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在压力为5.56.2 GPa, 温度为12801450 ℃的条件下, 利用温度梯度法详细考察了氮氢协同掺杂对100晶面生长宝石级金刚石的影响. 实验结果表明伴随合成腔体内氮、氢浓度的升高, 合成条件明显升高, 金刚石生长V形区间上移; 晶体的红外光谱中与氮相关的吸收峰急剧增强, 氮含量可达2000 ppm, 同时位于2850 cm-1和2920 cm-1对应于 sp3杂化 CH 键的对称伸缩振动和反对称伸缩振动的红外特征峰逐渐增强, 表明晶体中既有高的氮含量, 同时又含有氢. 对晶体进行电镜扫描发现, 氮氢协同掺杂对晶体形貌影响明显, 出现拉长的{111}面, 且晶体表面上有三角形生长纹理. 拉曼测试表明, 晶体的峰位向高频偏移、半峰宽变大, 说明氮、氢杂质的进入对晶体内部产生了应力. 本文成功地以{100}晶面为生长面合成出高氮含氢宝石级金刚石单晶, 在探究氮氢共存环境下金刚石生长特性的同时, 也可为理解天然金刚石的形成机理提供帮助.As is well known, most natural diamonds usually contain not only aggregated nitrogen up to thousands of ppm but also hydrogen. Therefore, the studies of nitrogen and hydrogen impurities in a diamond are of interest for improving the physical properties of a diamond and solving the problems about natural diamond genesis. From this point of view, in this paper, we choose C3N6H6 powders as a nitrogen and hydrogen source and select high-quality seed crystals with {100} facets as the growth facets. The effects of nitrogen and hydrogen co-doped on {100}-oriented single diamond in the NiMnCo-C system at pressures ranging from 5.5 GPa to 6.2 GPa and temperatures of 1280-1450 ℃ are investigated. Experimental results show that both pressure and temperature, which are the synthesis conditions, increase with the increases of nitrogen and hydrogen content in diamond-growth environment, and the V-shape region of diamond-forming moves up. From the obtained Fourier transform infrared spectra, we notice that there is a significant change of the nitrogen concentration in the synthesized diamond with increasing the nitrogen and hydrogen content in the diamond-growth environment. We calculate the nitrogen concentrations in those diamonds and the results indicate that the highest concentration of nitrogen is up to 2000 ppm. Meanwhile, we notice that the hydrogen associated infrared peaks of 2850 and 2920 cm-1 are gradually enhanced, which shows that both nitrogen and hydrogen are successfully co-doped into the diamond. Scanning electron microscope micrographs show that the {111} face is elongated and has triangulated textures appearing on the surface with nitrogen and hydrogen co-doped into the diamond. This result indicates that the synergistic doping of nitrogen and hydrogen has a great influence on the morphology of {100}-oriented single diamond. From the obtained Raman spectra, we find a shift towards higher frequency of the Raman peak from 1330.23 cm-1 to 1330.40 cm-1 and the full width at half maximum increases from 3.12 cm-1 to 4.66 cm-1 with increasing the concentrations of nitrogen and hydrogen in diamond-growth environment. This is the first report about nitrogen and hydrogen co-doped on 100-oriented single diamond by far. This work can provide a new method to study the influences of nitrogen and hydrogen impurities on diamond synthesis and it will help us to further understand the genesis of natural diamond in the future.
