KDP晶体潮解抛光的实验研究
摘要
在惯性约束聚变固体激光驱动器、强激光武器及核武器等关键设备所需的众多光学元器件中,KDP晶体作为一种优质的非线性材料,被广泛地应用于激光和非线性光学领域。但由于其具有软脆、易潮解、对温度变化敏感等特点,给高质量的加工要求带来了极大的困难,目前被公认为最难加工的光学零件之一。
为了探索软脆功能晶体材料KDP的超精密加工新方法,本文从KDP晶体易潮解的性质出发,研究晶体潮解的机理,研究利用潮解原理实现KDP晶体的抛光加工,最终获得一种新的超精密加工方法,并在此基础上配制抛光液,分析比较各工艺条件对抛光效果的影响。
在本文中,首先通过对KDP晶体材料特性以及潮解机理的研究分析了KDP晶体潮解抛光的材料去除机理;并通过分析知道KDP晶体在纯水中的溶解速度很快并且很难控制,用纯水作为抛光液很难达到加工要求。为此本文对KDP晶体潮解抛光的抛光液配方进行了研究。
选择乙醇作为水的稀释剂,并通过实验发现仅使用水和乙醇的混合液作为抛光液抛光KDP晶体得到的抛光效果不好,研究发现表面活性剂在化学机械抛光中起着重要作用,所以在抛光液中加入表面活性剂。用已选取的各个抛光液的成分配制不同成分比例的抛光液进行抛光实验,通过对抛光后材料去除率及表面粗糙度的分析,最终确定性能良好的抛光液组成。
最后,通过对影响潮解抛光KDP晶体的去除率及表面质量的主要工艺参数的分析,选择了四个主要的工艺参数利用已经配制好的抛光液进行单因素实验。通过对抛光后的材料去除率以及表面粗糙度的分析,研究各参数对抛光效果的影响规律,并总结出了最佳的压力、抛光液流量等工艺条件,最后研究了抛光垫对抛光效果的影响。为潮解抛光KDP晶体技术的进一步深入研究奠定了基础。
On the high-energy multi-path Inertial Confinement Fusion solid laser driver, laser weapon and other advanced equipment, only the large-size non-linear electrical-optical crystal KDP with high accuracy can be used to make optical frequency multiplication transition and switch parts. However, it is difficult for KDP crystal to machine because of its properties of the softness, brittleness, deliquescence and sensitivity to the change of temperature.
In order to explore a new method of ultra-precision machining of KDP crystals,the deliquescence mechanism of KDP crystals was studied, and on the basis of the obtained results the mechanism of deliquescence polishing was analyzed, and the slurry was developed, and the surface quality was also analyzed by changing technological conditions.
In this paper, through study of material characteristic and the deliquescence mechanism of KDP crystals the experiments of the KDP crystal dissolution in water, we can conclude that the pure water can not be used as slurry, because it is difficult to achieve the processing requirements. So, in this paper the slurry was studied.
Ethanol was chosen as the diluent of water, and the result of the KDP crystal polished only using the mixture of water and ethanol as the slurry was not so good. The surfactant in the chemical mechanical polishing plays an important role, which was found in others research. So the surfactant was added to the slurry. Polishing experiments were done using slurry of different proportion constituents which had been chosen. Through the analysis of the material removal rate and the surface roughness of the KDP crystals after polished, the slurry of the most excellent performance can be identified. At last, the slurry was prepared.
Finally, through the analysis of the main processing parameters affecting the material removal rate and the surface quality after polishing, using the good preparation slurry, selecting the four main processing parameters, the single factor experiments were done. The laws of each parameter affecting the polishing results were studied through the analysis of the material removal rate and surface roughness of the KDP crystals after polishing. And the best processing conditions, such as the pressure and the slurry flow were summed up. At last, the effect of polishing pad on the polishing quality was studied. The study will be the basis for the further study of the deliquescence polishing technology of KDP crystal.
