Fe_（90）Zr_7B_3在空气中的动力学行为研究及性能的变化
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摘要
铁基非晶态合金与传统晶体材料相比,因具有优良的软磁性能、极高的强度、硬度以及优异的物理化学性能作为一种新型材料而倍受人们的关注。铁基金属玻璃应用广泛,可以被用作微电子线圈和软磁管。为了在不同温度下使用铁基非晶态合金,对氧化行为的研究显得十分必要。一些学者已经开始了对铁基非晶合金氧化行为的研究。我们对条带进行了表面的轻微氧化处理,以模拟和讨论实际使用过程中氧化带来的变化。
本论文主要工作包括五个方面: l、利用单辊技术制备了铁基非晶态合金Fe_(90)Zr_7B_3条带,分别用X射线衍射(XRD)、差热量分析仪(DSC)和热重分析仪(TG)研究了合金的相结构、热量和重量变化。借助X射线衍射分析证实为非晶态结构,DSC测试分析表明非晶态合金的晶化温度Tx为512.8℃;2、在不同的加热速率下测量了非晶态合金Fe_(90)Zr_7B_3在空气中的氧化曲线,测试表明合金的开始氧化温度Tonset为637.8℃,并利用Kissinger方程计算得到了合金的活化能,其值为483 kJ/mol;3、在空气条件下,T=600℃时,样品的质量开始明显增加。从室温到1100℃,样品的质量增重有三个明显的阶段。这三个明显的增重阶段与合金的组成元素及其质量含量有关,并了解了合金在整个过程中的氧化分数;4、利用X射线衍射(XRD)分析了非晶态合金Fe_(90)Zr_7B_3在空气中不同温度下短期氧化后的物相结构,并讨论了短期氧化后样品与原始样品热重曲线的区别;5、选择在玻璃化温度Tg附近的不同温度等温处理相同时间和在同一温度对样品进行不同时间氧化处理后,测量了样品的磁性能。测试结果表明原样品具有良好的软磁性能,在低于玻璃化温度短期热处理或低温较长时间热处理后,合金的磁性能相对变化较小,在450℃氧化15 min后合金的磁滞回线发生了改变。讨论了合金随着氧化温度的提高和氧化时间的增长磁性能的变化趋势。氧化处理提高了合金的比饱和磁化强度σs,但同时比剩余磁化强度σr和矫顽力的值也变大了。
Fe-base amorphous alloy have got people’s attention and been considered for use in many commercial components because of their excellent soft magical property, excellent strength, stiffness and better physical/chemical properties, as compared to traditional crystalline alloys.Fe-base amorphous alloy are of particular applications, such as micro-electronic cores and soft magnet tubes. In order to use Fe-base amorphous alloy for different temperature applications, a profound understanding of the oxidation behavior is essential. Fe_(90)Zr_7B_3 amorphous alloy have been used in industry for their excellent magnetic properties, it’s necessary to understand the oxidation behavior at high temperature in different atmosphere. Some papers have already mentioned the oxidation of Fe-base amorphous alloy. We conducted a band of minor surface oxidation to simulate and discuss the actual use of the process of change brought about by oxidation.
This article mainly introduced five aspects work. First of all, Fe_(90)Zr_7B_3 amorphous alloy was prepared by single-rolling method and its structure, glass-forming ability and thermal stability were also studied by use of X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetry analyzer (TG). It showed the alloy was amorphous and the crystallization of the alloy was 512.8℃. Secondly, non-isothermal oxidation studies of Fe_(90)Zr_7B_3 amorphous alloy were carried out in air at different heating rates and its relative oxidation behavior was studied. The onset temperature of the alloy was 637.8℃and the alloy was very stable under 480℃. The activation energy of the Fe_(90)Zr_7B_3 amorphous ribbons was calculated by Kissinger plot. And the activation energy value of the alloy was 483 kJ/mol. Thirdly,the weight gains began at 600℃and finished at 1100℃. The tg curves of the alloy in air showed the oxidation of the alloy had three stages. And it may be related to the components of the alloy. It also showed the oxidation fracture of the alloy in the total oxidation stage. Fourthly, the structures of the alloy heat treatment for short time at different temperture were studied by X-ray diffraction. The TGA curves’s difference between the the original sample and the sample heat treatment after a short-term oxidation were discussed. At last, the magnetic properties of the alloy were measured after heat treatment at different temperature for different times. Also, the heat treatment temperature was near or below the glass-forming temperature. The results showed the magnetic properties changed little at lower temperature and it related to the amorphous state of the alloy. The hysteresis loops of Fe_(90)Zr_7B_3 amorphous alloy heat treatment at 450℃for 15 min has changed. The changes of the alloy’s magnetic properties with the oxidation temperature and oxidation time were discussed. The values of saturation magnetization were improved by oxidation, but the values of residual magnetization and coercivity of the alloy were enlarged at the same time.
