叶蜡石高压同步辐射X射线衍射分析
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摘要
针对北京门头沟叶蜡石粉末进行了高压同步辐射X射线衍射分析,发现叶蜡石升压至15 GPa时(002)衍射峰消失,叶蜡石层状有序堆垛结构被破坏,其准等静压传压功能消失,因而确定其传压上限压力为15 GPa。叶蜡石在升压过程中晶格被压缩,卸压过程中发生回弹但始终处于被压缩状态,且压缩程度c轴最大、b轴次之、a轴最低。在金刚石合成压力(6 GPa)范围内,(002)晶面间距压缩率为3.76%,大于(020)和(200)晶面间距压缩率(1.26%);卸压时(200)晶面回弹率为0.6%～0.7%,高于(020)晶面的(0.1%～0.2%)。叶蜡石卸压过程中的密封性能与(002)、(200)晶面回弹效应密切相关。
High-pressure synchrotron radiation X-ray diffraction experiment on pyrophyllite powders of Mentougou in Bejing were carried out.It was found that the(002) peak of pyrophyllite was diminished when pressure up to 15 GPa,the layered orderly stacking structure of pyrophyllite was destroyed,so the iso-static pressure transmission properties of pyrophyllite decreased greatly and the upper limited pressure was determined to be 15 GPa.The crystal face spacing of high-pressure synchrotron radiation X-ray diffraction analysis results of pyrophyllite was compressed during the pressure uploading process,and resilienced but always in a compressed state during the pressure unloading process.The compression ratio of pyrophyllite in(002) crystal face was the maximum,next in(020) and finally in(200) face.Under the diamond synthesis pressure of 6 GPa,the compression ratio of pyrophyllite in(002) crystal face is 3.76% which is about 3 times greater than that of the(020) and(200) face of pyrophyllite,the ratio of pyrophyllite in(200) crystal face is about 0.6%～0.7%,which is much higher than that in(020) crystal face(0.1%～0.2%) under unloading process.Therefore the sealing function mainly depended on the rebounding property of(002) and(200) crystal face during unloading process.
High-pressure synchrotron radiation X-ray diffraction experiment on pyrophyllite powders of Mentougou in Bejing were carried out.It was found that the(002) peak of pyrophyllite was diminished when pressure up to 15 GPa,the layered orderly stacking structure of pyrophyllite was destroyed,so the iso-static pressure transmission properties of pyrophyllite decreased greatly and the upper limited pressure was determined to be 15 GPa.The crystal face spacing of high-pressure synchrotron radiation X-ray diffraction analysis results of pyrophyllite was compressed during the pressure uploading process,and resilienced but always in a compressed state during the pressure unloading process.The compression ratio of pyrophyllite in(002) crystal face was the maximum,next in(020) and finally in(200) face.Under the diamond synthesis pressure of 6 GPa,the compression ratio of pyrophyllite in(002) crystal face is 3.76% which is about 3 times greater than that of the(020) and(200) face of pyrophyllite,the ratio of pyrophyllite in(200) crystal face is about 0.6%～0.7%,which is much higher than that in(020) crystal face(0.1%～0.2%) under unloading process.Therefore the sealing function mainly depended on the rebounding property of(002) and(200) crystal face during unloading process.
引文
[1] 陶知耻.传压介质——叶蜡石及其在超高压高温下的密封机理[J].超硬材料工程,1995,7(2):5-11.Tao Zhichi.Pressure transmission medium-mechanism of pyrophyllite and its sealing edge under ultra-high pressure and high temperature[J].Superhard Material Engineering,1995,7(2):5-11
[2] 贾攀,卢灿华,郝兆印.叶蜡石密封性能及密封保温作用[J].超硬材料工程,2009,21(5):23-27.Jia Pan,Lu Canhua,Hao Zhaoyin.Properties and sealed heat insulation function of pyrophyllite[J].Superhard Material Engineering,2009,21(5):23-27.
