异质金属体系扩散行为和界面反应的强磁场控制研究
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摘要
强磁场作为一种极端条件,以其独特的非接触性、方向性、显著的磁化能量和磁化力效果,对金属材料制备的各种过程,如固态相变、晶界迁移、再结晶、凝固、化学反应等都有明显的影响。这些过程又都与原子的扩散行为息息相关。扩散是物质传输的重要方式,是控制材料的微观组织和性能的重要因素,在金属或合金的各种物理化学处理中起到基本作用。因此研究强磁场对扩散的影响机制是阐明其对材料组织作用机理的前提和基础。
本文在12T超导强磁场装置中实验研究了固态Cu/固态Ni、液态Bi/固态Bi0.4Sb0.6(互溶扩散)、液态Al (Zn)/固态Cu(反应扩散)、气态A1/固态Cu等扩散偶中的互扩散行为和界面反应,较系统地考察了强磁场的强度、方向、梯度等参数对扩散层组织的演化过程的影响。通过考察界面迁移距离、扩散层厚度等从动力学角度计算强磁场下有效扩散系数,并且从热力学角度获得强磁场条件下的扩散常数和扩散激活能。从磁自由能和磁场力学效果出发对实验现象进行理论分析,初步探讨了强磁场对异质界面扩散行为的影响规律和作用机制。得到以下主要结果：
(1)磁场方向与扩散方向平行时,随着磁场强度的增加,固态Cu/固态Ni界面处扩散层厚度和柯肯达尔标记间的距离都显著增加。但当磁场强度超过某一值后,磁场强度的进一步增大对惰性标记间的距离的影响变小,表明磁场强度的影响趋于饱和。不同磁场强度下,利用俣野平面法结合Darken方程计算的互扩散系数结果表明,强磁场促进了Cu、Ni之间的互扩散。但是,垂直于扩散方向的磁场对固态Cu/固态Ni扩散偶中的柯肯达尔效应几乎没有影响；“负向”梯度强磁场显著抑制了Cu、Ni之间的互扩散。
(2)无论有无强磁场作用,液态Bi/固态Bi0.4Sb0.6中界面迁移距离和扩散时间之间都存在抛物线规律,但是随着磁场强度的增大界面迁移距离显著减小,11.5T磁场下的界面迁移距离比无磁场作用时甚至减小了1200μm,表明强磁场强烈的抑制了液态金属与固态合金之间的扩散迁移行为。磁场下有效扩散系数显著减小应归功于强磁场使液相黏度增加,增大了原子的扩散激活能。梯度磁场条件下的实验结果表明,无论磁场梯度的方向是正或负,其扩散阻碍作用都比均恒磁场的作用效果更显著。
(3)实验研究了强磁场对液态Al(Zn)/固态Cu中发生的界面反应扩散的影响,发现施加强磁场不会改变界面扩散层的形貌和相组成,但是随着磁场强度在0-12T范围内改变,扩散层厚度呈现先减小后增大再减小的非线性变化规律,Al元素和Zn元素的物性差异导致扩散层厚度极大值分别对应于磁场强度8.8T和8T。另外,平行磁场方向的扩散层总是厚于垂直磁场方向的扩散层。分析表明强磁场抑制自然对流和诱发热电磁对流两方面作用产生了上述实验结果。理论推导的强磁场条件下的扩散定律结果表明,有效扩散系数随磁场强度非线性变化,与实验结果吻合的很好。对扩散层生长过程的热力学分析表明,11.5T强磁场增大了原子扩散激活能,导致扩散系数较无磁场作用时显著降低。与液态Bi/固态Bi0.4Sb0.6中的实验结果相似,梯度强磁场显著抑制了液态Al (Zn)/固态Cu系统中的反应扩散行为。
(4)在1173K保温4.5小时的纯铜表面气相渗铝实验中施加强磁场,发现强磁场诱导基体Cu表面最终产物的形貌、结构、相组成发生了显著变化。磁场强度从0T到8.8T范围内,表面渗层由α+γ2和α两层结构组成,但是当磁场强度(≥10T)时,渗层仅由含有大量kirkendall空穴的α层组成。随着磁场强度的增大,渗层厚度显著增加并在磁场强度6.6T时达到最大值,但是随着磁场强度的进一步增大,渗层厚度显著减小。强磁场对化学反应和扩散行为的矛盾作用产生了以上实验结果。
本论文工作对于探索强磁场对金属材料学中各种与扩散有关的金属学现象的影响机理以及强磁场下异质界面的扩散反应行为控制具有积极意义。
Due to its unique properties of non-contact, directionality, marked magnetizability and magnetic force, a high magnetic field as one kind of extreme conditions can exert an obvious influence on the processing of many metallic materials, such as solid-state phase transformation, grain boundary migration, recrystallization, solidification, and chemical reaction. These processes mentioned above have a closely relationship with the diffusion behavior of atoms. Diffusion is an important way for mass transport process, being a key factor for the control of the microstructure and properties of materials, and playing a basic role during the process of metallurgical physical chemistry. Therefore, a detailed discussion of the effects of high magnetic field on the diffusion behavior is the precondition and foundation for the control of microstructures using a high magnetic field.
