结果表明在相同的B掺杂比下随着合成压力的提高,合成腔体内金刚石的成核数增加,但晶形完整率下降,并且合成压力对含硼金刚石的颜色影响不大而合成温度是影响晶体中硼含量的主要因素。最后本文还考察了合成金刚石中包裹体的分布规律,证明了硼杂质进入金刚石时可能有着明显的生长区域的选择性这一重要规律。     

活性碳,碳黑,石墨与金刚石晶种的生长

介绍了活性碳、碳黑与石墨在过剩压驱动下金刚石晶种的生长．对两种无定形碳以及石墨在触媒中的分散溶解输运与再结晶进行了观察，对活性碳、碳黑在金刚石晶种生长中的机理作了探索性的讨论．三种碳片上的晶种均有明显长大，无定形碳作晶种生长的碳源是可行的     

Study on growth of coarse grains of diamond with high quality under HPHT

The growth of coarse grains of diamond was observed with graphite as carbon source and Fe₈₀Ni₂₀ alloy powder as catalyst at HPHT in a China-type SPD 6×1670T cubic high-pressure apparatus with highly exact control system. To synthesize coarse grains of diamond crystal with high quality, advanced indirect heat assembly, powder catalyst technology and catalyst with optimal granularity were used. Especially the nucleation of diamond and the growth rate were strictly controlled by the optimized synthesis craft. At last, diamond crystals (about 0.85 mm) in the perfect hex-octahedron shape were successfully synthesized at ~5.4 GPa and ~1360℃ in 60 min. The characteristic of crystal growth with powder catalyst technology under HPHT was discussed. The results and techniques might be useful for production of coarse grains of diamond.     

The nature and origin of interstellar diamond

Microscopic diamond was recently discovered in oxidized acid residues from several carbonaceous chondrite meteorites (for example, the C delta component of the Allende meteorite). Some of the reported properties of C delta seem in conflict with those expected of diamond. Here we present high spatial resolution analytical data which may help to explain such results. The C delta diamond is an extremely fine-grained (0.5-10 nm) single-phase material, but surface and interfacial carbon atoms, which may comprise as much as 25% of the total, impart an 'amorphous' character to some spectral data. These data support the proposed high-pressure conversion of amorphous carbon and graphite into diamonds due to grain-grain collisions in the interstellar medium although a low-pressure mechanism of formation cannot be ruled out.     

Diamond synthesis from a system of chromium-carbide and Ni70Mn25Co5 alloy

In order to ascertain the mechanism of interaction between carbide and metallic catalyst and formation of diamond under high pressure and high temperature, and find a new method to synthesize diamond with special properties, it is necessary to investigate the reaction behavior of different carbides and metallic solvent_catalysts under high pressure and high temperature. A system of Cr-3C-2 powder and Ni 70Mn 25Co 5 alloy in weight ratio of 1∶6 was treated under 6 0 GPa and 1 500℃ for 20, 30 or 60 min respectively. X_ray diffraction of the samples indicated the Cr 3C 2 decomposed partially after high pressure and temperature treatment, and Cr 7C 3, Cr and diamond formed respectively. There was not any trace of graphite in the samples. The result suggested that the separated carbon atoms could form diamond directly without conversion process of graphite into diamond. The observation of SEI, WDX and EDX also showed that diamond crystals were synthesized in the system, which have perfect surfaces and shapes, with the average grain size of about 40 μm. The properties of the crystals are being investigated.     

金刚石产品的脉冲激光制备与应用

详细介绍了用脉冲激光法制备金刚石产品的发展过程 ,并总结了脉冲激光沉积 (PLD)、液体靶脉冲激沉积 (LYPLD)以及脉冲激光诱导液 -固界面反应 (PLIIR)等几种典型的实验方法、实验装置以及所取得的成果 在脉冲激光沉积法 (PLD)制备金刚石薄膜方面重点总结了最近比较新颖的液体靶脉冲激光沉积技术 ,而在金刚石纳米晶的制备方面综述了脉冲激光诱导液 -固界面反应法 ,此法在制备亚稳态纳米晶体方面显示出了较独特的优越性 图 4,参 1 6     

Fe-Si-C体系合成金刚石的生长特性

研究高温高压下掺Si合成金刚石, 并与Fe-C体系合成的金刚石进行比较. 实验结果表明, 体系中掺入Si, 合成的晶体颜色比Fe-C体系合成的晶体颜色浅, 在相同的合成时间内, Fe-Si-C体系合成金刚石的粒度比Fe-C体系合成金刚石的粒度小; 通过X射线衍射(XRD)可见, 该体系产生FeSi和Fe₃C两种新物质.      

金刚石晶体生长研究进展

介绍利用高温高压（HPHT）合成高质量金刚石单晶和化学气相沉积法（CVD）制备金刚石薄膜的设备、方法、工艺参数以及热丝CVD和微波等离子体CVD的优缺点;P型和N型金刚石掺杂研制现状.重点介绍N型金刚石掺杂的困难,氮、锂、钠、磷、硫等杂质的掺杂效果,共掺杂对于金刚石薄膜的影响,以及近年来P型和N型掺杂取得的成果.     

山东郯城地区金刚石砂矿地质地貌特征

郯城金刚石砂矿属冲积层产状被破坏的阶地砂矿，金刚石产在残余二阶地冲积砂砾层中，金刚石颗粒大，宝石级金刚石较多，是宝石工业的重要原料基地。     

Preparation of high-performance ultrafine-grained AISI 304L stainless steel under high temperature and pressure

Bulk ultra-fine grained (UFG) AISI 304L stainless steel with excellent mechanical properties was prepared by a high-temperature and high-pressure (HTHP) method using nanocrystalline AISI 304L stainless steel powders obtained from ball milling. Samples were sintered in high-pressure conditions using the highest martensite content of AISI 304L stainless steel powders milled for 25 h. Analyses of phase composition and grain size were accomplished by X-ray diffraction and Rietveld refinement. By comparing the reverse martensite transformation under vacuum and HTHP treat, we consider that pressure can effectively promote the change in the process of transformation. Compared with the solid-solution-treated 304L, the hardness and yield strength of the samples sintered under HTHP are considerably higher. This method of preparation of UFG bulk stainless steel may be widely popularised and used to obtain UFG metallic materials with good comprehensive performance.