为了探索软脆功能晶体材料KDP的超精密加工新方法,本文从KDP晶体易潮解的性质出发,研究晶体潮解的机理,研究利用潮解原理实现KDP晶体的抛光加工,最终获得一种新的超精密加工方法,并在此基础上配制抛光液,分析比较各工艺条件对抛光效果的影响。
在本文中,首先通过对KDP晶体材料特性以及潮解机理的研究分析了KDP晶体潮解抛光的材料去除机理;并通过分析知道KDP晶体在纯水中的溶解速度很快并且很难控制,用纯水作为抛光液很难达到加工要求。为此本文对KDP晶体潮解抛光的抛光液配方进行了研究。
选择乙醇作为水的稀释剂,并通过实验发现仅使用水和乙醇的混合液作为抛光液抛光KDP晶体得到的抛光效果不好,研究发现表面活性剂在化学机械抛光中起着重要作用,所以在抛光液中加入表面活性剂。用已选取的各个抛光液的成分配制不同成分比例的抛光液进行抛光实验,通过对抛光后材料去除率及表面粗糙度的分析,最终确定性能良好的抛光液组成。
最后,通过对影响潮解抛光KDP晶体的去除率及表面质量的主要工艺参数的分析,选择了四个主要的工艺参数利用已经配制好的抛光液进行单因素实验。通过对抛光后的材料去除率以及表面粗糙度的分析,研究各参数对抛光效果的影响规律,并总结出了最佳的压力、抛光液流量等工艺条件,最后研究了抛光垫对抛光效果的影响。为潮解抛光KDP晶体技术的进一步深入研究奠定了基础。
On the high-energy multi-path Inertial Confinement Fusion solid laser driver, laser weapon and other advanced equipment, only the large-size non-linear electrical-optical crystal KDP with high accuracy can be used to make optical frequency multiplication transition and switch parts. However, it is difficult for KDP crystal to machine because of its properties of the softness, brittleness, deliquescence and sensitivity to the change of temperature.
In order to explore a new method of ultra-precision machining of KDP crystals,the deliquescence mechanism of KDP crystals was studied, and on the basis of the obtained results the mechanism of deliquescence polishing was analyzed, and the slurry was developed, and the surface quality was also analyzed by changing technological conditions.
In this paper, through study of material characteristic and the deliquescence mechanism of KDP crystals the experiments of the KDP crystal dissolution in water, we can conclude that the pure water can not be used as slurry, because it is difficult to achieve the processing requirements. So, in this paper the slurry was studied.
Ethanol was chosen as the diluent of water, and the result of the KDP crystal polished only using the mixture of water and ethanol as the slurry was not so good. The surfactant in the chemical mechanical polishing plays an important role, which was found in others research. So the surfactant was added to the slurry. Polishing experiments were done using slurry of different proportion constituents which had been chosen. Through the analysis of the material removal rate and the surface roughness of the KDP crystals after polished, the slurry of the most excellent performance can be identified. At last, the slurry was prepared.
Finally, through the analysis of the main processing parameters affecting the material removal rate and the surface quality after polishing, using the good preparation slurry, selecting the four main processing parameters, the single factor experiments were done. The laws of each parameter affecting the polishing results were studied through the analysis of the material removal rate and surface roughness of the KDP crystals after polishing. And the best processing conditions, such as the pressure and the slurry flow were summed up. At last, the effect of polishing pad on the polishing quality was studied. The study will be the basis for the further study of the deliquescence polishing technology of KDP crystal.
引文
1. Rainer F. A historical perspective on fifteen years of laser damage thresholds at LLNL.SPIE, 1993, Vol. 2114: 9~12.
2.叶青.法国惯性约束聚变计划概述.激光与光电子学进展, 2000, (7): 4~6.
3.张杰.浅谈惯性约束聚变.物理, 1999, 28(3): 142~152.
4.彭翰生,张小民,范滇元,朱健强.高功率固体激光装置的发展与工程科学问题.中国工程科学, 2001, 3(3):1~8.
5.苏根博,曾金波,贺友平,李征东,黄炳荣,江日洪.大截面KDP晶体在激光核聚变研究中的应用.硅酸盐学报, 1997, 25(6):717~719.
6.杨力.先进光学制造技术.科学出版社. 2001:239~241.
7.杨福兴.激光核聚变光学元件超精密加工技术研究[J].光学技术,2003,29(6):649~651
8.张君. KDP晶体各向异性对加工表面粗糙度影响的研究.哈尔滨工业大学硕士学位论文. 2006, 2~5.
9.张文生,张飞虎等.光学脆性材料的金刚石切削加工.光学精密工程, 2003, 11 (2) :139 ~ 143.
10.杨福兴.激光核聚变光学元件超精密加工技术研究.光学技术, 2003, 29 (6) :649~651.
11.王洪祥,王景贺,孙涛,张龙江.磷酸二氢钾晶体超精密加工存在的若干问题分析.兵工学报, 2006, 27(5):911~915.
12. Liang Y, Moronuki N, Furukawa Y. Calculations of the effect of material anisotropy on micro-cutting processes. Precision Engineering, April 1994, 16(2):132-138.
13. Furukawa Y, Nobuyuki M. Effect of material properties on ultra-precision cutting processes. Annals of the CIRP, 1988, 37:113.
