Fe_（78）Si_9B_（13）非晶合金低频磁脉冲处理效应及其经验电子理论研究
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摘要
纳米晶弥散分布于非晶载体的铁基软磁合金一般通过快速冷凝非晶相的部分反玻璃化来制备。为了优化这一新型纳米合金的软磁性能,可以通过控制晶化程度改变晶粒尺寸、体积分数等实现。因此非晶-纳米晶双相合金的制备和性能研究引起了国内外学者的广泛兴趣,成为近年来软磁材料研究的热点。
本论文采用低频磁脉冲处理非晶Fe78Si9B13制得了非晶-纳米晶双相合金,采用穆斯堡尔谱、XRD、TEM、DSC等手段对低频磁脉冲处理前后的样品进行微结构和性能测定,利用DSC曲线和Kissinger方程计算相变过程的激活能,研究低频磁脉冲处理非晶合金的相变热力学和动力学。再借助于EET理论和非晶合金的微晶模型,建立非晶相和晶化相的结构模型,采用BLD法计算非晶Fe78Si9B13合金晶化前后的相结构因子、界面结构因子和某些物理参数,并与实测值比较,从而确定磁脉冲参数(如场强Hp、频率fP、时间t等)与析出量、结构等与性能之间的关系,从电子层次探讨非晶合金磁致低温纳米晶化的微观机制。
研究结果表明,在低频磁脉冲处理过程中,试样的最大温升At<10℃,而且内部和外部温升差别不大,不存在高温和瞬间高温,具有较好的温度均匀性。因此,用低频磁脉冲处理非晶合金并使之在低温发生纳米晶化既不同于普通的等温退火,也克服了电脉冲处理中由于焦耳热效应而导致的温升过高的缺点,是继电脉冲处理后又一种新的方法,其特点体现在脉冲磁场强度、脉冲频率和脉冲处理时间的协同作用。
在低频磁脉冲作用下,非晶Fe78Si9B13合金的晶化量和磁矩值均与磁脉冲处理参数有关,且随着磁场强度和处理时间的增加,晶化量和磁矩值均呈线性增加；而随脉冲频率的增加却呈非单调变化。对应本研究的磁脉冲处理条件,30-35Hz为最佳频率范围。同时低频磁脉冲处理后的样品发生纳米晶化,导致其超精细磁场发生变化,原始非晶样品的超精细磁场为单峰分布,且超精细磁场值较大,约为260kOe左右。而低频磁脉冲处理后的样品的超精细磁场单峰向低位场移动,在高位场也有出现另一单峰的迹象,脉冲处理参数不同,各峰出现的位置不同。
磁脉冲处理非晶Fe,8Si9B13合余发生纳米晶化过程的DSC曲线上出现两个放热峰,说明发生了两次相转变,且转变方式为初晶晶化,析出的晶化相为单相b.c.cα-Fe(Si)。将DSC曲线上第一放热峰的峰顶温度利用Kissinger方程进行处理,再用最小二乘法拟合,得出原始非晶Fe78Si9B13合金样品的第一放热峰的激活能为433.6 kJ/mol；磁致低温纳米晶化后的非晶Fe78Si9B13合金样品的第一放热峰的激活能均在219.3 kJ/mol以下,与原始非晶Fe78Si9B13合金相比,相变激活能大幅度降低,说明低频磁脉冲处理后的样品的相变势垒减小,相变更容易发生。这是由于在脉冲磁场作用下,非晶合金晶化前后样品的微结构发生了改变,临界形核半径rc、临界形核自由能ΔGc降低,而形核率Ⅰ增大,使形核长大容易,从而促进非晶合金晶化。
利用经验电子理论(EET理论)中的BLD方法计算了磁脉冲处理前后非晶相和晶化相的价电子结构,根据非晶Fe78Si9B13合金中原子的比例和相结构因子nA以及各个晶胞铁原子对非晶Fe78Si9B13合金磁矩的贡献,建立了非晶相和晶化相总磁矩计算的经验公式,计算出了非晶相的总磁矩为1.895μB,晶化相的总磁矩为2.5579μB。再根据晶化相和非晶相的组成及磁矩计算出了磁致低温纳米晶化后的双相合金的磁矩值,并与实测值进行比较,其理论计算值与实验测定值的误差均小于10%,说明在一级近似下,从价电子层次上计算非晶的磁矩是可以实现的,这对于优化非晶Fe78SigB13合金的软磁性能将具有理论指导意义。但其磁矩值与脉冲磁场处理参数之间的关系还有待于进一步的研究。
计算了与非晶相和晶化相性能有关的异相界面价电子结构参数P(hk1)、P(uvw)、Δp等；并利用相结构因子和界面结合因子解释了非晶Fe78Si9B13合金磁致低温纳米晶化的微观机理。对于非晶Fe78Si9B13合金,非晶基体中的a-Fe的nA值最小,相变驱动力最小,形核率最大,所以α-Fe晶体首先析出；其次是α-Fe-Si,所以在α-Fe之后也随之析出,形成α-Fe(Si)固溶体。而且非晶相α-Fe类(110)//晶化相α-Fe(110)面、非晶相α-Fe类(110)//晶化相α-Fe-Si(110)面、非晶相α-Fe-Si类(110)//晶化相α-Fe-Si(110)面和晶化相α-Fe(110)//晶化相α2-Fe-Si (110)面均满足一级近似下的电子密度连续,且两侧的电子密度都很高,当脉冲磁场处理时,非晶基体中的那些具有位相关系的电子密度高、密度差小的面便通过扩散实现有序化,形成α-Fe和α-Fe(Si)晶核。然后通过粒子相界面的推移、相界面积增加的过程实现晶粒的长大。若相界面的电子密度差越大,界面上的原子尺寸变化越大,界面上的原子状态与相内的原子状态变化越剧烈,相界面的推移阻力越大,晶粒长大越困难,即电子密度差使它们的聚集、长大受阻,所以脉冲磁场作用下的晶化只能形成细小的α-Fe(Si)晶化相且弥散分布于剩余非晶基体中。
