Fe73.5Si13.5-xGexB9Cu1Nb3(x=3, 6)非晶合金的结晶动力学*

doi:10.11901/1005.3093.2013.603

材料研究学报

2014, Vol. 28

Issue (3): 204-210 DOI: 10.11901/1005.3093.2013.603

本期目录 | 过刊浏览

Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6)非晶合金的结晶动力学^*

汪汝武^1,³(

),刘静^1,²,甘章华¹,曾春³,张凤泉³

1. 武汉科技大学材料与冶金学院武汉 430081
2. 北京科技大学新金属材料国家重点实验室北京 100083
3. 国家硅钢工程技术研究中心武汉 430080

Crystallization Kinetics of Amorphous Alloys Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6)

Ruwu WANG^1,^3,^**(

),Jing LIU^1,²,Zhanghua GAN¹,Chun ZENG³,Fengquan ZHANG³

1. College of Materials Science and Metallurgical Engineering, Wuhan University of Science and Technology, Wuhan 430081
2. State Key Laboratory for Advanced Metals and Materials, Beijing University of Science and Technology,
Beijing 100083
3. National Engineering Research Center for Silicon Steel, Wuhan 430080

引用本文:

汪汝武,刘静,甘章华,曾春,张凤泉. Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6)非晶合金的结晶动力学^*[J]. 材料研究学报, 2014, 28(3): 204-210.
Ruwu WANG, Jing LIU, Zhanghua GAN, Chun ZENG, Fengquan ZHANG. Crystallization Kinetics of Amorphous Alloys Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6)[J]. Chinese Journal of Materials Research, 2014, 28(3): 204-210.

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摘要:

用标准单辊甩带技术在大气环境下制备Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6)非晶条带, 分别在470℃、510℃、550℃和590℃对非晶条带进行真空等温退火1 h后, 在非晶基体中形成了纳米晶相。用X射线衍射(XRD), 透射电镜(TEM)和差示扫描量热法(DSC)测量研究了快淬态和热处理后样品的结构和结晶动力学。基于差热分析的数据, 使用Kissinger, Ozawa和Augis-Bennett模型计算了非晶条带的结晶激活能, 利用Johnson-Mehl-Avrami(JMA)方程计算了非晶条带初始结晶的局域Avrami因子n。局域Avrami因子n随晶化体积分数α的显著变化说明, 非晶条带非等温初始结晶的机理在不同的晶化阶段是不同的。晶化初期的机理是扩散控制的三维形核和晶粒生长的整体晶化, 形核速率逐渐减小; 晶化中后期为一维形核和生长的表面晶化过程, 形核速率近似为零。基于XRD和TEM测量结果, 分别在510℃、550℃和590℃真空等温退火1 h后, 在Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6)非晶条带中析出的α-Fe (Si, Ge)相的平均晶粒尺寸D小于15 nm。

关键词 ：材料科学基础学科, Fe_73.5Si_13.5-xGe_xB₉Cu₁Nb₃, 结构, 结晶动力学

Abstract：

Amorphous ribbons Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃(x=3, 6) were prepared by a normal single copper wheel melt spinning technique in atmosphere, which then were isothermally annealed at 470℃、510℃、550℃ and 590℃ respectively for 1 h in a vacuum furnace. The microstructure and crystallization kinetics of the ribbons were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential scanning calorimeter (DSC) measurements. While the crystallization activation energies of amorphous ribbons were calculated by using Kissinger, Ozawa and Augis-Bennett models based on differential thermal analysis data. The local Avrami exponent n for primary crystallization was calculated by using Johnson-Mehl-Avrami (JMA) equation. The significant variation of local Avrami exponent n with crystallization volume fraction α demonstrated that the primary crystallization kinetics of amorphous ribbons varied at different stages. In the initial stage, the crystallization mechanism was diffusion controlled bulk crystallization with three dimensional nucleation and grain growth, while the nucleation rate deceased with time. In the following stage, it was surface crystallization with one dimensional nucleation and grain growth, while the nucleation rate was near zero. The average sizes D of α-Fe (Si, Ge) grains for the samples annealed at 510℃、550℃ and 590℃for 1 h in a vacuum furnace were less than 15 nm as confirmed both by XRD and TEM measurements.

Key words： foundational discipline in materials science Fe_73.5Si_13.5-_xGe_xB₉Cu₁Nb₃ microstructure crystallization kinetics

收稿日期: 2013-08-16

基金资助:* 北京科技大学新金属材料国家重点实验室开放基金2011-ZD03, 湖北省教育厅D20111103资助项目。

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本文联系人: 汪汝武

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图1 Fe73.5Si13.5-xGexB9Cu1Nb3 (x=3, 6)淬态样品的XRD图谱

图2 Fe73.5Si10.5Ge3B9Cu1Nb3淬态样品在不同加热速率下的DSC曲线, 加热速率从5–20℃/min

图3 Fe73.5Si7.5Ge6B9Cu1Nb3淬态样品在不同加热速率下的DSC曲线, 加热速率从5–20℃/min

表1 据DSC曲线确定的Fe73.5Si13.5-xGexB9Cu1Nb3 (x=3, 6)非晶合金的晶化开始温度和晶化峰值温度(Tx1, Tp1和Tx2, Tp2)和ΔT=Tp2-Tp1

图4 Fe73.5Si13.5-xGexB9Cu1Nb3 (x=3, 6)淬态样品的Kissinger拟合图, R1表示一次晶化, R2表示二次晶化

图5 Fe73.5Si13.5-xGexB9Cu1Nb3 (x=3, 6)淬态样品的Ozawa拟合图, R1表示一次晶化, R2表示二次晶化

图6 Fe73.5Si13.5-xGexB9Cu1Nb3 (x=3, 6)淬态样品的Augis-Bennett拟合图, R1表示一次晶化, R2表示二次晶化

表2 Fe73.5Si13.5-xGexB9Cu1Nb3 (x=3, 6)非晶合金的晶化表观激活能, R1代表一次晶化, R2代表二次晶化

图7 Fe73.5Si13.5-xGexB9Cu1Nb3 (x=3, 6)淬态样品一次晶化峰的局域Avrami因子n随晶化分数α的变化关系, 加热速率为10℃/min

图8 Fe73.5Si10.5Ge3B9Cu1Nb3淬态样品在不同温度真空等温退火1 h后的XRD图谱

图9 Fe73.5Si7.5Ge6B9Cu1Nb3淬态样品在不同温度真空等温退火1 h后的XRD图谱

图10 Fe73.5Si7.5Ge6B9Cu1Nb3的TEM图, 淬态样品以及分别在470℃, 510℃, 550℃, 590℃保温1 h样品, 图中的插图为SAED图

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