14. Moronuki N, Liang Y, Furukawa Y. Experiments on the effect of material properties on micro-cutting processes. Precision Engineering, 1994, 16:124.
15. Nakasuji T et al. Diamond turning of brittle materials for optical components. Annals of the CIRP, 1990, 39:89.
16. Lahaye Philippe,Chomont Christian,Dumont Pierre et al.Using a design of experiment method to improve KDP crystal machining process. Proceedings of SPIE the International society for Optical Engineering, 1998, 3492:814~820.
17. Fang Tong, Lambropoulos, John C. Micro-hardness and Indentation Fracture of Potassium Dihydrogen Phosphate(KDP). Journal of the American Ceramic Society. 2002, Vol.85:174~178.
18. Hou Jing,Zhang Jianfeng,Chen Jinlin,Zhang Xiaoli,Hu Dezhi. Surface quality of large KDP crystal fabricated by single point diamond turning. Proc. of SPIE, 2006, Vol.6149.
19.滕晓辑. KDP晶体潮解机理及材料溶解可加工性实验研究.大连理工大学硕士学位论文. 2007, 2~3.
20. Baruch. A. fuchs. Fine Diamond Turning of KDP Crystals.1986, Vol.25:1733~1735.
21. Namba Yoshiharu, Katagiri Masanori, Nakatsuka Masahiro. Single point diamond turning of KDP inorganic optical crystals for laser fusion. Journal of the Japan Society Precision Engineering. 1998, 64(10):1487~1491.
22. Kozlowski, mark R, Thomas, Ian M, Edwards, Gary etal. Influence of Diamond Turning and Surface Cleaning Processes on the Degradation of KDP Crystal Surface. Proceedings of SPIE-the International Society for Optical Engineering. 1991, Vol.1561:59~69.
23.王景贺,陈明君,董申,尚元江.晶体光学零件超精密加工技术研究的新进展.工具技术, 2004, 38(9):56～59.
24. Arrasmith, S. R, Kozhinova, I.A, Gregg, L.L, Shory, A.B, Romanofsky, H.J,Jacobs, S.D, Golini, D, Kordonski, W.I, Hogan, S, Dumas, P. Details of the polishing spot in magnetorheological finishing (MRF). Proceedings of SPIE -The International Society for Optical Engineering. 1999, Vol.3782:92~100.
25.李仲谨等.无机精细化学品.北京:化学工业出版社, 2005.
26. Frazer B C, Peninsky R.X-ray Analysis of the Ferroelectric Transition in KH2PO4, Acts. Crystallogr, 1953, 6:273.
27. Bacon G E, by Fourier Pease R S. Synthesis. A Neutron Diffraction Study of Potassium Dihydrogen Phosphate Proc. Roy. Soc, Lond, 1953, 220:397.
28.钟维烈.铁电体物理学.科学出版社,2000:27~108.
29. Vriesde S A, Goedtkindt P, et al. Surface Atomic Structure of KDP Crystals in Aqueous Solution: An Explanation of the GrowthShape. Phys. Rev. Lett, 1998, 80:2229.
30. Reedijk M F, Arsic J, et al. Liquid Order at the Interface of KDP Crystals with Water: Evidence for Icelike Layers. Phys. Rev. Lett, 2003, 90:103.
31. Lu G W, Sun X, et al. Raman Study of Lattice Vibration Modesand Growth Mechanism of KDP Single Crystals. Cryst. Res. Technol, 2002, 37:93.
32. Tatartchenko, Vitali, Beriot, Emmanuel. Growth of large KDP crystals in the form of plates. Proc SPIE, 1999, 3482:386-390.
33. Zaitseva N P, De Yoreo J J, Dehaven M R, Vital R L, Montgomery K E, Richardson M, L J Atherton. Rapid growth of large-scale (40-55cm) KH2PO4, crystals. Journal of Crystal Growth, 1997, 180:255-262.
34.张克从,王希敏.非线性光学晶体材料科学.北京:科学出版社, 1996.
35.李仲伢,李成富,程雷. KDP晶体激光损伤的研究.中国激光. 1996:279~282.
36.刁立成,张克从,常新安. KDP晶体激光损伤阈值研究的新进展.人工晶体学报. 2002:99~103.
37. T. A. Eremina,V. A. Kuznetsov,N. N. Eremin, T. M. Okhrimenko, N. G Furmanova, E.P Efremova, Mirosawa Rak. On the mechanism of impurity influence on growth kinetics and surface morphology of KDP crystals II:experimental study of influence of bivalent and trivalent impurity ions on growth kinetics and surface morphology of KDP crystals. Journal of Crystal Growth. 2005:577~585.