Fe-based soft magnetic alloys containing nanocrystalline precipitates embedded in an amorphous matrix are generally prepaared by partial devitrification of rapidly solidified amorphous phase. In order to improve the soft magnetic properties of the double-phase nanocrystalline alloy, the grain sizes and volume fractions of the nanocrystalline will be adjusted by controlling the crystallization process. Therefore, the research on the formation and properties of the double-phase nanocrystalline alloy has attracted widespread attention in recent years and become a focus in soft magnetic materials.
In this thesis the low frequency pulse magnetic field (LFPMF) treatment was adopted to nanocrystallize Fe78Si9B13 amorphous alloy to form the double-phase alloy. The microstructures and properties of untreated as well as treated alloys were examined by Mossbauer spectra, X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential scanning calorimetric (DSC). The activation energy in phase transition process was determined through DSC profiles by Kissinger's equation, and phase transformation thermodynamics and kinetics in nanocrystallization of amorphous alloy treated by LFPMF were studied. Then the models of amorphous and microcrystalline phase were established with the empirical electron theory (EET) and the microcrystalline model of amorphous alloy. The phase structure factors, interface structure factors and some other physical parameters of the Fe78Si9B13 amorphous alloys before and after the LFPMF treatment were calculated with BLD method and compared with the experimental values. The effect of magnetic pulses parameters, such as field intensity Hp, frequency fp, time t, etc., on the amount of nanocrystalline, the structure and properties of the alloy was determined. And the micromechanism in nanocrystallization of amorphous alloy by LFPMF treatment was discussed in the electronic level.
Experimental results showed that the maximum temperature risingΔt in the LFPMF treatment process is no more than 10℃. and the internal and external temperature rising did not show significant difference. There did not exist high temperature or transient high temperature and temperature uniformity was good. Therefore, the LFPMF treatment on amorphous alloy for nanocrystallization at low temperatures is an innovative process because it is not only different from ordinary isothermal annealing, and also superior to the pulse electric field treatment in which the Joule heating effect always cause a high temperature rising.
