高氮含量宝石级金刚石的合成
摘要
氮是金刚石中最主要的杂质元素,天然金刚石含氮量约为2×103ppm,多为无色(Ia型):而人工合成金刚石的含量仅仅约为300ppm,为黄色(Ib型)。两种金刚石在氮浓度及存在形式上有很大差异,导致了两种金刚石的诸多性质不同。合成具有完整晶型的高氮含量金刚石能提供一种人工合成类“天然”金刚石和“硼皮氮芯”金刚石的开创性技术。更为重要的是这一突破能使人们对天然金刚石的形成机制有一个更新的认识。本实验室前期已经通过添加NaN3使用粉末触媒合成出了氮含量与天然金刚石相当的工业级金刚石。然而,工业级金刚石颗粒毕竟尺寸有限,一般粒径只有O.5mm左右,这与天然金刚石颗粒还是有着相当大的距离的。此外由于粒径较小,也限制了高氮金刚石在诸多方面的应用。因此在此基础上对高温高压条件下合成高氮含量的大尺寸宝石级金刚石进行研究有着十分重要的意义。
本文使用国产六面项压机,首次用不同触媒(FeNiMnCo、FeNiCo)+C+不同比例的添加剂NaN3合成出具有完整晶型的优质深绿色高氮含量宝石级金刚石单晶,研究了NaN3对宝石级金刚石中氮含量及生长行为的影响。
为了进一步考察NaN3的添加对于晶体生长的影响,我们借助扫描电镜的手段对晶体的形貌进行了研究。随着NaN3的加入,晶体逐渐向富{111}晶面形态转变,此时晶体表面也逐渐趋于平滑,很少出现熔坑等缺陷。当NaN3的添加比例进一步提高时,晶体表面开始出现一系列的相互平行的凹槽。当NaN3的添加比例提高到0.6wt%时,晶体表面出现了不规则分布的三角形凹坑,以及大量不规则形状的凸台。
综上所述,本文通过对高氮含量宝石级金刚石合成的研究,找到了生长优质高氮晶体的有效手段。并首次合成出了含氮量达1707ppm的宝石级金刚石单晶。合成出尺寸达3.2mm含氮量达1520ppm的优质晶体。
It is well known that nitrogen is one of the most common impurities in industry and natural diamond. In natural diamond the concentration of nitrogen is commonly about 2×103 ppm, mostly colorless (type Ia), but the synthetic diamond is only about 300ppm, yellow (type Ib). There are so significant differences in nitrogen concentration and form between the two type diamond. It cause a lot of differences in properties. Syntheses of diamond with a high concentration of nitrogen in laboratory provide a means for fabricating diamond with nitrogen concentration and form similar to those of the natural diamond and for fabricating diamond with "boron skin and nitrogen core". Furthermore, these can provide new knowledge of mechanisms for natural diamond nucleation and growth. It should be helpful for future study toward the understanding of how nitrogen atoms accommodate themselves in the synthetic diamond, and how high concentrations of nitrogen eventually become platelets or tetrahedron in the natural diamond. In our previous studies, using powder catalyst and NaN3 as an addition, we have already synthesized industrial diamond with a considerable nitrogen content of natural diamond. However, industrial-grade diamond particulate's size is limited, and the general size is only about 0.5mm. There is still a distance with natural diamonds. In addition due to the smaller size also limits the applications of high nitrogen content diamonds. Therefore, it is very important to study on high nitrogen content diamond synthesis in HPHT condition.
In this study, we use a cubic anvil HPHT apparatus. Using catalysts (FeNiMnCo, FeNiCo), graphite and addition of NaN3, large green single crystal diamond with high nitrogen concentration is firstly synthesized by temperature gradient method. We have studied the NaN3 effect on the nitrogen contents and growth of gem diamond.