The interdiffusion behaviors and interfacial reaction in solid Cu/solid Ni, liquid Bi/solid Bi0.4Sb0.6, liquid Al(Zn)/solid Cu, and gas Al/solid Cu diffusion couples have been experimentally studied under high magnetic field of up to 12T. The effects of magnetic flux density(B), direction and gradient on the structural evolution of diffusion layers have been examined systematically. Based on the distance of interfacial migration and the thickness of diffusion layers, we have obtained the effective diffusion coefficient, the diffusion constant and the diffusion activation energy under various high magnetic field conditions as viewed from the kinetics and thermodynamics of atom diffusion, respectively. Theoretical analyses in terms of the magnetic free energy and external force induced by the magnetic field have been made to explain the experimental results. Moreover, the influence regularity and mechanism of high magnetic fields on the diffusion behaviors at heterogeneous interface have been discussed primarily. Following are the main results:
(1) The shift distance of Kirkendall marker and the thickness of diffusion layers in the solid Cu/solid Ni diffusion couples increased with increasing magnetic flux density in case of the direction of diffusion parallel to B. But the effects of high magnetic field on the shift distance intended to get saturation when B was over a critical threshold. An analysis of the diffusion coefficients by means of the Matano plane and Darken equations indicated that the interdiffusion between Cu and Ni was accelerated by the high magnetic fields. On the other hand, in case of the direction of diffusion perpendicular to B, the shift distance of Kirkendall marker almost kept invariant under the application of varying magnetic fields. In addition, the interdiffusion behavior was retarded markedly by a "negative" magnetic field gradient.
(2) The kinetic of interface migration in the liquid Bi/solid Bio.4Sbo.6 diffusion couple appeared to follow a parabolic relationship whether with or without a high magnetic field. It was found that the migration of the interface due to interdiffusion decreased markedly with the increasing strength of magnetic-field, even becoming 1200μm smaller at 11.5T than without a magnetic field. From the above result, we concluded that the interdiffusion behavior between the liquid metal and the solid alloy was strongly retarded by the application of high magnetic fields. This was relevant to the increasing of the viscosity in the liquid metal under a high magnetic field, as in turn caused the diffusion activation energy to increase. Moreover, the retarding effect of magnetic field gradient on diffusion was found to be more significant than that of a uniform magnetic field.
(3) Reactive diffusion experiments at the liquid Al(Zn)/solid Cu interface were experimentally investigated under a high magnetic field. Although there was no noticeable influence of the magnetic field on the microstructure and phase composition of diffusion layers, the thickness of diffusion layers exhibited a decrease with a superposed peak centred on a field of 8.8T(Al/Cu) and 8T (Zn/Cu). The difference of the position of peak value might be induced by the different physical propertied between Al and Zn. In addition, the mean thickness of the diffusion layers (parallel to B) was found to be always greater than that of the diffusion layers (perpendicular to B) under the applied magnetic fields. These phenomena should be attributed to the effects of magnetic fields suppressing natural convection and inducing thermo-electromagnetic convection at the liquid/solid interface. The theoretical derivation of diffusion equation under high magnetic fields indicated that the effective diffusion coefficient went through a non-monotonic variation with magnetic flux densities, as agreed well with the experimental results. Thermodynamic analysis for the growth of diffusion layers shown that a high magnetic field of 11.5T enhanced the activation energy for atom diffusion, which resulted in the decrease of diffusion coefficient comparing with that without a magnetic field. A negative or positive field gradient could retard the diffusion of liquid Al(Zn) in solid Cu, as was similar with the experimental result obtained in the liquid Bi/solid Bi0.4Sb0.6 diffusion couple.
(4) The application of a high magnetic field during pack aluminization process at a temperature of 1173K for 4.5h induced a significant change in the final products at the surface of substrate Cu. Experimental studies demonstrated that the coatings consisted of two layers namelyα+γ2 and a with B ranging from 0 to 8.8T, whereas only theαlayer with Kirkendall voids was observed in case of B≥10T. With the magnetic flux density increasing, the total thickness of coating first increased to a maximum at a field of 6.6T, and then decreased with further increasing magnetic flux density. These results may be attributed to the contradictory effects of high magnetic fields on chemical reaction and on diffusion。
The studies in this paper might be helpful to understand the metallurgical phenomena related to diffusion in high magnetic fields, and provide foundation for the control of diffusion and reaction behaviors at a heterogeneous interface using high magnetic fields.