Treated by pulse magnetic field, the amount of crystalline and the magnetic moment of the Fe78Si9B13 alloys increased linearly with the magnetic field intensity and treating time, but did not show determined tendency with the magnetic field frequency. The optimal frequency range in this study was determined as 30-35Hz. At the same time, the hyperfine magnetic field of the alloy was affected after the LFPMF treatment due to the occurrence of nanocrystallization. The distribution of hyperfine magnetic field of the original amorphous samples is a single-peak located at about 260kOe. After the LFPMF treatment, this single-peak shifted to lower magnetic field and there was a sign of appearance of another single-peak at higher magnetic field. The peaks position varied with the pulse magnetic field parameters.
There appeared two exothermic peaks in the DSC profiles in the nanocrystallization process of Fe78Si9B13 alloy treated by LFPMF, indicating that two phase transitions took place and the transformation were both primary crystallization. The crystallized phase was single-phase b.c.c a-Fe(Si). The activation energy of the first exothermic peak of the original Fe78Si9B13 amorphous alloy was determined by Kissinger's equation as 433.6 kJ/mol. While the activation energy was only less than 219.3 kJ/mol when treated by LFPMF. The sharp decrease of the activation energy implied that the phase transition barrier was reduced and phase transition took place more easily when treated by LFPMF. This may be ascribed to that the LFPMF treatment decreases the critical nucleating radius rc, the critical nucleating free energyΔGc, increase of the nucleation rateⅠ, and then faster nucleation and growth, thus promoted the crystallizations of the amorphous alloys.
The covalence electronic structures of amorphous and crystalline phases before and after LFPMF treatment were calculated using the bond length difference (BLD) method in the empirical electron theory (EET). The empirical calculation formula of the total magnetic moment were established according to the atoms proportions, phase structure factor nA and the contribution of each cell iron atoms to the magnetic moment of the Fe78Si9B13 alloy. The total magnetic moment of amorphous phase was calculated as 1.895μB and that of crystallized phase was 2.5579μB-Then the magnetic moment of the double-phase alloys after the nanocrystallization by LFPMF treatment was calculated based on the alloy composition and the total magnetic moment obtained above, and compared with experimental values. The error of these two is less than 10%, indicating that it is possible and reliable to calculate the magnetic moment of amorphous alloy from covalence electronic level in the first approximation. This can be applied to guide the optimization of soft magnetic properties of Fe78Si9B13 amorphous alloy. But the relationship between the magnetic moment and pulse magnetic filed parameters require further investigation.
The out-of-phase interface valence electron parameters (P(hkl),P(uvw) andΔp, etc), those are related to the properties of amorphous and crystalline phases, were calculated and the micromechanism of nanocrystallization of Fe7gSi9B13 alloy by LFPMF treatment was explained using phase structure factor and interface conjunction factors. For Fe78Si9B13 amorphous alloy, the nA ofα-Fe in amorphous matrix is smaller than the others, then the driving force of phase transition is smaller while the nucleation rate is larger. Soα-Fe crystal is first crystallized. And then isα-Fe-Si crystal. They form a-Fe(Si) solid solution. Moreover, the electronic densities of the amorphous a-Fe (110) planes//crystallized a-Fe (110) planes, amorphous a-Fe (110) planes//crystallized a-Fe-Si (110) planes, amorphous a-Fe-Si (110) planes//crystallizedα-Fe-Si (110) planes, crystallized a-Fe (110) planes//crystallizedα-Fe-Si (110) planes are continuous under the first approximation, and the electronic density of both sides are high. When Fe78Si9B13 amorphous alloy was treated by LFPMF, the planes with certain phase difference and high electronic density, small density difference in the amorphous matrix can be ordered by diffusion and form the crystal nucleus of a-Fe andα-Fe(Si). Then with the movement of particle phase interface and the increase of phase interface area, the grains grow up. If the electronic density difference of phase interface is larger, the change of atomic size on interface will be more significant, the atoms states on interface or in phase will change much more, the resistance of interface movement will be higher, the grain's growth will be more difficult. In another word, the electron density difference makes their accumulation and growth inhibited. Therefore, the crystallization under pulse magnetic field can only form tiny crystallized phase a-Fe-(Si) well dispersed in the amorphous matrix.
