铽镝铁磁致伸缩材料的制备及性能研究
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摘要
铽镝铁磁致伸缩材料是水声换能器、精密致动器、智能传感器等器件的核心材料,广泛应用于军事装备、超声探测、精密自动控制、机器人等高技术领域。我国研制铽镝铁磁致伸缩材料起步较晚,目前制备工艺不太先进,制造成本较高,材料性能指标落后于国际水平,造成产品应用规模较小且不能满足高档器件的要求。论文采用“一步法”定向凝固、铸造—粉末烧结、速凝成晶—粘结等工艺,重点研究了工艺制度对微观组织和性能的影响,为制备高性能的材料提供了实验基础。此外还研究了材料的表面改性处理。
研究了具有自主知识产权的“一步法”定向凝固工艺中凝固速率、合金成分、热处理温度等对微观组织和性能的影响,并得到了优化的工艺参数。当凝固速率V=70mm/h时,晶体以胞状晶生长方式生长,<110>择优取向,材料性能较高；V=110-150mm/h,晶体以胞枝晶生长方式生长,<110>取向减弱,<113>增强；V=200mm/h,晶体以发达的枝状晶生长方式生长,择优取向失败,材料性能较差。对于(TbxDy1-x)Fe1.95合金,x=0.3时的磁晶各向异性场最低,偏离此值的材料性能均有所下降。提高Tb/Dy比例可增大磁晶负的各向异性常数,降低自旋再取向温度Tr,材料低温特性较好；当x=0.35,在无压应力、160kA/m磁场时,材料的磁致伸缩温度系数很小(-1.9×10-6/℃),适用于低温且温度变化大(如-50℃～40℃)的特殊工作环境。900℃和950℃热处理,使得合金中的富稀土相由网状分布变为球状分布,减少了与主相之间的相界面,磁致伸缩性能得到明显提高；高温热处理(如>1000℃)造成合金中析出第二相REFey(y=3-5),性能几乎没有改善。利用高纯金属和优化的工艺参数(如V=70-85mm/h,950℃热处理2h),制备了Φ50mm的(Tb0.3Dy0.7)Fe1.95棒材,10MPa、80kA/m下的磁致伸缩系数λ为1380×10-6,达到国际先进水平,并在大功率水声换能器和磁致伸缩驱动阀等器件中得以应用。
研究了铸造—粉末烧结工艺与材料性能的关系。粒度小于0.147mm时,烧结样品的性能和密度较高；磁场对<111>取向的作用最大,取向度达到40.56%；增大等静压力和延长压制时间有利于提高样品的性能和密度；烧结温度1200℃,可获得高性能的材料。在240kA/m外磁场、8.0MPa预应力,样品λ达到1613×10-6,居国内领先水平。
提出速凝成晶技术制备TbDyFe粘结磁致伸缩材料的方法,并研究了工艺参数与性能的关系。研究发现：随着冷却速度的增加,速凝合金片的晶体生长方式由枝状晶向胞枝晶变化,择优取向由<112>向<110>转变,<112>择优取向样品的λ高于<110>的样品。得到了优化的工艺参数：选用弹性模量小的粘结剂(如环氧树脂),环氧树脂含量4%；粉末粒度对样品的性能存在一定影响,优化的粉末粒度为≤(100-150)μm；固化温度150℃、固化时间2h；磁场取向成型有利于性能的提高。实验获得了高性能的粘结材料,在240kA/m磁场下λ达到740×10-6。
首次采用离子渗氮技术对稀土磁致伸缩材料进行了表面改性处理的研究。研究结果表明：在材料表面生成了一层FeN化合物,有效延缓了富稀土相在酸介质中的腐蚀速度,显著改善了材料的耐腐蚀性能、表面硬度(从587HV提高到622HV)以及耐磨性能,提高了材料在恶劣环境中的应用可靠性。表面离子渗氮对材料性能几乎没有影响,是一种较好的稀土磁致伸缩材料表面处理方法。
Tb-Dy-Fe magnetostrictive materials are the core materials used for producing underwater acoustic transducer, precision actuator, intelligent sensor and the like devices, and they are widely used in high-tech fields such as military equipment, ultrasonic detection, precision automation and robot etc.. In china, the research on Tb-Dy-Fe magnetostrictive material is done with a later start. Up to now, the preparation technologies are not advanced enough, the main problems are the higher producing cost, the lower performance than international level, the less application scale and the inferior properties which can not meet the requirements of the high-grade devices. In this paper, the research involving the effects of the processing parameters on microstructures and properties was carried out by using the " one-step " directional solidification process, casting-powder sintering method and strip-casting binding method, thus it can provide the experiment foundations for preparing the materials with high quality. Furthermore, the surface-modified treatment for Tb-Dy-Fe material is also investigated in this paper.
