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实现玻璃微晶化过程控制的基础是要充分认识其析晶行为及动力学机理. 利用示差扫描量热法和析晶热处理等手段, 研究发现 20GeS2·80Sb2S3硫系玻璃属于表面析晶, 在268℃(Tg+30℃)下热处理60 h, 可以获得表面约40 μm的Sb2S3晶层复合玻璃陶瓷样品. 在此基础上, 利用非等温法从理论上分析该玻璃的析晶动力学机理. 计算得到其析晶活化能Ec为(223.6±24.1)kJ·mol-1, 在热处理温度(268℃)下的析晶速率常数K为1.23×10-4 s-1, 属于较难析晶的玻璃组成; 玻璃的晶体生长指数m和晶体生长维数n均为2, 表明其Sb2S3相的析晶行为是二维生长过程, 与析晶实验结果完全相符. 由此可知, 对于Sb2S3晶体复合的硫系玻璃陶瓷样品可通过玻璃粉末压片烧结、带铸法或丝网印刷法制备获得, 为今后功能硫系玻璃的开发提供实验依据和理论指导.Knowledge of crystallization behavior and kinetics mechanism is essential to achieve the controllable crystallization. Surface crystallization of 20GeS2·80Sb2S3 chalcogenide glass is realized using differential scanning calorimeter technique and heat treatment method. An about 40 μm thick Sb2S3 crystal layer is precipitated after heat treatment at 268℃ (Tg+30℃) for 60 h. Then, non-isothermal method is employed to theoretically analyze the crystallization kinetics of this glass sample. Crystallization activation energy Ec is calculated to be (223.6±24.1) kJ·mol-1, and crystallization rate constant K at 268℃ was obtained to be 1.23×10-4 s-1, indicating that the crystallization of 20GeS2·80Sb2S3 glass is more difficult than that of other chalcogenide glass system, such as GeS2-Ga2S3. The crystal growth index, m and crystal growth dimensionality, n both are equal to 2, which suggests that the crystallization of Sb2S3 glass phase is of 2D growth process. This work would contribute to the fabrication of Sb2S3 crystallites embedded chalcogenide glass-ceramics.
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Keywords:
- chalcogenide glass /
- crystallization /
- crystallization kinetics /
- crystallization behavior
[1] Song B A, Dai S X, Xu T F, Nie Q H, Shen X, Wang X S, Lin C G 2011 Acta Phys. Sin. 60 084217 (in Chinese) [宋宝安, 戴世勋, 徐铁峰, 聂秋华, 沈祥, 王训四, 林常规 2011 60 084217]
[2] Lin C G, Li Z B, Qin H J, Ni W H, Li Y Y, Dai S X 2012 Acta Phys. Sin. 61 154212 (in Chinese) [林常规, 李卓斌, 覃海娇, 倪文豪, 李燕颖, 戴世勋 2012 61 154212]
[3] Lin C G, Calvez L, Li Z B, Dai S X, Tao H Z, Ma H L, Zhang X H, Moine B, Zhao X J 2013 J. Am. Ceram. Soc. 96 816
[4] Lin C G, Calvez L, Ying L, Chen F F, Song B A, Shen X, Dai S X, Zhang X H 2011 Appl. Phys. A 104 615
[5] Mizuno F, Hayashi A, Tadanaga K, Tatsumisago M 2005 Adv. Mater. 17 918
[6] Chen H P, Tao H Z, Wu Q D, Zhao X J 2013 J. Am. Ceram. Soc. 96 801
[7] Tao H Z, Zhao X J, Liu Q M 2013 J. Non-Crystal. Solids DOI: 10.1016/j.jnoncrysol.2013.02.001
[8] Lin C G, Calvez L, Bureau B, Tao H Z, Allix M, Hao Z X, Seznec V, Zhang X H, Zhao X H 2010 Phys. Chem. Chem. Phys. 12 3780
[9] Lin C G, Tao H Z, Pan R K, Zheng X L, Dong G P, Zang H C, Zhao X J 2008 Chem. Phys. Lett. 460 125
[10] Delaizir G, Lucas P, Zhang X, Ma H, Bureau B, Lucas J 2007 J. Am. Ceram. Soc. 90 2073
