低磁场下合金元素Zn对Gd_5Si_2Ge_2相变行为和磁热效应影响的研究
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摘要
Gd5Si2Ge2合金具有无毒性、相变温度接近室温和其巨磁热效应,是近年来倍受关注的磁制冷工质材料。但是,它的巨磁热效应必须在高成本的超导高磁场(5 T -12 T)下获得,低磁场(1.0 T-1.7 T)下无法激发合金产生巨磁热效应,导致其应用成本增高。同时Gd5Si2Ge2合金的相变温度与室温相比较低,制冷过程中磁滞后现象严重,这些问题阻碍了该合金未来的商业化应用。因此,在较低磁场下,如何提高Gd5Si2Ge2合金的相变温度和磁热效应,并降低其磁滞后成为目前研究的热点。
本文系统研究了添加Zn元素同时或单独替代Si和Ge以及热处理对其合金在△H=1.5 T磁场下的相变温度、相变性质、相变过程中的磁滞后、磁热效应和磁制冷能力的影响,阐述了添加适量Zn元素可以提高Gd5Si2Ge2合金磁相变温度和磁热性能的机理和规律,为Gd5Si2Ge2合金在低磁场下获得巨磁热效应提供了有效的方法和依据。研究结果表明:
1.添加微量Zn元素可以促进合金中Gd5Si2Ge2型单斜相形成,抑制Gd5Si4型正交相产生;降低相变时需要的能量,提高一级相变的驱动力,降低发生一级相变时的临界诱发磁场,使合金在△H=1.5 T磁场下产生巨磁热效应。在Gd5Si2-xGe2Znx和Gd5Si2-zGe2-zZn2z合金系中,当x或者2z由0变化到0.001时,其最大等温磁熵变分别由5.03 J/ kg·K提高到20.70 J/kg·K和25.30 J/kg·K;相变温度分别由276 K提高到284 K和280 K;磁制冷能力分别由55.30 J/kg提高到96.14 J/kg和101.00 J/kg磁热性能高于目前文献中报道的Gd5Si2Ge2及GdSiGeGa铸锭合金在高磁场(5 T)变化下的性能(|ΔSM|=20.5 J/kg·K ,Tc=276 K)[4] ,合金的综合磁热性能优秀。
2.添加微量Zn元素后,使得通过传导电子才能相互作用的Gd原子之间4 f-4 f电子之间作用力增强,自旋波能量增加,合金中Gd原子的磁矩提高;减小了室温Gd5Si2Ge2单斜相晶胞体积,增强了磁性Gd原子之间的相互作用能,宽化了制冷区,提高了合金一级磁相变温度和制冷能力。在Gd5Si2Ge2-yZny合金系中,当y由0变化到0.011时,合金的相变温度由276 K提高到288 K;磁制冷能力由55.30 J/kg提高到169 J/kg,合金的综合磁热性能优良。
3.用微量Zn元素对Gd5Si2Ge2化合物进行合金化处理后,降低了合金的磁各向异性能,使合金在一级相变过程中磁畴壁或磁矩运动的阻力减小,一级相变的临界诱发磁场降低,减小了合金在相变过程中磁滞后现象,有利于提高合金的综合磁热性能。
无论Zn元素单独或同时替代Si和Ge,都会使得合金在1.5 T磁场下的相变温度、最大等温磁熵变、磁滞后和制冷能力得到改善,只是不同的替代方式对各项性能提高的幅度有所不同。
4.通过研究热处理温度对GdSiGeZn合金磁热效应的影响,发现添加微量Zn元素后可以有效降低合金的最佳热处理温度,阻止Gd5Si2Ge2单斜相在773 K温度下的共析反应,增加β相在此温度下的稳定性,降低Gd5Si4正交相含量,改善β相的磁内禀性能和对温度变化和磁场变化的敏感性,增加一级相变的驱动力。在Gd5Si2Ge2-yZny合金中,当y=0.011时,773 K温度下的热处理有助于提高合金的相变温度、等温磁熵变和磁制冷能力,降低一级相变过程中的磁滞后。当热处理温度高于1413K时,由于快速冷却导致合金组织缺陷增加和相变驱动力减小,合金的相变温度、等温磁熵变和磁制冷能力趋于减小,磁滞后现象严重。
本研究工作开发了拥有自主知识产权的GdSiGeZn合金,使Gd5Si2Ge2合金在1.5 T低磁场下,磁热效应提高了4-5倍,相变温度提高了4~6 K,改变了磁制冷技术需要依赖高磁场的应用理念,在价格低廉NdFeB磁体能够达到的磁场强度下,使Gd5Si2Ge2合金的应用成为可能。
Non-toxic Gd5Si2Ge2 alloys with magnetic phase temperature close to room temperature and giant magnetocaloric effect(GMCE) are the promising candidates for refrigerant materials in recent years. However, their GMCE can only be obtained in high-cost superconducting magnetic fields(5-10 T), which brings out high costs in practical application. On the other hand, the low magnetic phase transformation temperature and magnetic hysteresis also impede the large-scale application of these alloys. Therefore, the improvement of magnetic phase transformation temperature and magnetocaloric effect and the reduction of magnetic hysteresis become currently hot topics of Gd5Si2Ge2 alloy to be investigated