The effects of directional solidification rate, alloy composition and heat treatment systems used in the "one-step" directional solidification process on the microstructures and properties are studied, and the preferred processing parameters are obtained. When the directional solidification rate is 70mm/h, the crystal growth mode is a cellular morphology, and the material has a<110> preferred orientation and thus can obtain better properties. When the directional solidification rate is 110-150mm/h, the crystal growth mode is still a cellular morphology, but the<110> orientation becomes weak while the<113> orientation enhance. When the directional solidification rate is 200mm/h, the crystal growth mode is a developed dendrite morphology, thus the material fails to get a preferred orientation and thereby obtain an inferior performance. For the (TbxDy1-x)Fe1.95 alloys, the anisotropism of the magnetocrystalline is the lowest when x=0.3, and the properties of materials in which x is deviated from the value are worsened to some extent. By increasing the ratio of Tb/Dy, the anisotropy constant can be increased and the spinning reorientation temperature Tr can be decreased, thus the material has better properties at lower temperature. When x is 0.3, the magnetic field is 160kA/m and there is no compression stress, the temperature coefficients for this magnetostrictive material is very small(-1.9×10-6/℃), so this material is suitable for0 using in the specific working circumstance which has lower and sharply changed temperature(e.g.-50℃-40℃). After the heat-treatment at 900℃and 950℃, the RE-riched phase in this alloy is changed from netlike distribution to spherical distribution, thus the phase interface between this phase and the main phase is decreased, and the magnetostrictive performance is markedly enchanced. The heat-treatment at higher temperature (e.g.>1000℃) can lead to a segregation of the second-phase REFey(y=3-5) in the alloy, and the performance is barely enchanced. By using the metal with higher purity and the preferred processing parameters(e.g.V=70-85mm/h, heat-treatment at 950℃for 2hs), a rod-shaped (Tb0.3Dy0.7)Fe1.95 material (φ50mm) with advanced world standard is obtained, wherein, it'sλis up to 1380×10-6 under lOMPa and 80kA/m, and it can be used in high power underwater-acoustic-transducer and magnetostrictive driving-valve etc..
Moreover, the relationship between the casting-powder sintering producing process and the material properties therefrom is also studied. When the particle size is smaller than 0.147mm, the performance and the density of the sintered sample is higher, and the magnetic field has the most effect on the orientation of<111> crystal orientation, furthermore, the degree of the orientation is up to 40.56%. Increasing the isostatic-pressure and extending the pressing time are helpful to improve the performance and the density of the sample. When the sintering is carried out at 1200℃, the material with higher performance can be obtained. With the external magnetic field of 240kA/m and the pre-stressing force of 8.0MPa, the magnetostriction for this sample can up to 1613×10-6 which is the leading national level.
The strip-casting technology for preparing TbDyFe bonded magnetostrictive material is put forward in this paper. And the relationship between the process and the material properties is studied. As the cooling speed increase, the crystal growth mode will transform from the dendrite morphology to the cellar morphology, and the preferred orientation changes from<112> to<110>, wherein, the sample with a preferred orientation<112> has the better performance than that with a preferred orientation<110>. The binder with small elastic modulus (e.g. epoxy resin) is helpful for the performance, and the optimized concentration of it is 4%.The particle size of the powder has some effect on the performance, and the preferred particle size of the powder is≤100-150μm. The optimized curing temperature is 150℃and the curing time is 2hs. The reorientation resulted by the magnetic field has a good effect on the performance. The binding material with higher performance is obtained through this research, and theλis up to 1380×10-6 under the magnetic field of 240kA/m.
