微晶玻璃硬盘基板的研究
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摘要
随着计算机技术朝小型化、高性能化飞速发展，同时应用软件和数据量的不断增大，必然要求硬盘具有更大的容量和更好的性能。
硬盘主要由盘片和磁头两部分组成。盘片主要包括：基板、磁性层和保护性衬层三个部分。在硬盘工作时，盘片受到各种作用力，且这些作用力主要由基板来承受。纵观近年来硬盘的发展趋势，硬盘正朝着更高的容量、更快的速度、更小的体积快速发展，要求基板材料具有更好的力学性能和平整的表面，原先的NiP／Al基板已经无法适应这一变化。
在所有的基板材料当中，微晶玻璃是最有希望用作硬盘基板的。其中以MgO-Al_2O_3-SiO_2系微晶玻璃性能最为优越。因此，对MAS系统微晶玻璃进行深入的研究具有重要的意义。
本文以MAS系统微晶玻璃为研究对象，运用XRD、SEM、IR等微观结构测试方法，结合微晶玻璃力学性能、热膨胀系数等，研究其组成、热处理制度、微观结构和性能四者之间的相互联系和影响，通过实验确定合理的组成和热处理制度，制备具有较高力学性能和合理晶相组成的微晶玻璃。
首先，研究微晶玻璃中MgO和Al_2O_3含量的改变对微晶玻璃微观结构和力学性能的影响，结果表明：对于MgO／Al_2O_3＜1的组成来说，微晶玻璃具有较高的力学性能和较合理的微观结构。在MgO／Al_2O_3＜1的组成里，随着Al_2O_3含量的升高，微晶玻璃的力学性能逐渐增强。
接着，对热处理制度进行较深入的研究，分析热处理制度的改交对微晶玻璃的晶相、力学性能、Si和Ti的价态基团、化学稳定性和晶体颗粒度的影响。结果表明：随着晶化温度的升高。[Si-O]键的不饱和程度进一步增加，残余玻璃相中的钛离子逐渐减少，化学稳定性也随着增强。
最后，对TiO_2和TiO_2+ZrO_2进行深入研究，对比TiO_2晶核剂和TiO_2+ZrO_2复合晶核剂对微晶玻璃性能的影响。结果表明：随着复合晶核剂的引入，微晶玻璃的析晶活化能由277.1 KJ／mol降低为207.8KJ／mol，同时降低微晶玻璃的初始析晶温度。
With the development of the computer science toward miniaturization and high performance, at the same time, soft and data increasing loo, so it requires hard disks have more capability and high performance.
Hard disks include two segments, they are: magnetic cores and disks. And disks are made up of three parts, they are substrate* magnetism layer and protective under layer. When hard disks are working, disks receive many kinds of force. And most of them are endured by substrate. From computers' development within these years, we can see that hard disks have a trend to smaller disk diameters (which allows more rapid design and integration) and more capacity and faster rotate speed. It will require substrate materials have high mechanical performance and good flatness, but the former NiP/Al substrate cannot accommodate to these change.
In the all candidate materials, glass-ceramic is the most superior material for hard-disk substrate. But in all glass-ceramics, MAS system glass-ceramic is the fit to substrate. So it has enormous scientific value to research on MAS system.
In this text, MAS system glass-ceramic was studied. The influence of the different heat treatments, composition on the microstructure and the mechanical properties of glass-ceramics was researched by the IR, XRD , SEM and mechanics tests. And it has a deep research on the composition, heat-treatments, micro-structure and capability. Then it will draw some conclusions that reason composition and heat- treatments and high-performance glass-ceramic substrate.
First, we research on the connection of MgO and Al2O3 content with the glass-ceramics' microstructure and mechanical performance. And the results demonstrate that glass-ceramics have better mechanical performance and reasonable micro- structure when MgO/Al2O3 Second, we research on the heat-treatments. We analyze the effect of the heat-treatments alterations on the phase, mechanical performance and chemical stable-
ness. And the results demonstrate that the unsaturated degree of [Si-0] will increase and the Ti4+ in the glass will decrease when the heat-treatments' temperature enhanced.
At last, we research on the change of nucleation agents (TiO2 and TiO2+ZrO2) and their effect on the glass-ceramic. And the results demonstrate that activation energy has reduced from 277.1 KJ/mol to 207.8KJ/mol when nucleation agents changed from TiO2 to TiO2+ZrO2.