In order to further study the impact of the addition of NaN3 to crystal growth, we used SEM to study the surface morphology of crystals. With the addition of NaN3, crystal gradually changed to (111) crystal plane rich patterns, at the same time the crystal surface became more and more smooth, rarely occurred defects such as melt pit. When the addition of NaN3 further improved, the crystal surface began to appear a series of parallel grooves. As the addition of NaN3 reached 0.6wt%, the crystal surface was irregularly distributed lots of triangular pits and irregular-shaped steps.
Above all, through the research on high nitrogen content gem diamond synthesis, we found a effective means to synthesize high-quality high-nitrogen diamond. synthetic crystals reached the maximum nitrogen content 1707ppm.
本文使用国产六面项压机,首次用不同触媒(FeNiMnCo、FeNiCo)+C+不同比例的添加剂NaN3合成出具有完整晶型的优质深绿色高氮含量宝石级金刚石单晶,研究了NaN3对宝石级金刚石中氮含量及生长行为的影响。
为了进一步考察NaN3的添加对于晶体生长的影响,我们借助扫描电镜的手段对晶体的形貌进行了研究。随着NaN3的加入,晶体逐渐向富{111}晶面形态转变,此时晶体表面也逐渐趋于平滑,很少出现熔坑等缺陷。当NaN3的添加比例进一步提高时,晶体表面开始出现一系列的相互平行的凹槽。当NaN3的添加比例提高到0.6wt%时,晶体表面出现了不规则分布的三角形凹坑,以及大量不规则形状的凸台。
综上所述,本文通过对高氮含量宝石级金刚石合成的研究,找到了生长优质高氮晶体的有效手段。并首次合成出了含氮量达1707ppm的宝石级金刚石单晶。合成出尺寸达3.2mm含氮量达1520ppm的优质晶体。
It is well known that nitrogen is one of the most common impurities in industry and natural diamond. In natural diamond the concentration of nitrogen is commonly about 2×103 ppm, mostly colorless (type Ia), but the synthetic diamond is only about 300ppm, yellow (type Ib). There are so significant differences in nitrogen concentration and form between the two type diamond. It cause a lot of differences in properties. Syntheses of diamond with a high concentration of nitrogen in laboratory provide a means for fabricating diamond with nitrogen concentration and form similar to those of the natural diamond and for fabricating diamond with "boron skin and nitrogen core". Furthermore, these can provide new knowledge of mechanisms for natural diamond nucleation and growth. It should be helpful for future study toward the understanding of how nitrogen atoms accommodate themselves in the synthetic diamond, and how high concentrations of nitrogen eventually become platelets or tetrahedron in the natural diamond. In our previous studies, using powder catalyst and NaN3 as an addition, we have already synthesized industrial diamond with a considerable nitrogen content of natural diamond. However, industrial-grade diamond particulate's size is limited, and the general size is only about 0.5mm. There is still a distance with natural diamonds. In addition due to the smaller size also limits the applications of high nitrogen content diamonds. Therefore, it is very important to study on high nitrogen content diamond synthesis in HPHT condition.
In this study, we use a cubic anvil HPHT apparatus. Using catalysts (FeNiMnCo, FeNiCo), graphite and addition of NaN3, large green single crystal diamond with high nitrogen concentration is firstly synthesized by temperature gradient method. We have studied the NaN3 effect on the nitrogen contents and growth of gem diamond.
In order to further study the impact of the addition of NaN3 to crystal growth, we used SEM to study the surface morphology of crystals. With the addition of NaN3, crystal gradually changed to (111) crystal plane rich patterns, at the same time the crystal surface became more and more smooth, rarely occurred defects such as melt pit. When the addition of NaN3 further improved, the crystal surface began to appear a series of parallel grooves. As the addition of NaN3 reached 0.6wt%, the crystal surface was irregularly distributed lots of triangular pits and irregular-shaped steps.
Above all, through the research on high nitrogen content gem diamond synthesis, we found a effective means to synthesize high-quality high-nitrogen diamond. synthetic crystals reached the maximum nitrogen content 1707ppm.
引文
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