本论文采用低频磁脉冲处理非晶Fe78Si9B13制得了非晶-纳米晶双相合金,采用穆斯堡尔谱、XRD、TEM、DSC等手段对低频磁脉冲处理前后的样品进行微结构和性能测定,利用DSC曲线和Kissinger方程计算相变过程的激活能,研究低频磁脉冲处理非晶合金的相变热力学和动力学。再借助于EET理论和非晶合金的微晶模型,建立非晶相和晶化相的结构模型,采用BLD法计算非晶Fe78Si9B13合金晶化前后的相结构因子、界面结构因子和某些物理参数,并与实测值比较,从而确定磁脉冲参数(如场强Hp、频率fP、时间t等)与析出量、结构等与性能之间的关系,从电子层次探讨非晶合金磁致低温纳米晶化的微观机制。
研究结果表明,在低频磁脉冲处理过程中,试样的最大温升At<10℃,而且内部和外部温升差别不大,不存在高温和瞬间高温,具有较好的温度均匀性。因此,用低频磁脉冲处理非晶合金并使之在低温发生纳米晶化既不同于普通的等温退火,也克服了电脉冲处理中由于焦耳热效应而导致的温升过高的缺点,是继电脉冲处理后又一种新的方法,其特点体现在脉冲磁场强度、脉冲频率和脉冲处理时间的协同作用。
在低频磁脉冲作用下,非晶Fe78Si9B13合金的晶化量和磁矩值均与磁脉冲处理参数有关,且随着磁场强度和处理时间的增加,晶化量和磁矩值均呈线性增加；而随脉冲频率的增加却呈非单调变化。对应本研究的磁脉冲处理条件,30-35Hz为最佳频率范围。同时低频磁脉冲处理后的样品发生纳米晶化,导致其超精细磁场发生变化,原始非晶样品的超精细磁场为单峰分布,且超精细磁场值较大,约为260kOe左右。而低频磁脉冲处理后的样品的超精细磁场单峰向低位场移动,在高位场也有出现另一单峰的迹象,脉冲处理参数不同,各峰出现的位置不同。
磁脉冲处理非晶Fe,8Si9B13合余发生纳米晶化过程的DSC曲线上出现两个放热峰,说明发生了两次相转变,且转变方式为初晶晶化,析出的晶化相为单相b.c.cα-Fe(Si)。将DSC曲线上第一放热峰的峰顶温度利用Kissinger方程进行处理,再用最小二乘法拟合,得出原始非晶Fe78Si9B13合金样品的第一放热峰的激活能为433.6 kJ/mol；磁致低温纳米晶化后的非晶Fe78Si9B13合金样品的第一放热峰的激活能均在219.3 kJ/mol以下,与原始非晶Fe78Si9B13合金相比,相变激活能大幅度降低,说明低频磁脉冲处理后的样品的相变势垒减小,相变更容易发生。这是由于在脉冲磁场作用下,非晶合金晶化前后样品的微结构发生了改变,临界形核半径rc、临界形核自由能ΔGc降低,而形核率Ⅰ增大,使形核长大容易,从而促进非晶合金晶化。
利用经验电子理论(EET理论)中的BLD方法计算了磁脉冲处理前后非晶相和晶化相的价电子结构,根据非晶Fe78Si9B13合金中原子的比例和相结构因子nA以及各个晶胞铁原子对非晶Fe78Si9B13合金磁矩的贡献,建立了非晶相和晶化相总磁矩计算的经验公式,计算出了非晶相的总磁矩为1.895μB,晶化相的总磁矩为2.5579μB。再根据晶化相和非晶相的组成及磁矩计算出了磁致低温纳米晶化后的双相合金的磁矩值,并与实测值进行比较,其理论计算值与实验测定值的误差均小于10%,说明在一级近似下,从价电子层次上计算非晶的磁矩是可以实现的,这对于优化非晶Fe78SigB13合金的软磁性能将具有理论指导意义。但其磁矩值与脉冲磁场处理参数之间的关系还有待于进一步的研究。
计算了与非晶相和晶化相性能有关的异相界面价电子结构参数P(hk1)、P(uvw)、Δp等；并利用相结构因子和界面结合因子解释了非晶Fe78Si9B13合金磁致低温纳米晶化的微观机理。对于非晶Fe78Si9B13合金,非晶基体中的a-Fe的nA值最小,相变驱动力最小,形核率最大,所以α-Fe晶体首先析出；其次是α-Fe-Si,所以在α-Fe之后也随之析出,形成α-Fe(Si)固溶体。而且非晶相α-Fe类(110)//晶化相α-Fe(110)面、非晶相α-Fe类(110)//晶化相α-Fe-Si(110)面、非晶相α-Fe-Si类(110)//晶化相α-Fe-Si(110)面和晶化相α-Fe(110)//晶化相α2-Fe-Si (110)面均满足一级近似下的电子密度连续,且两侧的电子密度都很高,当脉冲磁场处理时,非晶基体中的那些具有位相关系的电子密度高、密度差小的面便通过扩散实现有序化,形成α-Fe和α-Fe(Si)晶核。然后通过粒子相界面的推移、相界面积增加的过程实现晶粒的长大。若相界面的电子密度差越大,界面上的原子尺寸变化越大,界面上的原子状态与相内的原子状态变化越剧烈,相界面的推移阻力越大,晶粒长大越困难,即电子密度差使它们的聚集、长大受阻,所以脉冲磁场作用下的晶化只能形成细小的α-Fe(Si)晶化相且弥散分布于剩余非晶基体中。