本文在12T超导强磁场装置中实验研究了固态Cu/固态Ni、液态Bi/固态Bi0.4Sb0.6(互溶扩散)、液态Al (Zn)/固态Cu(反应扩散)、气态A1/固态Cu等扩散偶中的互扩散行为和界面反应,较系统地考察了强磁场的强度、方向、梯度等参数对扩散层组织的演化过程的影响。通过考察界面迁移距离、扩散层厚度等从动力学角度计算强磁场下有效扩散系数,并且从热力学角度获得强磁场条件下的扩散常数和扩散激活能。从磁自由能和磁场力学效果出发对实验现象进行理论分析,初步探讨了强磁场对异质界面扩散行为的影响规律和作用机制。得到以下主要结果：
(1)磁场方向与扩散方向平行时,随着磁场强度的增加,固态Cu/固态Ni界面处扩散层厚度和柯肯达尔标记间的距离都显著增加。但当磁场强度超过某一值后,磁场强度的进一步增大对惰性标记间的距离的影响变小,表明磁场强度的影响趋于饱和。不同磁场强度下,利用俣野平面法结合Darken方程计算的互扩散系数结果表明,强磁场促进了Cu、Ni之间的互扩散。但是,垂直于扩散方向的磁场对固态Cu/固态Ni扩散偶中的柯肯达尔效应几乎没有影响；“负向”梯度强磁场显著抑制了Cu、Ni之间的互扩散。
(2)无论有无强磁场作用,液态Bi/固态Bi0.4Sb0.6中界面迁移距离和扩散时间之间都存在抛物线规律,但是随着磁场强度的增大界面迁移距离显著减小,11.5T磁场下的界面迁移距离比无磁场作用时甚至减小了1200μm,表明强磁场强烈的抑制了液态金属与固态合金之间的扩散迁移行为。磁场下有效扩散系数显著减小应归功于强磁场使液相黏度增加,增大了原子的扩散激活能。梯度磁场条件下的实验结果表明,无论磁场梯度的方向是正或负,其扩散阻碍作用都比均恒磁场的作用效果更显著。
(3)实验研究了强磁场对液态Al(Zn)/固态Cu中发生的界面反应扩散的影响,发现施加强磁场不会改变界面扩散层的形貌和相组成,但是随着磁场强度在0-12T范围内改变,扩散层厚度呈现先减小后增大再减小的非线性变化规律,Al元素和Zn元素的物性差异导致扩散层厚度极大值分别对应于磁场强度8.8T和8T。另外,平行磁场方向的扩散层总是厚于垂直磁场方向的扩散层。分析表明强磁场抑制自然对流和诱发热电磁对流两方面作用产生了上述实验结果。理论推导的强磁场条件下的扩散定律结果表明,有效扩散系数随磁场强度非线性变化,与实验结果吻合的很好。对扩散层生长过程的热力学分析表明,11.5T强磁场增大了原子扩散激活能,导致扩散系数较无磁场作用时显著降低。与液态Bi/固态Bi0.4Sb0.6中的实验结果相似,梯度强磁场显著抑制了液态Al (Zn)/固态Cu系统中的反应扩散行为。
(4)在1173K保温4.5小时的纯铜表面气相渗铝实验中施加强磁场,发现强磁场诱导基体Cu表面最终产物的形貌、结构、相组成发生了显著变化。磁场强度从0T到8.8T范围内,表面渗层由α+γ2和α两层结构组成,但是当磁场强度(≥10T)时,渗层仅由含有大量kirkendall空穴的α层组成。随着磁场强度的增大,渗层厚度显著增加并在磁场强度6.6T时达到最大值,但是随着磁场强度的进一步增大,渗层厚度显著减小。强磁场对化学反应和扩散行为的矛盾作用产生了以上实验结果。
本论文工作对于探索强磁场对金属材料学中各种与扩散有关的金属学现象的影响机理以及强磁场下异质界面的扩散反应行为控制具有积极意义。
Due to its unique properties of non-contact, directionality, marked magnetizability and magnetic force, a high magnetic field as one kind of extreme conditions can exert an obvious influence on the processing of many metallic materials, such as solid-state phase transformation, grain boundary migration, recrystallization, solidification, and chemical reaction. These processes mentioned above have a closely relationship with the diffusion behavior of atoms. Diffusion is an important way for mass transport process, being a key factor for the control of the microstructure and properties of materials, and playing a basic role during the process of metallurgical physical chemistry. Therefore, a detailed discussion of the effects of high magnetic field on the diffusion behavior is the precondition and foundation for the control of microstructures using a high magnetic field.