[3] 杨炳飞,岳铁兵.我国传压、密封介质研究现状及进展[J].超硬材料工程,2005,17(3):43-45.Yang Bingfei,Yue Tiebing.Status and future of sealing and pressure transmission media[J].Superhard Material Engineering,2005,17(3):43-45
[4] 杨炳飞,冯安生,岳铁兵,等.叶蜡石在高压合成中作为密封传压介质的应用研究[J].矿产综合利用,2006,18 (1):35-39.Yang Bingfei,Feng Ansheng,Yue Tiebing,et al.The use of pyrophyllite as hermetical and pressure medium in high pressure synthesis[J].Multipurpose Utilization of Mineral Resource,2006,18(1):35-39.
[5] 徐文炘,李衡,郭陀珠,等.叶蜡石传压介质资源初步研究[J].矿产与地质,2003,17 (3):242-244.Xu Wenxin,Li Heng,Guo Tuozhu,et al.Mineral resouraces of pyrophyllite as stress conduction medium[J].Mineral Resouraces and Geology,2003,17 (3):242-244.
[6] 陈天虎,王道轩,方啸虎,等.合成金刚石生产中叶蜡石传压密封材料矿物学研究[J].矿物学报,2001,21(3):547-550.Chen Tianhu,Wang Daoxuan,Fang Xiaohu,et al.Mineralogical research on pyrophyllite-A pressure-transfer and sealing material in production of synthetic diamond[J].Acta Mineralogical Sinica,2001,21(3):547-550.
[7] 庞贵彬,苏桂.新型传压介质的研究[J].金刚石与磨料磨具工程,2001(4):32-33.Pang Guibin,Su Gui.Research on the pressure-transfer of pyrophyllite[J].Diamond Abrasives and Engineering,2001(4):32-33.
[8] 陶知耻,蒲正行.赵家台叶蜡石的品种类型、矿物相变及其对合成金刚石的影响[J].中国科学,1977(2):173-181.Tao Zhichi,Pu Zhengxing.Effects of variety types,mineral phase transitions of pyrophyllite on diamond syntheses in Zhaojiatai[J].Science of China,1977(2):173-181.
[9] 徐国平,郑日升,梁红原.叶蜡石的矿物成分对合成金刚石的影响[J].金刚石与磨料磨具工程,2005(2):64-66.Xu Guoping,Zheng Risheng,Liang Hongyuan.Study on mineral component of pyrophyllite on diamond sintering[J].Diamond Abrasives and Engineering,2005(2):64-66.
[10] 方啸虎,马万金,徐经苗,等.试谈高CaO高SiO2叶蜡石对金刚石合成金刚石工艺稳定性的影响[J].工业金刚石,2002 (1):16-18.Fang Xiaohu,Ma Wanjin,Xu Jingmiao,et al.Study on the stability of diamond synthesis process by pyrophyllite with high CaO high SiO2[J].Chinese Diamond,2002 (1):16-18.
[11] 王松顺.叶蜡石性质对金刚石合成技术的影响[J].珠宝科技,2003,15(3):19-22.Wang Songshun.Effect of diamond sintering technology on pyrophyllite[J].China Jewelry,2003,15(3):19-22.
[12] 汪洋,万隆,刘小磐,等.叶蜡石性能对合成金刚石的影响[J].超硬材料工程,2005,17(3):21-24.Wang Yang,Wan Long,Liu Xiaopan,et al.Effect of diamond sintering on pyrophyllite[J].Superhard Material Engineering,2005,17(3):21-24.
[13] 徐跃,陈晓东,郝兆印.高温高压叶蜡石相变的研究[J].金刚石与磨料磨具工程,2007(6):76-79.Xu Yue,Chen Xiaodong,Hao Zhaoyin.Research of phases transition of pyrophyllite after high pressure and high temperature[J].Diamond Abrasives and Engineering,2007(6):76-79.
[14] 李明达,刘光照,周军学.水促进的叶蜡石在超高压高温下的相转变及其对技术应用的影响[J].科学通报,1978,23(8):481-485.Li Mingda,Liu Guangzhao,Zhou Junxue.Study on water content for phases transfer of pyrophyllite on high pressure and high temperature sintering process[J].Chinese Science Bulletin,1978,23(8):481-485.