Fe-based soft magnetic alloys containing nanocrystalline precipitates embedded in an amorphous matrix are generally prepaared by partial devitrification of rapidly solidified amorphous phase. In order to improve the soft magnetic properties of the double-phase nanocrystalline alloy, the grain sizes and volume fractions of the nanocrystalline will be adjusted by controlling the crystallization process. Therefore, the research on the formation and properties of the double-phase nanocrystalline alloy has attracted widespread attention in recent years and become a focus in soft magnetic materials.
In this thesis the low frequency pulse magnetic field (LFPMF) treatment was adopted to nanocrystallize Fe78Si9B13 amorphous alloy to form the double-phase alloy. The microstructures and properties of untreated as well as treated alloys were examined by Mossbauer spectra, X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential scanning calorimetric (DSC). The activation energy in phase transition process was determined through DSC profiles by Kissinger's equation, and phase transformation thermodynamics and kinetics in nanocrystallization of amorphous alloy treated by LFPMF were studied. Then the models of amorphous and microcrystalline phase were established with the empirical electron theory (EET) and the microcrystalline model of amorphous alloy. The phase structure factors, interface structure factors and some other physical parameters of the Fe78Si9B13 amorphous alloys before and after the LFPMF treatment were calculated with BLD method and compared with the experimental values. The effect of magnetic pulses parameters, such as field intensity Hp, frequency fp, time t, etc., on the amount of nanocrystalline, the structure and properties of the alloy was determined. And the micromechanism in nanocrystallization of amorphous alloy by LFPMF treatment was discussed in the electronic level.
Experimental results showed that the maximum temperature risingΔt in the LFPMF treatment process is no more than 10℃. and the internal and external temperature rising did not show significant difference. There did not exist high temperature or transient high temperature and temperature uniformity was good. Therefore, the LFPMF treatment on amorphous alloy for nanocrystallization at low temperatures is an innovative process because it is not only different from ordinary isothermal annealing, and also superior to the pulse electric field treatment in which the Joule heating effect always cause a high temperature rising.
