Fe76Ga5Ge5B6P7Cu1 合金的非等温晶化动力学

doi:10.11900/0412.1961.2021.00287

金属学报

2022, Vol. 58

Issue (6): 799-806 DOI: 10.11900/0412.1961.2021.00287

研究论文

本期目录 | 过刊浏览

Fe₇₆Ga₅Ge₅B₆P₇Cu₁ 合金的非等温晶化动力学

郭璐¹^,², 朱乾科¹^,²(

), 陈哲¹^,², 张克维¹^,²(

), 姜勇¹^,²

^1.太原科技大学材料科学与工程学院太原 030024
^2.太原科技大学磁电功能材料及应用山西省重点实验室太原 030024

Non-Isothermal Crystallization Kinetics of Fe₇₆Ga₅Ge₅B₆P₇Cu₁ Alloy

GUO Lu¹^,², ZHU Qianke¹^,²(

), CHEN Zhe¹^,², ZHANG Kewei¹^,²(

), JIANG Yong¹^,²

^1.School of Materials Science and Engineering, Taiyuan University of Science and Technology, Taiyuan 030024, China
^2.Shanxi Province Key Laboratory of Magnetic and Electric Functional Materials and Their Applications, Taiyuan University of Science and Technology, Taiyuan 030024, China

引用本文:

郭璐, 朱乾科, 陈哲, 张克维, 姜勇. Fe₇₆Ga₅Ge₅B₆P₇Cu₁ 合金的非等温晶化动力学[J]. 金属学报, 2022, 58(6): 799-806.
Lu GUO, Qianke ZHU, Zhe CHEN, Kewei ZHANG, Yong JIANG. Non-Isothermal Crystallization Kinetics of Fe₇₆Ga₅Ge₅B₆P₇Cu₁ Alloy[J]. Acta Metall Sin, 2022, 58(6): 799-806.

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摘要:

采用单辊旋淬法制备了Fe₇₆Ga₅Ge₅B₆P₇Cu₁带材,并研究了其晶化行为和机理。结果表明Fe₇₆Ga₅Ge₅B₆-P₇Cu₁合金的晶化过程分为2个阶段,第1个阶段为α-Fe(Ga, Ge)相的析出,第2个阶段为Fe(B, P)硬磁相的析出。在非等温加热的情况下,初始表观激活能大于晶化表观激活能。根据Johnson-Mehl-Avrami-Kolmogorov (JMAK)方程得出,对于非完全非晶结构的合金,其晶化过程为预先存在的晶核或团簇不断长大,同时伴随着新的晶核不断析出且形核率不断下降。此外,快速升温的退火工艺更适合形成均匀弥散的纳米晶组织。通过实验验证,退火时升温速率为100 K/min的合金软磁性能优于升温速率为10和50 K/min的合金,其最优起始磁导率为2.86 × 10^-2 H/m,矫顽力为1.77 A/m。

关键词 ：非等温晶化动力学, α-Fe(Ga, Ge), JMAK方程, Avrami指数, 矫顽力

Abstract：

Fe-based amorphous and nanocrystalline alloys can be used for technological applications on iron core materials owing to their high permeability, low coercivity, and core loss. However, when compared to Si-steels, their application is limited owing to low saturation magnetization. Thus, the saturation magnetization of Fe-based amorphous and nanocrystalline alloys should be improved, which may reduce the content of metalloid elements, and thus, the amorphous forming ability. Consequently, as-spun Fe-based amorphous and nanocrystalline alloys with high saturation magnetization may be incompletely amorphous. In this case, annealing processes should be modified by investigating crystallization behavior because traditional annealing processes with low heating rates may degrade ferromagnetic exchange and soft magnetic properties owing to grain-size inhomogeneity. Fe₇₆Ga₅Ge₅B₆P₇Cu₁ ribbons were fabricated using the melt spinning technique, and their crystallization behavior and mechanism were studied. Results showed that two exothermic peaks are present in the DSC curve, which correspond to the precipitation of α-Fe(Ga, Ge) and Fe(B, P) phases. Under nonisothermal conditions, the initial activation energy is greater than the apparent activation energy. According to the Johnson-Mehl-Avrami-Kolmogorov (JMAK) equation, for an incomplete amorphous alloy, the crystallization process combines the growth of pre-existing nucleus and nucleation, whereas the nucleation rate decreases. Moreover, a rapid heating annealing process is conducive to the formation of a uniform and dispersed nanocrystalline structure. It was found that the magnetic properties of the annealed alloy with a heating rate of 100 K/min was better than those with 10 and 50 K/min. Further, the optimal initial permeability was 2.86 × 10^-2 H/m, and the coercivity was 1.77 A/m.

Key words： non-isothermal crystallization kinetics α-Fe(Ga, Ge) JMAK equation Avrami index coercivity

收稿日期: 2021-07-12

ZTFLH:

TM271

基金资助:山西省回国留学人员科研教研项目(HGKY2019083);山西省重点研发计划(国际合作)项目(201803D421046);山西省高等学校科技创新项目(2021L293);来晋工作优秀博士奖励资金项目(20212045);太原科技大学博士启动金项目(20202034)

作者简介: 张克维, drzkw@126.com,主要从事磁性功能材料研究朱乾科, drzhuqianke@126.com,主要从事磁性功能材料研究
郭璐,女,1989年生,博士生

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图1 淬态Fe76Ga5Ge5B6P7Cu1合金的XRD谱,在不同加热速率下的DSC曲线、特征温度(Tx1、Tp1、Tx2、Tp2)随lnβ (β为加热速率)变化的拟合曲线,以及Fe76Ga5Ge5B6P7Cu1合金不同温度退火后的XRD谱

表1 淬态Fe76Ga5Ge5B6P7Cu1在不同加热速率下的特征温度 (K)

图2 淬态Fe76Ga5Ge5B6P7Cu1合金采用Kissinger和Ozawa方程的拟合图

图3 在不同的加热速率下第1个峰和第2个峰晶化体积分数(α)随温度的变化

图4 第1个峰和第2个峰的Avrami指数(n)随α的变化

表2 第1个峰晶化机理的表征参数

表3 第2个峰晶化机理的表征参数

图5 不同升温速率下起始磁导率(μi)和矫顽力(Hc)随退火温度的变化

图6 升温速率10 K/min、退火温度400℃和升温速率100 K/min、退火温度425℃时Fe76Ga5Ge5B6P7Cu1合金退火后的TEM像、SAED花样和晶粒尺寸分布及晶化示意图

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