In this thesis, a systematic study was conducted on the magnetic phase transformation temperature, phase transformation property, magnetic hysteresis in phase transformation process, magnetocaloric effect and magnetic refrigeration capacity under a low magnetic field ranging from 0-1.5 T for the cast and heat-treated alloys with Zn substitution for Si and Ge simultaneously or individually. The mechanisms and roles of the enhancement of phase transformation temperature and magnetocaloric effect after adding Zn into Gd5Si2Ge2 alloys were also studied. The achievements of those studies provide an effective method and basic knowledge for obtaining the GMCE under low magnetic field. The main conclusions are as follows:
1) The addition of trace amount of Zn element has a great impact on the phase formation in the solidification process of the alloy, benefiting the formation of Gd5Si2Ge2-type monoclinic structure and inhibiting the formation of Gd5Si4-type orthorhombic structure;The driving force for the first phase transformation is enhanced and the intensity of external magnetic field needed is reduced, and therefore, the GMCE is generated at a low magnetic field ranging from 0 to 1.5 T. For Gd5Si2-xGe2Znx and Gd5Si2-zGe2-zZn2z alloys, when x or 2z changed from 0 to 0.001, the maximum isothermal magnetic entropy change, magnetic phase transformation temperature, and magnetic refrigerant capacity are increased from 5.03 J/kg?K, 276 K, and 55.30 J/kg to 20.70 J/kg?K and 25.30 J/kg?K, 280 K and 284 K, and 96.14 J/kg and 101.00 J/kg, respectively, for a low magnetic field ranging from 0 to 1.5 T. These magnetocaloric properties are better than that of Gd5Si2Ge2 and GdSiGeGa cast alloys reported in literatures and the comprehensive properties are the best among the other Gd5Si2Ge2 alloys.
2) The addition of trace Zn element enhances the interaction force between the 4f-4f electrons of Gd atoms, in which the interaction only happened through conduction electrons, and increases the spin-wave energy of Gd atoms, it in turn increases the magnetic moment of Gd atoms; the cell volume of monoclinic Gd5Si2Ge2 phase is reduced without destroying the crystal structure and the interaction energy between the Gd atoms is increased due to the similarity of the covalent radius of Zn, Si and Ge atoms, and therefore the magnetic phase transformation temperature is increased and the peak of ??SM? is widen. For Gd5Si2Ge2-yZny alloys, when y changed from 0 to 0.011, the magnetic phase transformation temperature and magnetic refrigerant capacity are increased from 276 K and 55.30 J/kg to 288 K and 196 J/kg, respectively, for a low magnetic field ranging from 0 to 1.5 T. These alloys show good comprehensive magnetocaloric properties.