38.兰志俊. KDP晶体SPDT加工时冷却液对表面质量影响的研究.哈尔滨工业大学硕士学位论文. 2006:11~13.
39.楼书聪,杨玉玲主编.化学试剂配制手册.江苏科学技术出版社. 2002.
40. Joseph M. Steigerwald Shyam P. Murarka Ronald J. Gutmann. Chemical Mechanical Planarization of Microelectronic Materials .A Willey-Interscience Publication,John Wiley&Sons INC 1997.
41.杜巧云,葛虹.表面活性剂基础及应用.北京:中国石化出版社, 1997:12-20.
42.慕慧.基础化学.北京:科学出版社, 2001.
43.刘程等.表面活性剂应用大全.北京:北京工业大学出版社, 1992.
44.孙杰编.表面活性剂的基础和应用.大连:大连理工大学出版社, 1992.
45.沈钟,王果庭等.胶体与表面化学.北京:化学工业出版社, 1991.
46. S. D. Hosali,A. R. Sethuraman, J. F. Wang et al. Planarization Process and Consumable Development for Shallow Trench Isolation. Proc. CMPMIC. 1997, 1:52.
47.狄卫国,杨明,刘玉岭.超大规模集成电路制备中硅衬底抛光液研究.石家庄铁道学院学报, 2003, 16(4), 38~41.
48. R Kolenkow, R Nagahara. Chemical-mechanical wafer polishing and planarization in batch systems. Solid State Technology, 1992, (12): 112~114
2.叶青.法国惯性约束聚变计划概述.激光与光电子学进展, 2000, (7): 4~6.
3.张杰.浅谈惯性约束聚变.物理, 1999, 28(3): 142~152.
4.彭翰生,张小民,范滇元,朱健强.高功率固体激光装置的发展与工程科学问题.中国工程科学, 2001, 3(3):1~8.
5.苏根博,曾金波,贺友平,李征东,黄炳荣,江日洪.大截面KDP晶体在激光核聚变研究中的应用.硅酸盐学报, 1997, 25(6):717~719.
6.杨力.先进光学制造技术.科学出版社. 2001:239~241.
7.杨福兴.激光核聚变光学元件超精密加工技术研究[J].光学技术,2003,29(6):649~651
8.张君. KDP晶体各向异性对加工表面粗糙度影响的研究.哈尔滨工业大学硕士学位论文. 2006, 2~5.
9.张文生,张飞虎等.光学脆性材料的金刚石切削加工.光学精密工程, 2003, 11 (2) :139 ~ 143.
10.杨福兴.激光核聚变光学元件超精密加工技术研究.光学技术, 2003, 29 (6) :649~651.
11.王洪祥,王景贺,孙涛,张龙江.磷酸二氢钾晶体超精密加工存在的若干问题分析.兵工学报, 2006, 27(5):911~915.
12. Liang Y, Moronuki N, Furukawa Y. Calculations of the effect of material anisotropy on micro-cutting processes. Precision Engineering, April 1994, 16(2):132-138.
13. Furukawa Y, Nobuyuki M. Effect of material properties on ultra-precision cutting processes. Annals of the CIRP, 1988, 37:113.
14. Moronuki N, Liang Y, Furukawa Y. Experiments on the effect of material properties on micro-cutting processes. Precision Engineering, 1994, 16:124.
15. Nakasuji T et al. Diamond turning of brittle materials for optical components. Annals of the CIRP, 1990, 39:89.
16. Lahaye Philippe,Chomont Christian,Dumont Pierre et al.Using a design of experiment method to improve KDP crystal machining process. Proceedings of SPIE the International society for Optical Engineering, 1998, 3492:814~820.
17. Fang Tong, Lambropoulos, John C. Micro-hardness and Indentation Fracture of Potassium Dihydrogen Phosphate(KDP). Journal of the American Ceramic Society. 2002, Vol.85:174~178.
18. Hou Jing,Zhang Jianfeng,Chen Jinlin,Zhang Xiaoli,Hu Dezhi. Surface quality of large KDP crystal fabricated by single point diamond turning. Proc. of SPIE, 2006, Vol.6149.
19.滕晓辑. KDP晶体潮解机理及材料溶解可加工性实验研究.大连理工大学硕士学位论文. 2007, 2~3.
20. Baruch. A. fuchs. Fine Diamond Turning of KDP Crystals.1986, Vol.25:1733~1735.
21. Namba Yoshiharu, Katagiri Masanori, Nakatsuka Masahiro. Single point diamond turning of KDP inorganic optical crystals for laser fusion. Journal of the Japan Society Precision Engineering. 1998, 64(10):1487~1491.
