CVD合成钻石工艺中种晶预处理及其后期处理研究进展
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摘要
由于钻石产量无法满足各领域对其的需求,主流的人工合成钻石方法之一——CVD合成钻石法开始出现并不断发展,其工艺是研究重点之一。CVD合成钻石中生长前处理以及生长完成后的改色处理是CVD合成钻石处理中很重要的两个方面。生长之前的种晶预处理对种晶来说是直接影响钻石成长质量的重要因素,预处理主要使用强酸煮种晶除杂、丙酮清洗除杂、酒精及去离子水除杂等工艺。生长后样品的处理是目前提高CVD钻石宝石价值的必要步骤。生长后使用等离子体刻蚀除去晶质较差以及非钻石相十分有效。在CVD钻石改色方面,目前出现的主流方法有辐照改色处理,HPHT处理和LPHT处理。
Since the production of diamond can not meet the demand in various fields,CVD synthetic diamond method,one of the mainstream synthetic diamond methods,emerged and developed.The pretreatment of CVD synthetic diamond and the color modification after growth are two important aspects of processed CVD synthetic diamonds.The pretreatment of seed crystals before growth is an important factor directly affecting diamond growth quality.It mainly uses strong acid to boil seed crystal to remove impurities,acetone to clean,and alcohol and deionized water to remove and so on.The treatment of grown samples is a necessary step to improve the value of CVD diamonds.After growth,plasma etching is very effective to remove poor crystals and non-diamond phase.In the field of CVD diamond color modification,the current mainstream methods are radiation modification,HPHT treatment,and LPHT treatment.
Since the production of diamond can not meet the demand in various fields,CVD synthetic diamond method,one of the mainstream synthetic diamond methods,emerged and developed.The pretreatment of CVD synthetic diamond and the color modification after growth are two important aspects of processed CVD synthetic diamonds.The pretreatment of seed crystals before growth is an important factor directly affecting diamond growth quality.It mainly uses strong acid to boil seed crystal to remove impurities,acetone to clean,and alcohol and deionized water to remove and so on.The treatment of grown samples is a necessary step to improve the value of CVD diamonds.After growth,plasma etching is very effective to remove poor crystals and non-diamond phase.In the field of CVD diamond color modification,the current mainstream methods are radiation modification,HPHT treatment,and LPHT treatment.
引文
[1]吴冰欣.甲烷浓度对金刚石单晶生长的影响和金刚石刻蚀坑的研究[D].吉林大学,2015.
[2] BUNDYF P.The P-T Phase and Reaction Diagram For Elemental Carbon[J].J.Geophys.Res,1979,85(B12):6930-6936.
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[4] Mokuno Y,Chayahara A,Hyamada.Synthesis of large single crystaldiamond plates by highrate homoepitaxial growth using microwaveplasma CVD and lift-off process[J].Diamond and Related Materials,2008,17(4-5):415-418.
[5] Dollet A.Multiscale modeling of CVD film growth--a review ofrecent work[J].Surface andCoatings Technology,2004,177-178:245-251.
[6]李明吉.大尺寸高质量金刚石厚膜制备及氮掺杂对金刚石膜生长的影响研究[D].吉林大学,2006.
[7]周建.微波等离子体化学气相沉积法制备高质量金刚石膜研究[D].武汉理工大学,2002.
[8]舒兴胜,邬钦崇,梁荣庆.氧气对MWPCVD制备金刚石膜的影响[J].真空科学与技术,2001(4):25-28+34.
[9] Fan W Y,R?倠pcke J,Davies P B.Effect of oxygen on methyl radical concentrations in a CH4/H2chemical vapor deposition reactor studied by infrared diode laser spectroscopy[J].Journal of Vacuum Science&Technology A Vacuum Surfaces&Films,1996,14(5):2970-2972.
[10] Tallaire A,Achard J,Silva F,et al.Growth of large size diamond single crystals by plasma assisted chemical vapour deposition:Recent achievements and remainingchallenges[J].Comptes Rendus Physique,2013,14(2):169-184.
[11] Yamamoto M,Teraji T,Ito T.Improvement in the crystalline qualityof homoepitaxial diamond films by oxygen plasma etching of mirror-polished diamond substrates[J].Journal of Crystal Growth,2005,285(1-2):130-136.
[12] Friel S L,Clewes H K,Dhillon,et al.Control of surface and bulkcrystalline quality in single crystal diamond grown by chemical vapourdeposition[J].Diamond and Related Materials,2009,18(5-8):808-815.
[13] Geis M W,Smith H I,Argoitia A,et al.Large-area mosaic diamond films approaching single-crystal quality[J].Applied Physics Letters,1991,58(22):2485-2487.
[14] Janssen G,Giling L J.“Mosaic”growth of diamond[J].Diamond and related materials,1995,4(7):1025-1031.