3) The magnetic anisotropy energy is reduced by adding appropriate amount of Zn element to Gd5Si2Ge2 alloy so that the movement resistance of the magnetic domain wall or the magnetic moment is reduced in the first phase transformation process. It makes the magnetic hystersis to reduce and the magnetic refrigerant capacity to enhance by decreasing the critical induced magnetic field.
Whether Zn substitutes Si and Ge individually or simultaneously, the magnetic phase transformation temperature, the maximum isothermal magnetic entropy change, and the magnetic hystersis and cooling capacity of the alloys are improved for a low magnetic field ranging from 0 to 1.5 T, while the Zn substitution mode has an influence on the increment of respective characters.
4) Heat treatment temperature significantly influences the magnetocaloric effect of GdSiGeZn alloys. When adding trace Zn to GdSiGe alloy, the heat treatment temperature may be effectively reduced and eutectoid reaction of Gd5Si2Ge2-type monoclinic structure (β-phase) at 773 K is prevented and therefore the stability ofβ-phase is increased; the Gd5Si4-type orthorhombic phase is inhibited and its volume fraction is decreased; the intrinsic performance ofβ-phase and its sensibility to the variation of temperature and magnetic field are improved, which lead to the enhancement of driving force for the first phase transformation. For Gd5Si2Ge2-yZny alloys with y of 0.011, heat treatment at 773 K is beneficial to increasing the magnetic phase transformation temperature, isothermal magnetic entropy change and magnetic refrigerant capacity, and lowering the magnetic hystersis in first phase transformation. When the heat treatment temperature is higher than 1413 K, the magnetic phase transformation temperature, isothermal magnetic entropy change and magnetic refrigerant capacity of the alloys decrease and the magnetic hystersis becomes worse due to the increase of structure defects and decrease of the driving force in the first phase transformation after fast cooling of the alloys.
The alloys of GdSiGeZn with our own intellectual property rights are developed, of which the magnetic effect is enhanced about 4~5 times and the magnetic phase transformation temperature is increased about 4 K~6 K for a low magnetic field ranging from 0 to 1.5 T. The research results change, in some extent, the application philosophy that magnetic refrigeration technology should be relied on high applied magnetic field. It makes possible that magnetic refrigeration technology could be applied in lower magnetic field obtained by the cheap NdFeB magnets.
本文系统研究了添加Zn元素同时或单独替代Si和Ge以及热处理对其合金在△H=1.5 T磁场下的相变温度、相变性质、相变过程中的磁滞后、磁热效应和磁制冷能力的影响,阐述了添加适量Zn元素可以提高Gd5Si2Ge2合金磁相变温度和磁热性能的机理和规律,为Gd5Si2Ge2合金在低磁场下获得巨磁热效应提供了有效的方法和依据。研究结果表明:
1.添加微量Zn元素可以促进合金中Gd5Si2Ge2型单斜相形成,抑制Gd5Si4型正交相产生;降低相变时需要的能量,提高一级相变的驱动力,降低发生一级相变时的临界诱发磁场,使合金在△H=1.5 T磁场下产生巨磁热效应。在Gd5Si2-xGe2Znx和Gd5Si2-zGe2-zZn2z合金系中,当x或者2z由0变化到0.001时,其最大等温磁熵变分别由5.03 J/ kg·K提高到20.70 J/kg·K和25.30 J/kg·K;相变温度分别由276 K提高到284 K和280 K;磁制冷能力分别由55.30 J/kg提高到96.14 J/kg和101.00 J/kg磁热性能高于目前文献中报道的Gd5Si2Ge2及GdSiGeGa铸锭合金在高磁场(5 T)变化下的性能(|ΔSM|=20.5 J/kg·K ,Tc=276 K)[4] ,合金的综合磁热性能优秀。
