大颗粒硼皮金刚石聚晶的研制

本文利用一般生产的黄金刚石单晶作原料,或采取表面加硼处理,或在粘结剂中掺少量硼,使金刚石单晶表面蒙上硼原子层,同时强化粘结剂,在高温高压下进行了硼皮金刚石聚晶的研制,具有悬挂键的金刚石单晶表面,由于微量硼原子的引入,可能产生重构,从而可能改善聚晶的性能。实验结果表明,在高温高压下聚合成的这种大颗粒硼皮金刚石聚晶体的耐热性和磨耗比都大大提高,并且赶上了以含硼黑金刚石单晶为原料合成的大颗粒含硼黑金刚石聚晶,用它们做成的石油取心钻头,效果良好,初步的实验,取得了预期的效果。     

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.     

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     

聚晶用石墨发热体的煅烧温度对聚晶相对耐磨性的影响

本文通过对聚晶金刚石用石墨发热体煅烧后吸附及压缩性能的观测,对比了以煅烧和未煅烧石墨发热体合成聚晶金刚石的相对耐磨性,结果表明以煅烧后石墨发热体合成的聚晶金刚石的相对耐磨性比未煅烧者高几倍,最高相对磨耗比达10万以上,改善了聚晶金刚石的性能,同时也从一个侧面为制造合成聚晶金刚石专用石墨提供了依据。     

“单含硼”和“双含硼”黑金刚石合成的比较

我们将样品按两种不同的原料匹配方式(含硼触媒合金与不含硼石墨,简称“单含硼”;含硼触媒合金与含硼石墨,简称“双含硼”),分半对称地组装在同一高温高压反应腔中,研究了硼不同的含量和原子分布情况对高温高压合成含硼黑金刚石的影响。实验结果表明,“双含硼”方式得到的金刚石与“单含硼”相比不仅平均单产高,而且粗颗粒度比也高;硼原子可以增加金刚石单晶体的长大速度,因此可能缩短大颗粒单晶的合成时间,在高温范围内,“双含硼”方式得到的金刚石单晶有着增强抗氧化性能的趋势。     

石墨中渗钴的实验研究

本文报道作者用 CoCl_2·6H_2O 溶液浸泡石墨片渗钴使钴元素在高温高压前进入石墨的实验结果.实验用扫描电镜、x 射线能谱及透射电镜观察,证明钴已渗入到石墨片中.用该石墨片合成的金刚石产量和粒度比都有明显改善.从而验证了石墨在触媒作用下向金刚石转化的机理.     

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．     

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.     

纳米级晶种预涂层法Silicalite-1型沸石膜合成及其结构分析

在大孔-αA l2O3陶瓷管载体上采用晶种预涂层法在澄清溶液体系中水热合成了S ilica lite-1型沸石膜,用SEM和XRD表征了晶种、晶种涂层后载体和成膜后沸石膜的结构、晶形变化、晶相结构等成膜情况,并初步考查了两种不同温度(130℃和160℃)下生长成膜的结构变化.结果表明:制备的晶种呈椭球形、晶粒小(约100 nm)而均匀、纯度高,适合作晶种涂层成膜;所用载体孔径大而不均匀、表面粗糙而不平整,但经晶种涂层后表面可形成一层厚度均匀、光滑的晶种层,再水热晶化时有利于成膜,所得膜连续、清晰无裂缺,载体、晶种层和沸石膜层之间相互结合紧密;连续晶种层改善了载体表面的性能,有利于连续S ilica lite-1沸石膜的形成;合成温度不同,沸石晶粒在载体表面生长的方向不同,所形成的膜微观结构也不同.该合成方法能适合其他不同类型沸石膜的制备.     

丙酮对金刚石膜生长速率的影响

采用灯丝热解化学气相沉积方法，在不同的碳源气体气氛中合成金刚石薄膜，并研究不同工艺条件下的金刚石膜生长速率．结果表明，在较低的灯丝分解气体温度和较近的灯丝与衬底距离条件下，以丙酮为碳源气体合成的金刚石膜具有较高的生长速率和较好的质量．     

Synthesis of high quality type-Ib diamond crystals in carats grade

High quality type-Ib tower-shape gem-diamond crystals in carats grade were synthesized in cubic anvil high pressure apparatus (SPD-6×1200) at 5.4 GPa and 1250-1450°C. The relationship between the growth time and the weight of growth diamond has been gained. The faces of {110} and {113} were found in the synthetic diamond crystals frequently. We found that the relative growth rate of {113} face was descending with the increase of growth temperature, and that of {110} face had no obvious change with the incre...     