[15] Findeling-Dufour C,Gicquel A,Chiron R.Growth of large single-crystal diamond layers:analysis of the junctions between adjacent diamonds[J].Diamond and related materials,1998,7(7):986-998.
[16] Yamada H,Chayahara A,Mokuno Y,et al.Developments of elemental technologies to produce inch-size single-crystal diamond wafers[J].Diamond and Related materials,2011,20(4):616-619.
[17]Hideaki Yamada,Akiyoshi Chayahara,Hitoshi Umezawa,NobuteruTsubouchi,YoshiakiMokuno,Shinichi Shikata.Fabrication and fundamental characterizations of tiled clones of single-crystal diamond with 1-inch size[J].Diamond&Related Materials,2012,24.
[18]舒国阳.Mosaic拼接法高质量大尺寸单晶金刚石生长研究[D].哈尔滨工业大学,2016.
[19] DORSCH O,WERNER M,OBERNEIER E,et al.Etching of polycrystallinediamond andamorphous carbon films by RIE[J].Diamond and Ralated Materials,1992,1(2-4):277-280.
[20] DORSCH O,WERNER M,OBERMEIER E,et al.Dry etching of undoped and boron doped polycrystalline diamond films[J].Diamond and Ralated Materials,1995,4(4):456-459.
[21] SIRINENI GMR,NASEEM HA,MALSHE AP.Reactive ion etching of diamond as a means of enhancing chemically-assisted mechanical polishing efficiency[J].Diamond and Relatedmaterials,1997,6(1):952-958.
[22] ENLUND J,ISBERG J.Anisotropic dry etching of boron doped single crystal CVD diamond[J].Carbon,2009,43(12):1839-1842.
[23]吕宪义,金曾孙,郝世强,等.氧等离子体对金刚石膜的刻蚀研究[J].新型炭材料,2003,18(3):191-194.
[24]李德贵,冉均国,廖晓明,等.空气等离子体刻蚀对金刚石薄膜性能的影响[J].微细加工技术,2006(2):30-32.
[25]郑先锋,马志斌,张磊,等.直流辉光氧等离子体刻蚀金刚石膜的研究[J].金刚石与磨料磨具工程,2007(1):35-38.
[26]戴安娜彩钻公司主页[EB/OL].http://www.Diane diamond.com.2016-02-05.
[27]王五一.天然、处理和合成粉红色——红色钻石颜色形成机制及其鉴别[A].国家珠宝玉石质量监督检验中心(National Gemstone Testing Center)、中国珠宝玉石首饰行业协会.2009中国珠宝首饰学术交流会论文集[C].国家珠宝玉石质量监督检验中心(National Gemstone Testing Center)、中国珠宝玉石首饰行业协会:,2009:2.
[28]张彩慧,陈美华.电子辐照产生蓝色钻石的工艺条件探索[J].宝石和宝石学杂志,2016,18(4):10-15.
[29] K.M.Chadwick.HPHT-Treated CVD synthetic diamond submitted for grading[J].G&G 44,365-367(2008).(Winter2008,Lab notes)
[30] D.J.Twitchen,P.M.Martineau,G.A.Scarsbrook.Colored diamond,US patent#7172655[P].filed in 2003,2003.
[31] Charles S J,Butler J E,Feygelson B N,et al.Characterization of nitrogen doped chemical vapor deposited single crystal diamond before and after high pressure,high temperature annealing[M]//Explaining the mental:Cambridge Scholars Pub.2004:2473-2485.
[32] R.H.Frushour,W.Li.Method of making enhanced CVD diamond,US patent#6811610[P],issued in 2004,2002.
[33] Qi Liang,Chih-shiue Yan,Yufei Meng,et al.Recent advances in high-growth rate single-crystal CVD diamond[J].Diamond and Related Materials,2009,18(5–8):698-703.
[34]Kyaw Soe Moe,Ulrika D’Haenens-Johansson,and Wuyi Wang.LPHT-Annealed Pink CVD SYNTHETIC DIAMONDS[J].GEMS&GEMOLOGY,SUMMER 2015.
[35] D'Haenensjohansson U F S,Edmonds A M,Newton M E,et al.EPR of a defect in CVD diamond involving both silicon and hydrogen that shows preferential alignment[J].Physical Review B,2010,82(15):155205.
[36] Glover C,Newton M E,Martineau P M,et al.Hydrogen incorporation in diamond:the vacancy-hydrogen complex.[J].Physical Review Letters,2004,92(13):135502.
[37] Tallaire A,Achard J,Brinza O,et al.Growth strategy for controlling dislocation densities and crystal morphologies of single crystal diamond by using pyramidal-shape substrates[J].Diamond&Related Materials,2013,33(3):71-77.