[1] Chrenko R M, Mcdonald R S, Darrow K A 1967 Nature 213 474
[2] Kunuku S, Sankaran K J, Tsai C Y, Chang W H, Tai N H, Leou K C, Lin I N 2013 Appl. Mater. Interfaces 5 7439
[3] Kim Y D, Choi W, Wakimoto H, Usami S, Tomokage H, Ando T 1999 Appl. Phys. Lett. 75 3219
[4] Zhang W J, Meng X M, Chan C Y, Wu Y, Bello I, Lee S T 2003 Appl. Phys. Lett. 82 2622
[5] Liang Z Z, Kanda H, Jia X P, Ma H A, Zhu P W, Guan Q F, Zang C Y 2006 Carbon 44 913
[6] Woods G S 1984 Phil. Mag. B 50 673
[7] de Corte K, Cartigny P, Shatsky V S, de Paepe P, Sobolev N V, Javoy M 1999 In Proceeding of 7th International Kimberlite Conference Cape Town, South Africa, April 13-17, 1999 p174
[8] Evans T 1992 The Properties of Natural and Synthetic Diamond (London: Academic Press) pp259-290
[9] Zhang Z F, Jia X P, Liu X B, Hu M H, Li Y, Yan B M, Ma H A 2012 Chin. Phys. B 21 038103
[10] Zhang Y F, Zang C Y, Ma H A, Liang Z Z, Zhou L, Li S S, Jia X P 2008 Diam. Relat. Mater. 17 209
[11] Yu R Z, Ma H A, Liang Z Z, Liu W Q, Zheng Y J, Jia X P 2008 Diam. Relat. Mater. 17 180
[12] Palyanov Y N, Kupriyanov I N, Borzdov Y M, Sokol A G, Khokhryakov A F 2009 Cryst. Growth. Des. 9 2922
[13] Li Y, Jia X P, Hu M H, Liu X B, Yan B M, Zhou Z X, Zhang Z F, Ma H A 2012 Chin. Phys. B 21 058101
[14] Zhang Z F, Jia X P, Sun S S, Liu X B, Li Y, Yan B M, Ma H A 2013 Int. J. Refract. Met. Hard Mater. 38 111
[15] Sun S S, Jia X P, Yan B M, Wang F B, Chen N, Li Y D, Ma H A 2014 Cryst. Eng. Commun. 16 2290
[16] Fang C, Jia X P, Chen N, Zhou Z X, Li Y D, Li Y, Ma H A 2015 Acta Phys. Sin. 64 128101 (in Chinese) [房超, 贾晓鹏, 陈宁, 周振翔, 李亚东, 李勇, 马红安 2015 64 128101]
[17] Liang Z Z, Jia X P, Zang C Y, Zhu P W, Ma H A, Ren G Z 2005 Diam. Relat. Mater. 14 243
[18] Kanda H, Akaishi M, Yamaok S 1999 Diam. Relat. Mater. 8 1441
[19] Briddon P, Jones R, Lister G M S 1988 J. Phys. C: Solid State Phys. 21 L1027
[20] Yan B M, Jia X P, Qin J M, Sun S S, Zhou Z X, Fang C, Ma H A 2014 Acta Phys. Sin. 63 048101 (in Chinese) [颜丙敏, 贾晓鹏, 秦杰明, 孙士帅, 周振翔, 房超, 马红安 2014 63 048101]
[21] Connella S H, Sellschopa J P F, Butlerb J E, Macleara R D, Doylea B P, Machi I Z 1998 Diam. Relat. Mater. 7 1714
[22] Liu X B, Ma H A, Zhang Z F, Zhao M, Guo W, Li Y, Jia X P 2011 Diam. Relat. Mater. 20 468
[23] Zhang Z F, Jia X P, Liu X B, Hu M H, Li Y, Yan B M, Ma H A 2012 Sci. China: Phys. Mech. Astron. 55 781
[24] Wentorf Jr R H 1971 J. Phys. Chem. 75 1833
[25] Sumiya H, Toda N, Satoh S 2002 J. Crystal Growth 237-239 1281
[26] Kiflawi I, Kanda H, Mainwood A 1998 Diam. Relat. Mater. 7 327
[27] Burns R C, Hansen J O, Spits R A, Sibanda M, Welbourn C M, Welch D L 1999 Diam. Relat. Mater. 8 1433
[28] Zhou Z X, Jia X P, Li Y, Yan B M, Wang F B, Fang C, Chen N, Li Y D, Ma H A 2014 Acta Phys. Sin. 63 248104 (in Chinese) [周振翔, 贾晓鹏, 李勇, 颜丙敏, 王方标, 房超, 陈宁, 李亚东, 马红安 2014 63 248104]