硬盘主要由盘片和磁头两部分组成。盘片主要包括：基板、磁性层和保护性衬层三个部分。在硬盘工作时，盘片受到各种作用力，且这些作用力主要由基板来承受。纵观近年来硬盘的发展趋势，硬盘正朝着更高的容量、更快的速度、更小的体积快速发展，要求基板材料具有更好的力学性能和平整的表面，原先的NiP／Al基板已经无法适应这一变化。
在所有的基板材料当中，微晶玻璃是最有希望用作硬盘基板的。其中以MgO-Al_2O_3-SiO_2系微晶玻璃性能最为优越。因此，对MAS系统微晶玻璃进行深入的研究具有重要的意义。
本文以MAS系统微晶玻璃为研究对象，运用XRD、SEM、IR等微观结构测试方法，结合微晶玻璃力学性能、热膨胀系数等，研究其组成、热处理制度、微观结构和性能四者之间的相互联系和影响，通过实验确定合理的组成和热处理制度，制备具有较高力学性能和合理晶相组成的微晶玻璃。
首先，研究微晶玻璃中MgO和Al_2O_3含量的改变对微晶玻璃微观结构和力学性能的影响，结果表明：对于MgO／Al_2O_3＜1的组成来说，微晶玻璃具有较高的力学性能和较合理的微观结构。在MgO／Al_2O_3＜1的组成里，随着Al_2O_3含量的升高，微晶玻璃的力学性能逐渐增强。
接着，对热处理制度进行较深入的研究，分析热处理制度的改交对微晶玻璃的晶相、力学性能、Si和Ti的价态基团、化学稳定性和晶体颗粒度的影响。结果表明：随着晶化温度的升高。[Si-O]键的不饱和程度进一步增加，残余玻璃相中的钛离子逐渐减少，化学稳定性也随着增强。
最后，对TiO_2和TiO_2+ZrO_2进行深入研究，对比TiO_2晶核剂和TiO_2+ZrO_2复合晶核剂对微晶玻璃性能的影响。结果表明：随着复合晶核剂的引入，微晶玻璃的析晶活化能由277.1 KJ／mol降低为207.8KJ／mol，同时降低微晶玻璃的初始析晶温度。
With the development of the computer science toward miniaturization and high performance, at the same time, soft and data increasing loo, so it requires hard disks have more capability and high performance.
Hard disks include two segments, they are: magnetic cores and disks. And disks are made up of three parts, they are substrate* magnetism layer and protective under layer. When hard disks are working, disks receive many kinds of force. And most of them are endured by substrate. From computers' development within these years, we can see that hard disks have a trend to smaller disk diameters (which allows more rapid design and integration) and more capacity and faster rotate speed. It will require substrate materials have high mechanical performance and good flatness, but the former NiP/Al substrate cannot accommodate to these change.
In the all candidate materials, glass-ceramic is the most superior material for hard-disk substrate. But in all glass-ceramics, MAS system glass-ceramic is the fit to substrate. So it has enormous scientific value to research on MAS system.
In this text, MAS system glass-ceramic was studied. The influence of the different heat treatments, composition on the microstructure and the mechanical properties of glass-ceramics was researched by the IR, XRD , SEM and mechanics tests. And it has a deep research on the composition, heat-treatments, micro-structure and capability. Then it will draw some conclusions that reason composition and heat- treatments and high-performance glass-ceramic substrate.
First, we research on the connection of MgO and Al2O3 content with the glass-ceramics' microstructure and mechanical performance. And the results demonstrate that glass-ceramics have better mechanical performance and reasonable micro- structure when MgO/Al2O3
ness. And the results demonstrate that the unsaturated degree of [Si-0] will increase and the Ti4+ in the glass will decrease when the heat-treatments' temperature enhanced.
At last, we research on the change of nucleation agents (TiO2 and TiO2+ZrO2) and their effect on the glass-ceramic. And the results demonstrate that activation energy has reduced from 277.1 KJ/mol to 207.8KJ/mol when nucleation agents changed from TiO2 to TiO2+ZrO2.