[38] Field J E,Nicholson E,Seward C R,et al.Strength,fracture and erosion properties of cvd diamond[M]//Thin Film Diamond.Springer Netherlands,1994:261-275.
[39] Qi Liang,Chih-shiue Yan,Yufei Meng,et al.Recent advances in high-growth rate single-crystal CVD diamond[J].Diamond and Related Materials,2009,18(5–8):698-703.
[40] Zaitsev S A M.Optical Properties of Diamond[M].Springer Berlin Heidelberg,2001.
[41] Meng Y F,Yan C S,Lai J,et al.From the Cover:Enhanced optical properties of chemical vapor deposited single crystal diamond by low-pressure/high-temperature annealing:National Acad Sciences,US20100104494[P].2010.
[42] Glover C,Newton M E,Martineau P M,et al.Hydrogen incorporation in diamond:the vacancy-hydrogen complex[J].Physical Review Letters,2004,92(13):135502.
[43] Meng Y F,Yan C S,Lai J,et al.From the Cover:Enhanced optical properties of chemical vapor deposited single crystal diamond by low-pressure/high-temperature annealing:National Acad Sciences,US20100104494[P].2010.
[2] BUNDYF P.The P-T Phase and Reaction Diagram For Elemental Carbon[J].J.Geophys.Res,1979,85(B12):6930-6936.
[3]朱金凤,满卫东,吕继磊,等.同质外延单晶CVD金刚石的研究进展[J].金刚石与磨料磨具工程,2011,31(4):15-22.
[4] Mokuno Y,Chayahara A,Hyamada.Synthesis of large single crystaldiamond plates by highrate homoepitaxial growth using microwaveplasma CVD and lift-off process[J].Diamond and Related Materials,2008,17(4-5):415-418.
[5] Dollet A.Multiscale modeling of CVD film growth--a review ofrecent work[J].Surface andCoatings Technology,2004,177-178:245-251.
[6]李明吉.大尺寸高质量金刚石厚膜制备及氮掺杂对金刚石膜生长的影响研究[D].吉林大学,2006.
[7]周建.微波等离子体化学气相沉积法制备高质量金刚石膜研究[D].武汉理工大学,2002.
[8]舒兴胜,邬钦崇,梁荣庆.氧气对MWPCVD制备金刚石膜的影响[J].真空科学与技术,2001(4):25-28+34.
[9] Fan W Y,R?倠pcke J,Davies P B.Effect of oxygen on methyl radical concentrations in a CH4/H2chemical vapor deposition reactor studied by infrared diode laser spectroscopy[J].Journal of Vacuum Science&Technology A Vacuum Surfaces&Films,1996,14(5):2970-2972.
[10] Tallaire A,Achard J,Silva F,et al.Growth of large size diamond single crystals by plasma assisted chemical vapour deposition:Recent achievements and remainingchallenges[J].Comptes Rendus Physique,2013,14(2):169-184.
[11] Yamamoto M,Teraji T,Ito T.Improvement in the crystalline qualityof homoepitaxial diamond films by oxygen plasma etching of mirror-polished diamond substrates[J].Journal of Crystal Growth,2005,285(1-2):130-136.
[12] Friel S L,Clewes H K,Dhillon,et al.Control of surface and bulkcrystalline quality in single crystal diamond grown by chemical vapourdeposition[J].Diamond and Related Materials,2009,18(5-8):808-815.
[13] Geis M W,Smith H I,Argoitia A,et al.Large-area mosaic diamond films approaching single-crystal quality[J].Applied Physics Letters,1991,58(22):2485-2487.
[14] Janssen G,Giling L J.“Mosaic”growth of diamond[J].Diamond and related materials,1995,4(7):1025-1031.
[15] Findeling-Dufour C,Gicquel A,Chiron R.Growth of large single-crystal diamond layers:analysis of the junctions between adjacent diamonds[J].Diamond and related materials,1998,7(7):986-998.
[16] Yamada H,Chayahara A,Mokuno Y,et al.Developments of elemental technologies to produce inch-size single-crystal diamond wafers[J].Diamond and Related materials,2011,20(4):616-619.
[17]Hideaki Yamada,Akiyoshi Chayahara,Hitoshi Umezawa,NobuteruTsubouchi,YoshiakiMokuno,Shinichi Shikata.Fabrication and fundamental characterizations of tiled clones of single-crystal diamond with 1-inch size[J].Diamond&Related Materials,2012,24.
[18]舒国阳.Mosaic拼接法高质量大尺寸单晶金刚石生长研究[D].哈尔滨工业大学,2016.
[19] DORSCH O,WERNER M,OBERNEIER E,et al.Etching of polycrystallinediamond andamorphous carbon films by RIE[J].Diamond and Ralated Materials,1992,1(2-4):277-280.