本论文主要工作包括五个方面: l、利用单辊技术制备了铁基非晶态合金Fe_(90)Zr_7B_3条带,分别用X射线衍射(XRD)、差热量分析仪(DSC)和热重分析仪(TG)研究了合金的相结构、热量和重量变化。借助X射线衍射分析证实为非晶态结构,DSC测试分析表明非晶态合金的晶化温度Tx为512.8℃;2、在不同的加热速率下测量了非晶态合金Fe_(90)Zr_7B_3在空气中的氧化曲线,测试表明合金的开始氧化温度Tonset为637.8℃,并利用Kissinger方程计算得到了合金的活化能,其值为483 kJ/mol;3、在空气条件下,T=600℃时,样品的质量开始明显增加。从室温到1100℃,样品的质量增重有三个明显的阶段。这三个明显的增重阶段与合金的组成元素及其质量含量有关,并了解了合金在整个过程中的氧化分数;4、利用X射线衍射(XRD)分析了非晶态合金Fe_(90)Zr_7B_3在空气中不同温度下短期氧化后的物相结构,并讨论了短期氧化后样品与原始样品热重曲线的区别;5、选择在玻璃化温度Tg附近的不同温度等温处理相同时间和在同一温度对样品进行不同时间氧化处理后,测量了样品的磁性能。测试结果表明原样品具有良好的软磁性能,在低于玻璃化温度短期热处理或低温较长时间热处理后,合金的磁性能相对变化较小,在450℃氧化15 min后合金的磁滞回线发生了改变。讨论了合金随着氧化温度的提高和氧化时间的增长磁性能的变化趋势。氧化处理提高了合金的比饱和磁化强度σs,但同时比剩余磁化强度σr和矫顽力的值也变大了。
Fe-base amorphous alloy have got people’s attention and been considered for use in many commercial components because of their excellent soft magical property, excellent strength, stiffness and better physical/chemical properties, as compared to traditional crystalline alloys.Fe-base amorphous alloy are of particular applications, such as micro-electronic cores and soft magnet tubes. In order to use Fe-base amorphous alloy for different temperature applications, a profound understanding of the oxidation behavior is essential. Fe_(90)Zr_7B_3 amorphous alloy have been used in industry for their excellent magnetic properties, it’s necessary to understand the oxidation behavior at high temperature in different atmosphere. Some papers have already mentioned the oxidation of Fe-base amorphous alloy. We conducted a band of minor surface oxidation to simulate and discuss the actual use of the process of change brought about by oxidation.
This article mainly introduced five aspects work. First of all, Fe_(90)Zr_7B_3 amorphous alloy was prepared by single-rolling method and its structure, glass-forming ability and thermal stability were also studied by use of X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetry analyzer (TG). It showed the alloy was amorphous and the crystallization of the alloy was 512.8℃. Secondly, non-isothermal oxidation studies of Fe_(90)Zr_7B_3 amorphous alloy were carried out in air at different heating rates and its relative oxidation behavior was studied. The onset temperature of the alloy was 637.8℃and the alloy was very stable under 480℃. The activation energy of the Fe_(90)Zr_7B_3 amorphous ribbons was calculated by Kissinger plot. And the activation energy value of the alloy was 483 kJ/mol. Thirdly,the weight gains began at 600℃and finished at 1100℃. The tg curves of the alloy in air showed the oxidation of the alloy had three stages. And it may be related to the components of the alloy. It also showed the oxidation fracture of the alloy in the total oxidation stage. Fourthly, the structures of the alloy heat treatment for short time at different temperture were studied by X-ray diffraction. The TGA curves’s difference between the the original sample and the sample heat treatment after a short-term oxidation were discussed. At last, the magnetic properties of the alloy were measured after heat treatment at different temperature for different times. Also, the heat treatment temperature was near or below the glass-forming temperature. The results showed the magnetic properties changed little at lower temperature and it related to the amorphous state of the alloy. The hysteresis loops of Fe_(90)Zr_7B_3 amorphous alloy heat treatment at 450℃for 15 min has changed. The changes of the alloy’s magnetic properties with the oxidation temperature and oxidation time were discussed. The values of saturation magnetization were improved by oxidation, but the values of residual magnetization and coercivity of the alloy were enlarged at the same time.
引文
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