引文
[1] Edward Grochowski and David A, Thompson Outlook for maintaining Areal Density Growth in Magnetic Recording, IEEE TRANSACTIONS ON MAGNETICS, VOL.30NO.6, 1994
[2] Hsiao-chu Tsai , ADVANTAGE AND CHALLENGE OF NONMETALLIC SUBSTRATES FOR RIGIDDISK APPLICATIONS IEEE TRANSACTIONS ON MAGNETICS, VOL.29NO.1 , 1993
[3] Hisao-Chu Tsai and Atef Eltoukhy , HEAD FLYING CHARACTERISITCS ON CANASITE DISKS, IEEE TRANSACTIONS ON MAGNETICS, VOL.27NO,6 , 1991
[4] Xiaoxia Tang , High coercivity and low noise media using glass substrateBill Reed, Robert Zubeck, IEEE TRANSACTIONS ON MAGNETICS, VOL.30, NO.6 , 1994
[5] Brij B. Lal and Michael A. Russak, Tribological characteristics of lithium disilicate glass substrates media, IEEE TRANSACTIONS ON MAGNETICS, VOL.31 NO.6 , 1995
[6] Gary C. Rauch, Jia Jay Liu, Sang Y. Lee; Glass-Ceramic Substrates for IGb/in~2 and beyond, IEEE TRANSACTIONS ON MAGNETICS, VOL.32, NO.5 , 1996
[7] George H. Beall and Linda R. Pinckney , Nanophase Glass-ceramics Journal of the American ceramic Society, Vol.82,No. 1,1999
[8] Sung-Bum Sohn ,Se-Young Choi , Crystallization behavior in the glass system MgO-Al_2O_3-SiO_2:influence of CeO_2 addition ,Journal of Non-crystalline Solids 282 (2001) 221-227
[9] Xuelu zou,Hisayoshi Toratani , Composition design of high modulus glasses for disk substrates Journal of Non-crystalline Solids 290 (2001) 180-188
[10] Shiang-Po Hwang and Jenn-Ming Wu , Effect of composition on microstructural development in MgO-Al_2O_3-SiO_2 Glass-ceramics Journal of the American ceramic Society, Vol. 84, No.5, 2001
[11] 迟玉山，沈菊云，陈学贤，计算机硬盘基板材料的研究，陶瓷学报，Vol．21，No．2，2000
[12] 迟玉山，沈菊云，陈学贤，硬盘基板用微晶玻璃的析晶过程研究无机材料学报，Vol．16，No．5，2001
[13] 王艳丽，沈菊云，陈学贤，低介低损耗微晶玻璃中晶相与热膨胀性能关系的研究，无机材料学报，Vol．14，No．4，1999
[14] 王艳丽，沈菊云等，添加铅硅玻璃对烧结堇青石基微晶玻璃性能的影响，无机材料学报，Vol．16，No．3，2001
[15] 刘平，陈显学，K_2O-MgO-Al_2O_3-SiO_2系玻璃的分相与析晶，无机材料学报，Vol．14，No．2．1999
[16] 孙洪巍，陈显求，高力明，组成对R_2O-CaO-ZnO-Al_2O_3-SiO_2系统分相的影响，无机材料学报，Vol．16，No．3．2001
[17] 韩建军 刘继翔 毛豫兰 周学东，透明微晶玻璃的研究，武汉工业大学学报
[18] 袁坚 汤李缨 许超，用DTA方法研究Li_2O-Al_2O_3-4SiO_2微晶玻璃的晶化，武汉工业大学学报
[19] 陈述才，近年日本光盘的玻璃基板生产、市场情况，光学技术
[20] 程金树 肖静，热处理制度对Li_2O-Al_2O_3-SiO_2系统微晶玻璃结构及性能的影响．武汉工业大学学报
[21] [英]P．W．麦克米伦，李家治译，微晶玻璃，中国建筑出版社
[22] 杨淑珍：周和平，无机非金属材料测试实验，武汉工业大学出版社
[23] Szabo , Structure,chemical,durability and microhardness of glass-ceramics containing apatie and leucite crystals, Journal of Non-crystalline Solids 272 (2000) 191-199
[24] M. Frank, Mechanisms of nucleation and controlled crystallization of needle-like apatite in glass-ceramics of the SiO_2-Al_2O_3-K_2O-CaO-P_2O_5 system, Journal of Non-crystalline Solids 253 (1999) 170-177
[25] M. C. Weinberg, A few topics concerning nucleation and crystallization in glasses, Journal of Non-crystalline Solids 255 (1999) 1-14