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[1] Chrenko R M, Mcdonald R S, Darrow K A 1967 Nature 213 474
[2] Kunuku S, Sankaran K J, Tsai C Y, Chang W H, Tai N H, Leou K C, Lin I N 2013 Appl. Mater. Interfaces 5 7439
[3] Kim Y D, Choi W, Wakimoto H, Usami S, Tomokage H, Ando T 1999 Appl. Phys. Lett. 75 3219
[4] Zhang W J, Meng X M, Chan C Y, Wu Y, Bello I, Lee S T 2003 Appl. Phys. Lett. 82 2622
[5] Liang Z Z, Kanda H, Jia X P, Ma H A, Zhu P W, Guan Q F, Zang C Y 2006 Carbon 44 913
[6] Woods G S 1984 Phil. Mag. B 50 673
[7] de Corte K, Cartigny P, Shatsky V S, de Paepe P, Sobolev N V, Javoy M 1999 In Proceeding of 7th International Kimberlite Conference Cape Town, South Africa, April 13-17, 1999 p174
[8] Evans T 1992 The Properties of Natural and Synthetic Diamond (London: Academic Press) pp259-290
[9] Zhang Z F, Jia X P, Liu X B, Hu M H, Li Y, Yan B M, Ma H A 2012 Chin. Phys. B 21 038103
[10] Zhang Y F, Zang C Y, Ma H A, Liang Z Z, Zhou L, Li S S, Jia X P 2008 Diam. Relat. Mater. 17 209
[11] Yu R Z, Ma H A, Liang Z Z, Liu W Q, Zheng Y J, Jia X P 2008 Diam. Relat. Mater. 17 180
[12] Palyanov Y N, Kupriyanov I N, Borzdov Y M, Sokol A G, Khokhryakov A F 2009 Cryst. Growth. Des. 9 2922
[13] Li Y, Jia X P, Hu M H, Liu X B, Yan B M, Zhou Z X, Zhang Z F, Ma H A 2012 Chin. Phys. B 21 058101
[14] Zhang Z F, Jia X P, Sun S S, Liu X B, Li Y, Yan B M, Ma H A 2013 Int. J. Refract. Met. Hard Mater. 38 111
[15] Sun S S, Jia X P, Yan B M, Wang F B, Chen N, Li Y D, Ma H A 2014 Cryst. Eng. Commun. 16 2290
[16] Fang C, Jia X P, Chen N, Zhou Z X, Li Y D, Li Y, Ma H A 2015 Acta Phys. Sin. 64 128101 (in Chinese) [房超, 贾晓鹏, 陈宁, 周振翔, 李亚东, 李勇, 马红安 2015 64 128101]
[17] Liang Z Z, Jia X P, Zang C Y, Zhu P W, Ma H A, Ren G Z 2005 Diam. Relat. Mater. 14 243
[18] Kanda H, Akaishi M, Yamaok S 1999 Diam. Relat. Mater. 8 1441
[19] Briddon P, Jones R, Lister G M S 1988 J. Phys. C: Solid State Phys. 21 L1027
[20] Yan B M, Jia X P, Qin J M, Sun S S, Zhou Z X, Fang C, Ma H A 2014 Acta Phys. Sin. 63 048101 (in Chinese) [颜丙敏, 贾晓鹏, 秦杰明, 孙士帅, 周振翔, 房超, 马红安 2014 63 048101]
[21] Connella S H, Sellschopa J P F, Butlerb J E, Macleara R D, Doylea B P, Machi I Z 1998 Diam. Relat. Mater. 7 1714
[22] Liu X B, Ma H A, Zhang Z F, Zhao M, Guo W, Li Y, Jia X P 2011 Diam. Relat. Mater. 20 468
[23] Zhang Z F, Jia X P, Liu X B, Hu M H, Li Y, Yan B M, Ma H A 2012 Sci. China: Phys. Mech. Astron. 55 781
[24] Wentorf Jr R H 1971 J. Phys. Chem. 75 1833
[25] Sumiya H, Toda N, Satoh S 2002 J. Crystal Growth 237-239 1281
[26] Kiflawi I, Kanda H, Mainwood A 1998 Diam. Relat. Mater. 7 327
[27] Burns R C, Hansen J O, Spits R A, Sibanda M, Welbourn C M, Welch D L 1999 Diam. Relat. Mater. 8 1433
[28] Zhou Z X, Jia X P, Li Y, Yan B M, Wang F B, Fang C, Chen N, Li Y D, Ma H A 2014 Acta Phys. Sin. 63 248104 (in Chinese) [周振翔, 贾晓鹏, 李勇, 颜丙敏, 王方标, 房超, 陈宁, 李亚东, 马红安 2014 63 248104]
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