[15] 杨雪梅,赵玉成.真空低温焙烧叶蜡石对合成金刚石性能的影响[J].工业金刚石,2000(1):10-13.Yang Xuemei,Zhao Yucheng.Research on the properties of synthesized diamond with low temperature and vacuum[J].Chinese Diamond,2000(1):10-13.
[16] Hicks T L,Secco A S.Dehydration and decomposition of pyrophyllite at high pressures:electrical conductivity and X-ray diffraction studies to 5 GPa[J].Canadian Journal of Earth Sciences ,1997,34(6):875-882.
[17] Heege J H,Renner J.In situ impedance spectroscopy on pyrophyllite and CaCO3 at high pressure and temperature:phase transformations and kinetics of atomistic transport[J].Physics & Chemistry of Minerals,2007 ,34(7):445-465.
[18] 邓雯丽,邓福铭,杨雪峰,等.高温高压合成金刚石用叶蜡石腔体热导率研究[J].矿业科学学报,2018,3(3):284-289.Deng Wenli,Deng Fuming,Yang Xuefeng,et al.Research on thermal conductivity of compressed pyrophyllite block during diamond synthesis at HT/HP[J].Journal of Mining Science and Technology,2018,3(3):284-289.
[19] 郝兆印,贾攀,卢灿华,等.高压高温条件下叶蜡石的相变[J].金刚石与磨料磨具工程,2003(3):59-63.Hao Zhaoyin,Jia Pan,Lu Canhua,et al.Phases transformation of pyrophyllite under high pressure and high temperature[J].Diamond Abrasives and Engineering,2003(3):59-63.
[2] 贾攀,卢灿华,郝兆印.叶蜡石密封性能及密封保温作用[J].超硬材料工程,2009,21(5):23-27.Jia Pan,Lu Canhua,Hao Zhaoyin.Properties and sealed heat insulation function of pyrophyllite[J].Superhard Material Engineering,2009,21(5):23-27.
[3] 杨炳飞,岳铁兵.我国传压、密封介质研究现状及进展[J].超硬材料工程,2005,17(3):43-45.Yang Bingfei,Yue Tiebing.Status and future of sealing and pressure transmission media[J].Superhard Material Engineering,2005,17(3):43-45
[4] 杨炳飞,冯安生,岳铁兵,等.叶蜡石在高压合成中作为密封传压介质的应用研究[J].矿产综合利用,2006,18 (1):35-39.Yang Bingfei,Feng Ansheng,Yue Tiebing,et al.The use of pyrophyllite as hermetical and pressure medium in high pressure synthesis[J].Multipurpose Utilization of Mineral Resource,2006,18(1):35-39.
[5] 徐文炘,李衡,郭陀珠,等.叶蜡石传压介质资源初步研究[J].矿产与地质,2003,17 (3):242-244.Xu Wenxin,Li Heng,Guo Tuozhu,et al.Mineral resouraces of pyrophyllite as stress conduction medium[J].Mineral Resouraces and Geology,2003,17 (3):242-244.
[6] 陈天虎,王道轩,方啸虎,等.合成金刚石生产中叶蜡石传压密封材料矿物学研究[J].矿物学报,2001,21(3):547-550.Chen Tianhu,Wang Daoxuan,Fang Xiaohu,et al.Mineralogical research on pyrophyllite-A pressure-transfer and sealing material in production of synthetic diamond[J].Acta Mineralogical Sinica,2001,21(3):547-550.
[7] 庞贵彬,苏桂.新型传压介质的研究[J].金刚石与磨料磨具工程,2001(4):32-33.Pang Guibin,Su Gui.Research on the pressure-transfer of pyrophyllite[J].Diamond Abrasives and Engineering,2001(4):32-33.
