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金刚石是一种用途极为广泛的极限功能材料，本研究在6.5 GPa压力条件下，利用温度梯度法研究了合成腔体中添加三硫化二硼(B2S3)时金刚石大单晶的合成.随着B2S3的添加，所合成金刚石的颜色由典型的黄色变为了浅蓝色，而且金刚石的生长速率也随之降低.拉曼(Raman)测试表明所制备样品为单一的sp3杂化金刚石相，但对应的Raman特征峰均趋于向低波数移动.借助傅里叶显微红外光谱(FTIR)测试结果，分析发现金刚石内部氮杂质浓度逐渐降低.此外，利用霍尔效应测试表征了所合成金刚石的电输运性能，结果表明B2S3可将(111)晶向金刚石电阻率降低至45.4 Ω·cm.然而，当合成体系中同时添加0.002 g B2S3和除氮剂时，对应金刚石晶体的电阻率锐减至0.43 Ω·cm，该研究为金刚石在半导体领域中的应用提供了重要的实验依据.Diamond is a kind of ultimate functional material, which is widely used in industry, science and technology, military defense, medical and health, jewelry and other fields. However, its application in the semiconductor field is still limited, because its electrical transport performance has not yet met the requirements of semiconductor devices. In order to improve the electrical transport performance of diamond as much as possible, the synthesis of diamond single crystal was studied with B2S3 additive in the synthesis system by temperature gradient growth (TGG) method at pressure of 6.5 GPa condition in this work. The growth rates of the synthesized diamond crystals reduced from 2.19 mg/h to 1.26 mg/h, indicating that the growth rate of diamond not only depended on the growth driving force, but also affected by the impurity elements in the synthetic cavity. Additionally, the colors of the synthesized diamond crystals transformed from yellow to baby blue, accompanying with the increase in the amount of additives added. Raman measurement results indicated that the obtained diamond appeared as a single sp3 hybrid phase without the sp3 hybrid graphite phase. However, the corresponding Raman characteristic peaks of the as-grown diamond crystals located at about 1331 cm-1 and consistently tended to move towards low wave number. According to FTIR measurement results, the absorption peaks at 1130 cm-1 and 1344 cm-1 attributed to nitrogen defects. It was found that the nitrogen defect concentrations of the synthesized diamond crystals decreased gradually from about 300 ppm to 60 ppm. Furthermore, the electrical transport performance of the synthesized diamond was characterized by Hall effects measurement. Diamond had an insulating behavior due to the absence of any additives in the synthetic cavity. However, the result showed that there was little difference in carrier hall mobility, but there was a difference of two orders of magnitude in carrier concentration, when B2S3 was introduced into the synthetic system as additive. Furthermore, the resistivity of the synthesized [111]-oriented diamond crystal reduced to 45.4 Ω·cm, due to the addition of B2S3 additive in the synthesis system. However, it is worth noting that the resistivity of the diamond crystal synthesized with 0.002 g B2S3 and Ti/Cu additives in the synthesis system drops sharply to 0.43 Ω·cm. Therefore, the nitrogen defects in diamond will have an important effect on its conductivity. It provides an important experimental basis for the application of diamond in semiconductor field.
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Keywords:
- high pressure and high temperature /
- diamond /
- crystal defects
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