22. Kozlowski, mark R, Thomas, Ian M, Edwards, Gary etal. Influence of Diamond Turning and Surface Cleaning Processes on the Degradation of KDP Crystal Surface. Proceedings of SPIE-the International Society for Optical Engineering. 1991, Vol.1561:59~69.
23.王景贺,陈明君,董申,尚元江.晶体光学零件超精密加工技术研究的新进展.工具技术, 2004, 38(9):56～59.
24. Arrasmith, S. R, Kozhinova, I.A, Gregg, L.L, Shory, A.B, Romanofsky, H.J,Jacobs, S.D, Golini, D, Kordonski, W.I, Hogan, S, Dumas, P. Details of the polishing spot in magnetorheological finishing (MRF). Proceedings of SPIE -The International Society for Optical Engineering. 1999, Vol.3782:92~100.
25.李仲谨等.无机精细化学品.北京:化学工业出版社, 2005.
26. Frazer B C, Peninsky R.X-ray Analysis of the Ferroelectric Transition in KH2PO4, Acts. Crystallogr, 1953, 6:273.
27. Bacon G E, by Fourier Pease R S. Synthesis. A Neutron Diffraction Study of Potassium Dihydrogen Phosphate Proc. Roy. Soc, Lond, 1953, 220:397.
28.钟维烈.铁电体物理学.科学出版社,2000:27~108.
29. Vriesde S A, Goedtkindt P, et al. Surface Atomic Structure of KDP Crystals in Aqueous Solution: An Explanation of the GrowthShape. Phys. Rev. Lett, 1998, 80:2229.
30. Reedijk M F, Arsic J, et al. Liquid Order at the Interface of KDP Crystals with Water: Evidence for Icelike Layers. Phys. Rev. Lett, 2003, 90:103.
31. Lu G W, Sun X, et al. Raman Study of Lattice Vibration Modesand Growth Mechanism of KDP Single Crystals. Cryst. Res. Technol, 2002, 37:93.
32. Tatartchenko, Vitali, Beriot, Emmanuel. Growth of large KDP crystals in the form of plates. Proc SPIE, 1999, 3482:386-390.
33. Zaitseva N P, De Yoreo J J, Dehaven M R, Vital R L, Montgomery K E, Richardson M, L J Atherton. Rapid growth of large-scale (40-55cm) KH2PO4, crystals. Journal of Crystal Growth, 1997, 180:255-262.
34.张克从,王希敏.非线性光学晶体材料科学.北京:科学出版社, 1996.
35.李仲伢,李成富,程雷. KDP晶体激光损伤的研究.中国激光. 1996:279~282.
36.刁立成,张克从,常新安. KDP晶体激光损伤阈值研究的新进展.人工晶体学报. 2002:99~103.
37. T. A. Eremina,V. A. Kuznetsov,N. N. Eremin, T. M. Okhrimenko, N. G Furmanova, E.P Efremova, Mirosawa Rak. On the mechanism of impurity influence on growth kinetics and surface morphology of KDP crystals II:experimental study of influence of bivalent and trivalent impurity ions on growth kinetics and surface morphology of KDP crystals. Journal of Crystal Growth. 2005:577~585.
38.兰志俊. KDP晶体SPDT加工时冷却液对表面质量影响的研究.哈尔滨工业大学硕士学位论文. 2006:11~13.
39.楼书聪,杨玉玲主编.化学试剂配制手册.江苏科学技术出版社. 2002.
40. Joseph M. Steigerwald Shyam P. Murarka Ronald J. Gutmann. Chemical Mechanical Planarization of Microelectronic Materials .A Willey-Interscience Publication,John Wiley&Sons INC 1997.
41.杜巧云,葛虹.表面活性剂基础及应用.北京:中国石化出版社, 1997:12-20.
42.慕慧.基础化学.北京:科学出版社, 2001.
43.刘程等.表面活性剂应用大全.北京:北京工业大学出版社, 1992.
44.孙杰编.表面活性剂的基础和应用.大连:大连理工大学出版社, 1992.
45.沈钟,王果庭等.胶体与表面化学.北京:化学工业出版社, 1991.
46. S. D. Hosali,A. R. Sethuraman, J. F. Wang et al. Planarization Process and Consumable Development for Shallow Trench Isolation. Proc. CMPMIC. 1997, 1:52.
47.狄卫国,杨明,刘玉岭.超大规模集成电路制备中硅衬底抛光液研究.石家庄铁道学院学报, 2003, 16(4), 38~41.
48. R Kolenkow, R Nagahara. Chemical-mechanical wafer polishing and planarization in batch systems. Solid State Technology, 1992, (12): 112~114