2.添加微量Zn元素后,使得通过传导电子才能相互作用的Gd原子之间4 f-4 f电子之间作用力增强,自旋波能量增加,合金中Gd原子的磁矩提高;减小了室温Gd5Si2Ge2单斜相晶胞体积,增强了磁性Gd原子之间的相互作用能,宽化了制冷区,提高了合金一级磁相变温度和制冷能力。在Gd5Si2Ge2-yZny合金系中,当y由0变化到0.011时,合金的相变温度由276 K提高到288 K;磁制冷能力由55.30 J/kg提高到169 J/kg,合金的综合磁热性能优良。
3.用微量Zn元素对Gd5Si2Ge2化合物进行合金化处理后,降低了合金的磁各向异性能,使合金在一级相变过程中磁畴壁或磁矩运动的阻力减小,一级相变的临界诱发磁场降低,减小了合金在相变过程中磁滞后现象,有利于提高合金的综合磁热性能。
无论Zn元素单独或同时替代Si和Ge,都会使得合金在1.5 T磁场下的相变温度、最大等温磁熵变、磁滞后和制冷能力得到改善,只是不同的替代方式对各项性能提高的幅度有所不同。
4.通过研究热处理温度对GdSiGeZn合金磁热效应的影响,发现添加微量Zn元素后可以有效降低合金的最佳热处理温度,阻止Gd5Si2Ge2单斜相在773 K温度下的共析反应,增加β相在此温度下的稳定性,降低Gd5Si4正交相含量,改善β相的磁内禀性能和对温度变化和磁场变化的敏感性,增加一级相变的驱动力。在Gd5Si2Ge2-yZny合金中,当y=0.011时,773 K温度下的热处理有助于提高合金的相变温度、等温磁熵变和磁制冷能力,降低一级相变过程中的磁滞后。当热处理温度高于1413K时,由于快速冷却导致合金组织缺陷增加和相变驱动力减小,合金的相变温度、等温磁熵变和磁制冷能力趋于减小,磁滞后现象严重。
本研究工作开发了拥有自主知识产权的GdSiGeZn合金,使Gd5Si2Ge2合金在1.5 T低磁场下,磁热效应提高了4-5倍,相变温度提高了4~6 K,改变了磁制冷技术需要依赖高磁场的应用理念,在价格低廉NdFeB磁体能够达到的磁场强度下,使Gd5Si2Ge2合金的应用成为可能。
Non-toxic Gd5Si2Ge2 alloys with magnetic phase temperature close to room temperature and giant magnetocaloric effect(GMCE) are the promising candidates for refrigerant materials in recent years. However, their GMCE can only be obtained in high-cost superconducting magnetic fields(5-10 T), which brings out high costs in practical application. On the other hand, the low magnetic phase transformation temperature and magnetic hysteresis also impede the large-scale application of these alloys. Therefore, the improvement of magnetic phase transformation temperature and magnetocaloric effect and the reduction of magnetic hysteresis become currently hot topics of Gd5Si2Ge2 alloy to be investigated
In this thesis, a systematic study was conducted on the magnetic phase transformation temperature, phase transformation property, magnetic hysteresis in phase transformation process, magnetocaloric effect and magnetic refrigeration capacity under a low magnetic field ranging from 0-1.5 T for the cast and heat-treated alloys with Zn substitution for Si and Ge simultaneously or individually. The mechanisms and roles of the enhancement of phase transformation temperature and magnetocaloric effect after adding Zn into Gd5Si2Ge2 alloys were also studied. The achievements of those studies provide an effective method and basic knowledge for obtaining the GMCE under low magnetic field. The main conclusions are as follows:
1) The addition of trace amount of Zn element has a great impact on the phase formation in the solidification process of the alloy, benefiting the formation of Gd5Si2Ge2-type monoclinic structure and inhibiting the formation of Gd5Si4-type orthorhombic structure;The driving force for the first phase transformation is enhanced and the intensity of external magnetic field needed is reduced, and therefore, the GMCE is generated at a low magnetic field ranging from 0 to 1.5 T. For Gd5Si2-xGe2Znx and Gd5Si2-zGe2-zZn2z alloys, when x or 2z changed from 0 to 0.001, the maximum isothermal magnetic entropy change, magnetic phase transformation temperature, and magnetic refrigerant capacity are increased from 5.03 J/kg?K, 276 K, and 55.30 J/kg to 20.70 J/kg?K and 25.30 J/kg?K, 280 K and 284 K, and 96.14 J/kg and 101.00 J/kg, respectively, for a low magnetic field ranging from 0 to 1.5 T. These magnetocaloric properties are better than that of Gd5Si2Ge2 and GdSiGeGa cast alloys reported in literatures and the comprehensive properties are the best among the other Gd5Si2Ge2 alloys.