[11] Lin C G, Dai S X, Liu C, Song B A, Xu Y S, Chen F F, Heo J 2012 Appl. Phys. Lett. 100 231910
[12] Itzhaik Y, Niitsoo O, Page M, Hodes G 2009 J. Phys. Chem. C 113 4254
[13] Lou W J, Chen M, Wang X B, Liu W M 2007 Chem. Mater. 19 872
[14] Yang J, Liu Y C, Lin H M, Chen C C 2004 Adv. Mater. 16 713
[15] Xiao X D, Liu Q M, Dong G P, Zhao X J 2007 Opt. Commun. 274 456
[16] Lin C G, Li Z B, Ying L, Xu Y S, Zhang P Q, Dai S X, Xu T F, Nie Q H 2012 J. Phys. Chem. C 116 5862
[17] Lin C G, Calvez L, Rozé M, Tao H Z, Zhang X H, Zhao X J 2009 Appl. Phys. A 97 713
[18] Bansal N, Hyatt M 1989 J. Mater. Res. 4 1257
[19] Johnson W, Mehl R 1939 Trans. Am. Inst. Min. Metall. Eng. 135 416
[20] Avrami M 1939 J. Chem. Phys. 7 1103
[21] Avrami M 1940 J. Chem. Phys. 8 212
[22] Ozawa T 1971 Polymer 12 150
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[1] Song B A, Dai S X, Xu T F, Nie Q H, Shen X, Wang X S, Lin C G 2011 Acta Phys. Sin. 60 084217 (in Chinese) [宋宝安, 戴世勋, 徐铁峰, 聂秋华, 沈祥, 王训四, 林常规 2011 60 084217]
[2] Lin C G, Li Z B, Qin H J, Ni W H, Li Y Y, Dai S X 2012 Acta Phys. Sin. 61 154212 (in Chinese) [林常规, 李卓斌, 覃海娇, 倪文豪, 李燕颖, 戴世勋 2012 61 154212]
[3] Lin C G, Calvez L, Li Z B, Dai S X, Tao H Z, Ma H L, Zhang X H, Moine B, Zhao X J 2013 J. Am. Ceram. Soc. 96 816
[4] Lin C G, Calvez L, Ying L, Chen F F, Song B A, Shen X, Dai S X, Zhang X H 2011 Appl. Phys. A 104 615
[5] Mizuno F, Hayashi A, Tadanaga K, Tatsumisago M 2005 Adv. Mater. 17 918
[6] Chen H P, Tao H Z, Wu Q D, Zhao X J 2013 J. Am. Ceram. Soc. 96 801
[7] Tao H Z, Zhao X J, Liu Q M 2013 J. Non-Crystal. Solids DOI: 10.1016/j.jnoncrysol.2013.02.001
[8] Lin C G, Calvez L, Bureau B, Tao H Z, Allix M, Hao Z X, Seznec V, Zhang X H, Zhao X H 2010 Phys. Chem. Chem. Phys. 12 3780
[9] Lin C G, Tao H Z, Pan R K, Zheng X L, Dong G P, Zang H C, Zhao X J 2008 Chem. Phys. Lett. 460 125
[10] Delaizir G, Lucas P, Zhang X, Ma H, Bureau B, Lucas J 2007 J. Am. Ceram. Soc. 90 2073
[11] Lin C G, Dai S X, Liu C, Song B A, Xu Y S, Chen F F, Heo J 2012 Appl. Phys. Lett. 100 231910
[12] Itzhaik Y, Niitsoo O, Page M, Hodes G 2009 J. Phys. Chem. C 113 4254
[13] Lou W J, Chen M, Wang X B, Liu W M 2007 Chem. Mater. 19 872
[14] Yang J, Liu Y C, Lin H M, Chen C C 2004 Adv. Mater. 16 713
[15] Xiao X D, Liu Q M, Dong G P, Zhao X J 2007 Opt. Commun. 274 456
[16] Lin C G, Li Z B, Ying L, Xu Y S, Zhang P Q, Dai S X, Xu T F, Nie Q H 2012 J. Phys. Chem. C 116 5862
[17] Lin C G, Calvez L, Rozé M, Tao H Z, Zhang X H, Zhao X J 2009 Appl. Phys. A 97 713
[18] Bansal N, Hyatt M 1989 J. Mater. Res. 4 1257
[19] Johnson W, Mehl R 1939 Trans. Am. Inst. Min. Metall. Eng. 135 416
[20] Avrami M 1939 J. Chem. Phys. 7 1103
[21] Avrami M 1940 J. Chem. Phys. 8 212
[22] Ozawa T 1971 Polymer 12 150
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