[20] DORSCH O,WERNER M,OBERMEIER E,et al.Dry etching of undoped and boron doped polycrystalline diamond films[J].Diamond and Ralated Materials,1995,4(4):456-459.
[21] SIRINENI GMR,NASEEM HA,MALSHE AP.Reactive ion etching of diamond as a means of enhancing chemically-assisted mechanical polishing efficiency[J].Diamond and Relatedmaterials,1997,6(1):952-958.
[22] ENLUND J,ISBERG J.Anisotropic dry etching of boron doped single crystal CVD diamond[J].Carbon,2009,43(12):1839-1842.
[23]吕宪义,金曾孙,郝世强,等.氧等离子体对金刚石膜的刻蚀研究[J].新型炭材料,2003,18(3):191-194.
[24]李德贵,冉均国,廖晓明,等.空气等离子体刻蚀对金刚石薄膜性能的影响[J].微细加工技术,2006(2):30-32.
[25]郑先锋,马志斌,张磊,等.直流辉光氧等离子体刻蚀金刚石膜的研究[J].金刚石与磨料磨具工程,2007(1):35-38.
[26]戴安娜彩钻公司主页[EB/OL].http://www.Diane diamond.com.2016-02-05.
[27]王五一.天然、处理和合成粉红色——红色钻石颜色形成机制及其鉴别[A].国家珠宝玉石质量监督检验中心(National Gemstone Testing Center)、中国珠宝玉石首饰行业协会.2009中国珠宝首饰学术交流会论文集[C].国家珠宝玉石质量监督检验中心(National Gemstone Testing Center)、中国珠宝玉石首饰行业协会:,2009:2.
[28]张彩慧,陈美华.电子辐照产生蓝色钻石的工艺条件探索[J].宝石和宝石学杂志,2016,18(4):10-15.
[29] K.M.Chadwick.HPHT-Treated CVD synthetic diamond submitted for grading[J].G&G 44,365-367(2008).(Winter2008,Lab notes)
[30] D.J.Twitchen,P.M.Martineau,G.A.Scarsbrook.Colored diamond,US patent#7172655[P].filed in 2003,2003.
[31] Charles S J,Butler J E,Feygelson B N,et al.Characterization of nitrogen doped chemical vapor deposited single crystal diamond before and after high pressure,high temperature annealing[M]//Explaining the mental:Cambridge Scholars Pub.2004:2473-2485.
[32] R.H.Frushour,W.Li.Method of making enhanced CVD diamond,US patent#6811610[P],issued in 2004,2002.
[33] Qi Liang,Chih-shiue Yan,Yufei Meng,et al.Recent advances in high-growth rate single-crystal CVD diamond[J].Diamond and Related Materials,2009,18(5–8):698-703.
[34]Kyaw Soe Moe,Ulrika D’Haenens-Johansson,and Wuyi Wang.LPHT-Annealed Pink CVD SYNTHETIC DIAMONDS[J].GEMS&GEMOLOGY,SUMMER 2015.
[35] D'Haenensjohansson U F S,Edmonds A M,Newton M E,et al.EPR of a defect in CVD diamond involving both silicon and hydrogen that shows preferential alignment[J].Physical Review B,2010,82(15):155205.
[36] Glover C,Newton M E,Martineau P M,et al.Hydrogen incorporation in diamond:the vacancy-hydrogen complex.[J].Physical Review Letters,2004,92(13):135502.
[37] Tallaire A,Achard J,Brinza O,et al.Growth strategy for controlling dislocation densities and crystal morphologies of single crystal diamond by using pyramidal-shape substrates[J].Diamond&Related Materials,2013,33(3):71-77.
[38] Field J E,Nicholson E,Seward C R,et al.Strength,fracture and erosion properties of cvd diamond[M]//Thin Film Diamond.Springer Netherlands,1994:261-275.
[39] Qi Liang,Chih-shiue Yan,Yufei Meng,et al.Recent advances in high-growth rate single-crystal CVD diamond[J].Diamond and Related Materials,2009,18(5–8):698-703.
[40] Zaitsev S A M.Optical Properties of Diamond[M].Springer Berlin Heidelberg,2001.
[41] Meng Y F,Yan C S,Lai J,et al.From the Cover:Enhanced optical properties of chemical vapor deposited single crystal diamond by low-pressure/high-temperature annealing:National Acad Sciences,US20100104494[P].2010.
[42] Glover C,Newton M E,Martineau P M,et al.Hydrogen incorporation in diamond:the vacancy-hydrogen complex[J].Physical Review Letters,2004,92(13):135502.
[43] Meng Y F,Yan C S,Lai J,et al.From the Cover:Enhanced optical properties of chemical vapor deposited single crystal diamond by low-pressure/high-temperature annealing:National Acad Sciences,US20100104494[P].2010.