2) The addition of trace Zn element enhances the interaction force between the 4f-4f electrons of Gd atoms, in which the interaction only happened through conduction electrons, and increases the spin-wave energy of Gd atoms, it in turn increases the magnetic moment of Gd atoms; the cell volume of monoclinic Gd5Si2Ge2 phase is reduced without destroying the crystal structure and the interaction energy between the Gd atoms is increased due to the similarity of the covalent radius of Zn, Si and Ge atoms, and therefore the magnetic phase transformation temperature is increased and the peak of ??SM? is widen. For Gd5Si2Ge2-yZny alloys, when y changed from 0 to 0.011, the magnetic phase transformation temperature and magnetic refrigerant capacity are increased from 276 K and 55.30 J/kg to 288 K and 196 J/kg, respectively, for a low magnetic field ranging from 0 to 1.5 T. These alloys show good comprehensive magnetocaloric properties.
3) The magnetic anisotropy energy is reduced by adding appropriate amount of Zn element to Gd5Si2Ge2 alloy so that the movement resistance of the magnetic domain wall or the magnetic moment is reduced in the first phase transformation process. It makes the magnetic hystersis to reduce and the magnetic refrigerant capacity to enhance by decreasing the critical induced magnetic field.
Whether Zn substitutes Si and Ge individually or simultaneously, the magnetic phase transformation temperature, the maximum isothermal magnetic entropy change, and the magnetic hystersis and cooling capacity of the alloys are improved for a low magnetic field ranging from 0 to 1.5 T, while the Zn substitution mode has an influence on the increment of respective characters.
4) Heat treatment temperature significantly influences the magnetocaloric effect of GdSiGeZn alloys. When adding trace Zn to GdSiGe alloy, the heat treatment temperature may be effectively reduced and eutectoid reaction of Gd5Si2Ge2-type monoclinic structure (β-phase) at 773 K is prevented and therefore the stability ofβ-phase is increased; the Gd5Si4-type orthorhombic phase is inhibited and its volume fraction is decreased; the intrinsic performance ofβ-phase and its sensibility to the variation of temperature and magnetic field are improved, which lead to the enhancement of driving force for the first phase transformation. For Gd5Si2Ge2-yZny alloys with y of 0.011, heat treatment at 773 K is beneficial to increasing the magnetic phase transformation temperature, isothermal magnetic entropy change and magnetic refrigerant capacity, and lowering the magnetic hystersis in first phase transformation. When the heat treatment temperature is higher than 1413 K, the magnetic phase transformation temperature, isothermal magnetic entropy change and magnetic refrigerant capacity of the alloys decrease and the magnetic hystersis becomes worse due to the increase of structure defects and decrease of the driving force in the first phase transformation after fast cooling of the alloys.
The alloys of GdSiGeZn with our own intellectual property rights are developed, of which the magnetic effect is enhanced about 4~5 times and the magnetic phase transformation temperature is increased about 4 K~6 K for a low magnetic field ranging from 0 to 1.5 T. The research results change, in some extent, the application philosophy that magnetic refrigeration technology should be relied on high applied magnetic field. It makes possible that magnetic refrigeration technology could be applied in lower magnetic field obtained by the cheap NdFeB magnets.
引文
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