Effects of carbon diffusing field in alloy solvent on the growth of tower-shape diamond single crystal

High-quality type-Ib tower-shape diamond single crystals were synthesized in cubic anvil high pressure apparatus (SPD-6×1200) at 5.4 GPa and 1250-1450°C. The (100) face of seed crystal was used as the growth face, and FeNiMnCo alloy was used as the solvent/catalyst. Two kinds of carbon diffusing fields (type-B and type-G) were simulated by finite element method (FEM). Using the two kinds of carbon diffusing fields, many diamond single crystals were synthesized. The effects of carbon diffusing fields on the ...     

Growth and characterization of large, high quality cubic diamond crystals

High quality cubic diamond crystals were grown using the temperature gradient method at high pressure and high temperature(HPHT),in a new FeNi alloy as solvent.The crystals were grown at relatively low temperatures suitable for the growth of {100} faces.An increase in the radial growth rate,and inhibition of the axial growth caused the growth of large,high quality cubic diamond single crystals at high growth rates.For example,over 33 h,the radial growth rate was 0.22 mm/h,while the axial growth rate was only 0.08 mm/h;the growth rate by weight was also increased to 7.3 mg/h.The yellow color of our crystal samples was more uniform than samples from Sumitomo Corporation of Japan and Element Six Corp.The Raman FWHW of the 1332 cm 1 peak in our diamond sample was smaller than the Element Six Corp.sample,but larger than that of the Sumitomo Corp.sample.The nitrogen content of our diamond samples was 240 ppm,which was much higher than the Sumitomo and Element Six samples because of the higher growth rate of our diamond samples.     

MPCVD金刚石薄膜形貌与晶向

以甲烷、氢气做为气源,利用微波等离子气相沉积的方法在硅片上沉积金刚石薄膜。研究了不同浓度的甲烷对金刚石薄膜形貌和晶向的影响。结果表明:当甲烷浓度为2.44%时,金刚石薄膜晶粒尺寸小,晶形较差,晶面取向以(111)、(220)面为主;甲烷浓度为0.50%时,金刚石薄膜晶粒尺寸较大,晶粒棱角分明,晶面取向以(111)面为主。     

Effects of Ti additive on HPHT diamond synthesis in Fe-Ni-C system

Diamond crystals with low nitrogen concentration were synthesized from the Fe-Ni-C system with Ti additive at high pressure and high temperature （HPHT） in a china-type cubic high pressure apparatus （CHPA）. The synthesis pressure range was 4.8-5.2 GPa, and the temperature range was 1420-1600 K. The lowest synthesis pressure for diamond fell first and then rose with the increase of Ti additive. The color, shape, surface morphology and nitrogen impurity concentration of the synthesized diamond crystals were characterized using optical microscopy （OM）, scanning electron microscopy （SEM） and micro Fourier transform infrared （FTIR） spectrometry. The results show that the Ti additive has significant effects on color, growth rate, crystal shape, surface morphology and nitrogen impurity con- centration of the synthesized diamond crystals. The color of diamond crystals synthesized without Ti additive is yellow, while that with Ti additive becomes light and nearly colorless. The growth rate without Ti additive is higher than that with Ti additive. The crystal shapes of as-grown diamond crystals vary with the increase of Ti additive. The {111} crystal faces become dominant and some {311} crystal faces appear with the increase of Ti additive. The concentration of nitrogen impurity in diamond crystals without Ti additive is higher than that with Ti additive.     

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.     

钢基底上预镀中间层沉积金刚石膜

利用表面预镀中间层在４５号钢上化学气相沉积（ＣＶＤ）得到了金刚石膜。钢基底表面金刚石涂层具有许多潜在应用价值，但直接在钢上沉积生长金刚石面临长的形核期，铁原子的触媒作用和热膨胀不匹配等严重问题。文中采用钢基底表面预镀中间层的方法，阻止碳向基底中扩散，增强膜基结合和抑制ＳＰ２杂化碳的沉积。分别研究了直接在钢基底上、表面预镀铜膜和表面预镀硅膜钢基底上热丝法沉积金刚石膜的工艺特点。通过ＳＥＭ、Ｒａｍａｎ谱和划痕法检验表明，钢基底表面预镀硅膜作为中间层，是一种在钢上沉积金刚石膜的有效方法。     

在铁基底上以Au/Cu为过渡层沉积金刚石膜

采用热丝法化学气相沉积以碳纳米管为形核剂在Ａｕ／Ｃｕ 镀膜为过渡层的铁基底上沉积金刚石膜,研究了以Ａｕ／Ｃｕ 作为过渡层的铁基底上沉积金刚石膜质量的影响因素。试验结果表明, Ａｕ／Ｃｕ 过渡层可以在铁基底上沉积出质量很好的金刚石膜,涂料、基底预处理以及沉积工艺对金刚石膜质量的改善具有明显的作用。