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Diamond is a kind of extremely functional material, which is widely used in the fields of industry, science and technology, military defense, medical and health, jewelry, and others. 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 is studied by adding B2S3 to the synthesis system using temperature gradient growth (TGG) method at a pressure of 6.5 GPa in this work. The growth rate of the synthesized diamond crystal decreases from 2.19 mg/h to 1.26 mg/h, indicating that the growth rate of diamond is dependent not only on the growth driving force, but also on the impurity element in the synthetic cavity. Additionally, with the increase of additive dosage, the color of the synthesized diamond crystal changes from yellow to baby blue . Raman measurement results indicate that the obtained diamond appears as a single sp3 hybrid phase without the sp3 hybrid graphite phase. However, the corresponding Raman characteristic peak of the as-grown diamond crystal is located at about 1331 cm–1 and tends to move towards low wave number. According to Fourier Transform Infrared Spectrometer (FTIR) measurement results, the absorption peaks at 1130 cm–1 and 1344 cm–1 are attributed to nitrogen defects. It is found that the nitrogen defect concentration of the synthesized diamond crystal decreases gradually from about 300×10–6 to 60×10–6. Furthermore, the electrical transport performance of the synthesized diamond is characterized by Hall effect measurement. Diamond has insulating properties due to the absence of any additives in the synthetic cavity. However, the results indicate that when B2S3 is introduced into the synthetic system as additive, there is almost no difference in carrier Hall mobility, but the difference in carrier concentration is as high as two orders of magnitude. Furthermore, the resistivity of the synthesized [111]-oriented diamond crystal decreases to 45.4 Ω·cm, due to the addition of B2S3 to 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 applying diamond to semiconductor field.
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Keywords:
- high pressure and high temperature /
- diamond /
- crystal defects
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图 1 金刚石高温高压合成的组装剖面示意图 1, 导电钢帽; 2, 白云石; 3, 石墨管; 4, 叶蜡石; 5, 石墨; 6, 触媒; 7, 籽晶; 8, 绝缘材料
Figure 1. Schematic diagram of the cell for diamond HPHT synthesis: 1, conductive ring; 2, dolomite; 3, graphite heater; 4, pyrophyllite; 5, carbon source; 6, catalyst; 7, seed crystal; 8, insulation materials.
图 2 温度梯度产生示意图
Figure 2. Schematic diagram of the temperature gradient generated.
图 3 金刚石样品光学照片 (a) 无添加剂; (b)添加0.01 g B2S3; (c) 添加0.03 g B2S3; (d) 添加0.002 g B2S3+钛/铜
Figure 3. Optical morphology of the synthesized diamond crystals: (a) Without any additive; (b) with 0.01 g B2S3 additive; (c) with 0.03 g B2S3 additive; (d) with 0.002 g B2S3 + Ti/Cu additives.
图 4 金刚石晶体Raman光谱
Figure 4. Raman spectra of the obtained diamond crystals.
图 5 金刚石样品FTIR光谱
Figure 5. FTIR spectra of the synthesized diamond crystals
表 1 金刚石合成实验参数
Table 1. Experimental parameters for diamond synthesis.
金刚石样品 B2S3/g 合成温度/℃ 生长时间/h 形貌 生长速率/(mg·h–1) 1 — 1330 21 六八面体 2.19 2 0.01 1330 21 六八面体 1.98 3 0.03 1325 21 六八面体 1.83 4 0.002+Ti/Cu 1335 21 六八面体 1.26 
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表 2 金刚石晶体Raman测试结果
Table 2. Raman measurement results of the synthesized diamond crystals.
金刚石样品 特征峰位/cm–1 FWHM/cm–1 内应力/MPa 1 1330.9 5.3370 382 2 1330.9 5.3175 382 3 1131.0 5.4276 347 4 1330.4 5.2285 555
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表 3 金刚石电输运性能参数
Table 3. Electric transport performance parameters of the obtained diamond crystals.
样品 B2S3/
g电阻率/
(Ω·cm)载流子浓度/
cm–3迁移率/
(cm–2·v–1·s–1)类型 1 — — — — — 2 0.01 8.98×10 6.63×1014 1.05×102 p 3 0.03 4.54×10 2.81×1014 4.88×102 p 4 0.002+Ti/Cu 4.33×10–1 3.39×1016 4.25×102 p
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