[26] P. Riello, P. Canton, Nucleation and crystallization behavior of glass-ceramic materials in the Li_2O-Al_2O_3-SiO_2 system of interest for their transparency properties , Journal of Non-crystalline Solids 288 (2001) 127-139
[27] J. Malzbender , Elastic modulus, hardness and fracture toughness of SiO_2-filled methyltrimethoxysilane coating on glass substrates , Journal of Non-crystalline Solids 265 (2000) 51-60
[28] Jack Xuan, Ga-Lane Chen , Effect of Isotropic Sub-Micron Crystallized Texture of Glass-Ceramics Disks on low Glide, Stiction, and CSS , IEEE TRANSACTIONS ON MAGNETICS, VOL.31, NO.6 , 1995
[29] N. Kitmura ,K. Fukumi, High pressure densification of lithium silicate glasses, Journal of Non-crystalline Solids 274 (2000) 244-248
[30] 温广武，雷廷权，Li_2O-Al_2O_3-SiO_2微晶玻璃的烧结特性与性能，机械工程材料，Vol. 20. No3, 1996
[31] 贺海燕，微晶玻璃的定向晶化，陶瓷工程，第33卷第一期，1999
[32] Katsumasa Yasukawa, Crystallinity Analysis of glass-ceramics by the rietveld method, Journal of the American ceramic Society, Vol.81,No.11,1998
[33] Bo. zhang, Aqueous sol-gel route to barium aluminosilicate glass-ceramics, Journal of the American ceramic Society, Vol.82,No. 1,1999
[34] 作花济夫著，蒋国栋等译，玻璃手册，中国建筑工业出版社
[35] [法]J．扎齐斯基，玻璃与非晶态材料，科学出版社
[36] 西北轻工业学院，玻璃工艺学，中国轻工业出版社
[37] 何莉萍等，氧化钛对微晶玻璃系统析晶过程及材料性能的影响，材料加工与性能，1997，vol 15．no．3
[38] 张云等，微晶玻璃及其抛光，航空精密制造技术，2000，VOL36．NO1
[39] 周济等，铁氧体-微晶玻璃纳米复合材料的结构与性能，无机材料学报，1999，VOL14，NO3
[40] [日]素木洋一，硅酸盐手册，轻工业出版社
[41] 周和平，无机非金属材料测试，武汉工业大学出版社
[42] 高官明，玻璃基板用电子料浆，昆明贵金属研究所
[43] 肖静，Li_2O-Al_2O_3-SiO_2系统微晶玻璃结构及性能的研究(硕士论文)，武汉工业大学，1999
[2] Hsiao-chu Tsai , ADVANTAGE AND CHALLENGE OF NONMETALLIC SUBSTRATES FOR RIGIDDISK APPLICATIONS IEEE TRANSACTIONS ON MAGNETICS, VOL.29NO.1 , 1993
[3] Hisao-Chu Tsai and Atef Eltoukhy , HEAD FLYING CHARACTERISITCS ON CANASITE DISKS, IEEE TRANSACTIONS ON MAGNETICS, VOL.27NO,6 , 1991
[4] Xiaoxia Tang , High coercivity and low noise media using glass substrateBill Reed, Robert Zubeck, IEEE TRANSACTIONS ON MAGNETICS, VOL.30, NO.6 , 1994
[5] Brij B. Lal and Michael A. Russak, Tribological characteristics of lithium disilicate glass substrates media, IEEE TRANSACTIONS ON MAGNETICS, VOL.31 NO.6 , 1995
[6] Gary C. Rauch, Jia Jay Liu, Sang Y. Lee; Glass-Ceramic Substrates for IGb/in~2 and beyond, IEEE TRANSACTIONS ON MAGNETICS, VOL.32, NO.5 , 1996
[7] George H. Beall and Linda R. Pinckney , Nanophase Glass-ceramics Journal of the American ceramic Society, Vol.82,No. 1,1999
[8] Sung-Bum Sohn ,Se-Young Choi , Crystallization behavior in the glass system MgO-Al_2O_3-SiO_2:influence of CeO_2 addition ,Journal of Non-crystalline Solids 282 (2001) 221-227
[9] Xuelu zou,Hisayoshi Toratani , Composition design of high modulus glasses for disk substrates Journal of Non-crystalline Solids 290 (2001) 180-188
[10] Shiang-Po Hwang and Jenn-Ming Wu , Effect of composition on microstructural development in MgO-Al_2O_3-SiO_2 Glass-ceramics Journal of the American ceramic Society, Vol. 84, No.5, 2001