[8] 陶知耻,蒲正行.赵家台叶蜡石的品种类型、矿物相变及其对合成金刚石的影响[J].中国科学,1977(2):173-181.Tao Zhichi,Pu Zhengxing.Effects of variety types,mineral phase transitions of pyrophyllite on diamond syntheses in Zhaojiatai[J].Science of China,1977(2):173-181.
[9] 徐国平,郑日升,梁红原.叶蜡石的矿物成分对合成金刚石的影响[J].金刚石与磨料磨具工程,2005(2):64-66.Xu Guoping,Zheng Risheng,Liang Hongyuan.Study on mineral component of pyrophyllite on diamond sintering[J].Diamond Abrasives and Engineering,2005(2):64-66.
[10] 方啸虎,马万金,徐经苗,等.试谈高CaO高SiO2叶蜡石对金刚石合成金刚石工艺稳定性的影响[J].工业金刚石,2002 (1):16-18.Fang Xiaohu,Ma Wanjin,Xu Jingmiao,et al.Study on the stability of diamond synthesis process by pyrophyllite with high CaO high SiO2[J].Chinese Diamond,2002 (1):16-18.
[11] 王松顺.叶蜡石性质对金刚石合成技术的影响[J].珠宝科技,2003,15(3):19-22.Wang Songshun.Effect of diamond sintering technology on pyrophyllite[J].China Jewelry,2003,15(3):19-22.
[12] 汪洋,万隆,刘小磐,等.叶蜡石性能对合成金刚石的影响[J].超硬材料工程,2005,17(3):21-24.Wang Yang,Wan Long,Liu Xiaopan,et al.Effect of diamond sintering on pyrophyllite[J].Superhard Material Engineering,2005,17(3):21-24.
[13] 徐跃,陈晓东,郝兆印.高温高压叶蜡石相变的研究[J].金刚石与磨料磨具工程,2007(6):76-79.Xu Yue,Chen Xiaodong,Hao Zhaoyin.Research of phases transition of pyrophyllite after high pressure and high temperature[J].Diamond Abrasives and Engineering,2007(6):76-79.
[14] 李明达,刘光照,周军学.水促进的叶蜡石在超高压高温下的相转变及其对技术应用的影响[J].科学通报,1978,23(8):481-485.Li Mingda,Liu Guangzhao,Zhou Junxue.Study on water content for phases transfer of pyrophyllite on high pressure and high temperature sintering process[J].Chinese Science Bulletin,1978,23(8):481-485.
[15] 杨雪梅,赵玉成.真空低温焙烧叶蜡石对合成金刚石性能的影响[J].工业金刚石,2000(1):10-13.Yang Xuemei,Zhao Yucheng.Research on the properties of synthesized diamond with low temperature and vacuum[J].Chinese Diamond,2000(1):10-13.
[16] Hicks T L,Secco A S.Dehydration and decomposition of pyrophyllite at high pressures:electrical conductivity and X-ray diffraction studies to 5 GPa[J].Canadian Journal of Earth Sciences ,1997,34(6):875-882.
[17] Heege J H,Renner J.In situ impedance spectroscopy on pyrophyllite and CaCO3 at high pressure and temperature:phase transformations and kinetics of atomistic transport[J].Physics & Chemistry of Minerals,2007 ,34(7):445-465.
[18] 邓雯丽,邓福铭,杨雪峰,等.高温高压合成金刚石用叶蜡石腔体热导率研究[J].矿业科学学报,2018,3(3):284-289.Deng Wenli,Deng Fuming,Yang Xuefeng,et al.Research on thermal conductivity of compressed pyrophyllite block during diamond synthesis at HT/HP[J].Journal of Mining Science and Technology,2018,3(3):284-289.
[19] 郝兆印,贾攀,卢灿华,等.高压高温条件下叶蜡石的相变[J].金刚石与磨料磨具工程,2003(3):59-63.Hao Zhaoyin,Jia Pan,Lu Canhua,et al.Phases transformation of pyrophyllite under high pressure and high temperature[J].Diamond Abrasives and Engineering,2003(3):59-63.
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