The interdiffusion behaviors and interfacial reaction in solid Cu/solid Ni, liquid Bi/solid Bi0.4Sb0.6, liquid Al(Zn)/solid Cu, and gas Al/solid Cu diffusion couples have been experimentally studied under high magnetic field of up to 12T. The effects of magnetic flux density(B), direction and gradient on the structural evolution of diffusion layers have been examined systematically. Based on the distance of interfacial migration and the thickness of diffusion layers, we have obtained the effective diffusion coefficient, the diffusion constant and the diffusion activation energy under various high magnetic field conditions as viewed from the kinetics and thermodynamics of atom diffusion, respectively. Theoretical analyses in terms of the magnetic free energy and external force induced by the magnetic field have been made to explain the experimental results. Moreover, the influence regularity and mechanism of high magnetic fields on the diffusion behaviors at heterogeneous interface have been discussed primarily. Following are the main results:
(1) The shift distance of Kirkendall marker and the thickness of diffusion layers in the solid Cu/solid Ni diffusion couples increased with increasing magnetic flux density in case of the direction of diffusion parallel to B. But the effects of high magnetic field on the shift distance intended to get saturation when B was over a critical threshold. An analysis of the diffusion coefficients by means of the Matano plane and Darken equations indicated that the interdiffusion between Cu and Ni was accelerated by the high magnetic fields. On the other hand, in case of the direction of diffusion perpendicular to B, the shift distance of Kirkendall marker almost kept invariant under the application of varying magnetic fields. In addition, the interdiffusion behavior was retarded markedly by a "negative" magnetic field gradient.
(2) The kinetic of interface migration in the liquid Bi/solid Bio.4Sbo.6 diffusion couple appeared to follow a parabolic relationship whether with or without a high magnetic field. It was found that the migration of the interface due to interdiffusion decreased markedly with the increasing strength of magnetic-field, even becoming 1200μm smaller at 11.5T than without a magnetic field. From the above result, we concluded that the interdiffusion behavior between the liquid metal and the solid alloy was strongly retarded by the application of high magnetic fields. This was relevant to the increasing of the viscosity in the liquid metal under a high magnetic field, as in turn caused the diffusion activation energy to increase. Moreover, the retarding effect of magnetic field gradient on diffusion was found to be more significant than that of a uniform magnetic field.
(3) Reactive diffusion experiments at the liquid Al(Zn)/solid Cu interface were experimentally investigated under a high magnetic field. Although there was no noticeable influence of the magnetic field on the microstructure and phase composition of diffusion layers, the thickness of diffusion layers exhibited a decrease with a superposed peak centred on a field of 8.8T(Al/Cu) and 8T (Zn/Cu). The difference of the position of peak value might be induced by the different physical propertied between Al and Zn. In addition, the mean thickness of the diffusion layers (parallel to B) was found to be always greater than that of the diffusion layers (perpendicular to B) under the applied magnetic fields. These phenomena should be attributed to the effects of magnetic fields suppressing natural convection and inducing thermo-electromagnetic convection at the liquid/solid interface. The theoretical derivation of diffusion equation under high magnetic fields indicated that the effective diffusion coefficient went through a non-monotonic variation with magnetic flux densities, as agreed well with the experimental results. Thermodynamic analysis for the growth of diffusion layers shown that a high magnetic field of 11.5T enhanced the activation energy for atom diffusion, which resulted in the decrease of diffusion coefficient comparing with that without a magnetic field. A negative or positive field gradient could retard the diffusion of liquid Al(Zn) in solid Cu, as was similar with the experimental result obtained in the liquid Bi/solid Bi0.4Sb0.6 diffusion couple.
(4) The application of a high magnetic field during pack aluminization process at a temperature of 1173K for 4.5h induced a significant change in the final products at the surface of substrate Cu. Experimental studies demonstrated that the coatings consisted of two layers namelyα+γ2 and a with B ranging from 0 to 8.8T, whereas only theαlayer with Kirkendall voids was observed in case of B≥10T. With the magnetic flux density increasing, the total thickness of coating first increased to a maximum at a field of 6.6T, and then decreased with further increasing magnetic flux density. These results may be attributed to the contradictory effects of high magnetic fields on chemical reaction and on diffusion。
The studies in this paper might be helpful to understand the metallurgical phenomena related to diffusion in high magnetic fields, and provide foundation for the control of diffusion and reaction behaviors at a heterogeneous interface using high magnetic fields.
引文
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