[11] 迟玉山，沈菊云，陈学贤，计算机硬盘基板材料的研究，陶瓷学报，Vol．21，No．2，2000
[12] 迟玉山，沈菊云，陈学贤，硬盘基板用微晶玻璃的析晶过程研究无机材料学报，Vol．16，No．5，2001
[13] 王艳丽，沈菊云，陈学贤，低介低损耗微晶玻璃中晶相与热膨胀性能关系的研究，无机材料学报，Vol．14，No．4，1999
[14] 王艳丽，沈菊云等，添加铅硅玻璃对烧结堇青石基微晶玻璃性能的影响，无机材料学报，Vol．16，No．3，2001
[15] 刘平，陈显学，K_2O-MgO-Al_2O_3-SiO_2系玻璃的分相与析晶，无机材料学报，Vol．14，No．2．1999
[16] 孙洪巍，陈显求，高力明，组成对R_2O-CaO-ZnO-Al_2O_3-SiO_2系统分相的影响，无机材料学报，Vol．16，No．3．2001
[17] 韩建军 刘继翔 毛豫兰 周学东，透明微晶玻璃的研究，武汉工业大学学报
[18] 袁坚 汤李缨 许超，用DTA方法研究Li_2O-Al_2O_3-4SiO_2微晶玻璃的晶化，武汉工业大学学报
[19] 陈述才，近年日本光盘的玻璃基板生产、市场情况，光学技术
[20] 程金树 肖静，热处理制度对Li_2O-Al_2O_3-SiO_2系统微晶玻璃结构及性能的影响．武汉工业大学学报
[21] [英]P．W．麦克米伦，李家治译，微晶玻璃，中国建筑出版社
[22] 杨淑珍：周和平，无机非金属材料测试实验，武汉工业大学出版社
[23] Szabo , Structure,chemical,durability and microhardness of glass-ceramics containing apatie and leucite crystals, Journal of Non-crystalline Solids 272 (2000) 191-199
[24] M. Frank, Mechanisms of nucleation and controlled crystallization of needle-like apatite in glass-ceramics of the SiO_2-Al_2O_3-K_2O-CaO-P_2O_5 system, Journal of Non-crystalline Solids 253 (1999) 170-177
[25] M. C. Weinberg, A few topics concerning nucleation and crystallization in glasses, Journal of Non-crystalline Solids 255 (1999) 1-14
[26] P. Riello, P. Canton, Nucleation and crystallization behavior of glass-ceramic materials in the Li_2O-Al_2O_3-SiO_2 system of interest for their transparency properties , Journal of Non-crystalline Solids 288 (2001) 127-139
[27] J. Malzbender , Elastic modulus, hardness and fracture toughness of SiO_2-filled methyltrimethoxysilane coating on glass substrates , Journal of Non-crystalline Solids 265 (2000) 51-60
[28] Jack Xuan, Ga-Lane Chen , Effect of Isotropic Sub-Micron Crystallized Texture of Glass-Ceramics Disks on low Glide, Stiction, and CSS , IEEE TRANSACTIONS ON MAGNETICS, VOL.31, NO.6 , 1995
[29] N. Kitmura ,K. Fukumi, High pressure densification of lithium silicate glasses, Journal of Non-crystalline Solids 274 (2000) 244-248
[30] 温广武，雷廷权，Li_2O-Al_2O_3-SiO_2微晶玻璃的烧结特性与性能，机械工程材料，Vol. 20. No3, 1996
[31] 贺海燕，微晶玻璃的定向晶化，陶瓷工程，第33卷第一期，1999
[32] Katsumasa Yasukawa, Crystallinity Analysis of glass-ceramics by the rietveld method, Journal of the American ceramic Society, Vol.81,No.11,1998
[33] Bo. zhang, Aqueous sol-gel route to barium aluminosilicate glass-ceramics, Journal of the American ceramic Society, Vol.82,No. 1,1999
[34] 作花济夫著，蒋国栋等译，玻璃手册，中国建筑工业出版社
[35] [法]J．扎齐斯基，玻璃与非晶态材料，科学出版社
[36] 西北轻工业学院，玻璃工艺学，中国轻工业出版社
[37] 何莉萍等，氧化钛对微晶玻璃系统析晶过程及材料性能的影响，材料加工与性能，1997，vol 15．no．3
[38] 张云等，微晶玻璃及其抛光，航空精密制造技术，2000，VOL36．NO1
[39] 周济等，铁氧体-微晶玻璃纳米复合材料的结构与性能，无机材料学报，1999，VOL14，NO3
[40] [日]素木洋一，硅酸盐手册，轻工业出版社
[41] 周和平，无机非金属材料测试，武汉工业大学出版社
[42] 高官明，玻璃基板用电子料浆，昆明贵金属研究所
[43] 肖静，Li_2O-Al_2O_3-SiO_2系统微晶玻璃结构及性能的研究(硕士论文)，武汉工业大学，1999