Treated by pulse magnetic field, the amount of crystalline and the magnetic moment of the Fe78Si9B13 alloys increased linearly with the magnetic field intensity and treating time, but did not show determined tendency with the magnetic field frequency. The optimal frequency range in this study was determined as 30-35Hz. At the same time, the hyperfine magnetic field of the alloy was affected after the LFPMF treatment due to the occurrence of nanocrystallization. The distribution of hyperfine magnetic field of the original amorphous samples is a single-peak located at about 260kOe. After the LFPMF treatment, this single-peak shifted to lower magnetic field and there was a sign of appearance of another single-peak at higher magnetic field. The peaks position varied with the pulse magnetic field parameters.
There appeared two exothermic peaks in the DSC profiles in the nanocrystallization process of Fe78Si9B13 alloy treated by LFPMF, indicating that two phase transitions took place and the transformation were both primary crystallization. The crystallized phase was single-phase b.c.c a-Fe(Si). The activation energy of the first exothermic peak of the original Fe78Si9B13 amorphous alloy was determined by Kissinger's equation as 433.6 kJ/mol. While the activation energy was only less than 219.3 kJ/mol when treated by LFPMF. The sharp decrease of the activation energy implied that the phase transition barrier was reduced and phase transition took place more easily when treated by LFPMF. This may be ascribed to that the LFPMF treatment decreases the critical nucleating radius rc, the critical nucleating free energyΔGc, increase of the nucleation rateⅠ, and then faster nucleation and growth, thus promoted the crystallizations of the amorphous alloys.
The covalence electronic structures of amorphous and crystalline phases before and after LFPMF treatment were calculated using the bond length difference (BLD) method in the empirical electron theory (EET). The empirical calculation formula of the total magnetic moment were established according to the atoms proportions, phase structure factor nA and the contribution of each cell iron atoms to the magnetic moment of the Fe78Si9B13 alloy. The total magnetic moment of amorphous phase was calculated as 1.895μB and that of crystallized phase was 2.5579μB-Then the magnetic moment of the double-phase alloys after the nanocrystallization by LFPMF treatment was calculated based on the alloy composition and the total magnetic moment obtained above, and compared with experimental values. The error of these two is less than 10%, indicating that it is possible and reliable to calculate the magnetic moment of amorphous alloy from covalence electronic level in the first approximation. This can be applied to guide the optimization of soft magnetic properties of Fe78Si9B13 amorphous alloy. But the relationship between the magnetic moment and pulse magnetic filed parameters require further investigation.
The out-of-phase interface valence electron parameters (P(hkl),P(uvw) andΔp, etc), those are related to the properties of amorphous and crystalline phases, were calculated and the micromechanism of nanocrystallization of Fe7gSi9B13 alloy by LFPMF treatment was explained using phase structure factor and interface conjunction factors. For Fe78Si9B13 amorphous alloy, the nA ofα-Fe in amorphous matrix is smaller than the others, then the driving force of phase transition is smaller while the nucleation rate is larger. Soα-Fe crystal is first crystallized. And then isα-Fe-Si crystal. They form a-Fe(Si) solid solution. Moreover, the electronic densities of the amorphous a-Fe (110) planes//crystallized a-Fe (110) planes, amorphous a-Fe (110) planes//crystallized a-Fe-Si (110) planes, amorphous a-Fe-Si (110) planes//crystallizedα-Fe-Si (110) planes, crystallized a-Fe (110) planes//crystallizedα-Fe-Si (110) planes are continuous under the first approximation, and the electronic density of both sides are high. When Fe78Si9B13 amorphous alloy was treated by LFPMF, the planes with certain phase difference and high electronic density, small density difference in the amorphous matrix can be ordered by diffusion and form the crystal nucleus of a-Fe andα-Fe(Si). Then with the movement of particle phase interface and the increase of phase interface area, the grains grow up. If the electronic density difference of phase interface is larger, the change of atomic size on interface will be more significant, the atoms states on interface or in phase will change much more, the resistance of interface movement will be higher, the grain's growth will be more difficult. In another word, the electron density difference makes their accumulation and growth inhibited. Therefore, the crystallization under pulse magnetic field can only form tiny crystallized phase a-Fe-(Si) well dispersed in the amorphous matrix.
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