The surface modifying on the magnetostrictive material by ion nitriding process is performed for the first time. By ion nitriding process, a FeN compound layer is formed on the surface of the material, and thus it can delay the corrosion speed of RE-riched phase under acid circumstance. And the anti-corrosion property, surface hardness and wearable property of the sample are remarkablely improved, wherein, the said surface hardness can be increased. from 587HV to 622HV. Ion nitriding process on the surface nearly has no effect on the property of the material, so it is a better surface-treating method to modifying Tb-Dy-Fe magnetostrictive material.
研究了具有自主知识产权的“一步法”定向凝固工艺中凝固速率、合金成分、热处理温度等对微观组织和性能的影响,并得到了优化的工艺参数。当凝固速率V=70mm/h时,晶体以胞状晶生长方式生长,<110>择优取向,材料性能较高；V=110-150mm/h,晶体以胞枝晶生长方式生长,<110>取向减弱,<113>增强；V=200mm/h,晶体以发达的枝状晶生长方式生长,择优取向失败,材料性能较差。对于(TbxDy1-x)Fe1.95合金,x=0.3时的磁晶各向异性场最低,偏离此值的材料性能均有所下降。提高Tb/Dy比例可增大磁晶负的各向异性常数,降低自旋再取向温度Tr,材料低温特性较好；当x=0.35,在无压应力、160kA/m磁场时,材料的磁致伸缩温度系数很小(-1.9×10-6/℃),适用于低温且温度变化大(如-50℃～40℃)的特殊工作环境。900℃和950℃热处理,使得合金中的富稀土相由网状分布变为球状分布,减少了与主相之间的相界面,磁致伸缩性能得到明显提高；高温热处理(如>1000℃)造成合金中析出第二相REFey(y=3-5),性能几乎没有改善。利用高纯金属和优化的工艺参数(如V=70-85mm/h,950℃热处理2h),制备了Φ50mm的(Tb0.3Dy0.7)Fe1.95棒材,10MPa、80kA/m下的磁致伸缩系数λ为1380×10-6,达到国际先进水平,并在大功率水声换能器和磁致伸缩驱动阀等器件中得以应用。
研究了铸造—粉末烧结工艺与材料性能的关系。粒度小于0.147mm时,烧结样品的性能和密度较高；磁场对<111>取向的作用最大,取向度达到40.56%；增大等静压力和延长压制时间有利于提高样品的性能和密度；烧结温度1200℃,可获得高性能的材料。在240kA/m外磁场、8.0MPa预应力,样品λ达到1613×10-6,居国内领先水平。
提出速凝成晶技术制备TbDyFe粘结磁致伸缩材料的方法,并研究了工艺参数与性能的关系。研究发现：随着冷却速度的增加,速凝合金片的晶体生长方式由枝状晶向胞枝晶变化,择优取向由<112>向<110>转变,<112>择优取向样品的λ高于<110>的样品。得到了优化的工艺参数：选用弹性模量小的粘结剂(如环氧树脂),环氧树脂含量4%；粉末粒度对样品的性能存在一定影响,优化的粉末粒度为≤(100-150)μm；固化温度150℃、固化时间2h；磁场取向成型有利于性能的提高。实验获得了高性能的粘结材料,在240kA/m磁场下λ达到740×10-6。
首次采用离子渗氮技术对稀土磁致伸缩材料进行了表面改性处理的研究。研究结果表明：在材料表面生成了一层FeN化合物,有效延缓了富稀土相在酸介质中的腐蚀速度,显著改善了材料的耐腐蚀性能、表面硬度(从587HV提高到622HV)以及耐磨性能,提高了材料在恶劣环境中的应用可靠性。表面离子渗氮对材料性能几乎没有影响,是一种较好的稀土磁致伸缩材料表面处理方法。
Tb-Dy-Fe magnetostrictive materials are the core materials used for producing underwater acoustic transducer, precision actuator, intelligent sensor and the like devices, and they are widely used in high-tech fields such as military equipment, ultrasonic detection, precision automation and robot etc.. In china, the research on Tb-Dy-Fe magnetostrictive material is done with a later start. Up to now, the preparation technologies are not advanced enough, the main problems are the higher producing cost, the lower performance than international level, the less application scale and the inferior properties which can not meet the requirements of the high-grade devices. In this paper, the research involving the effects of the processing parameters on microstructures and properties was carried out by using the " one-step " directional solidification process, casting-powder sintering method and strip-casting binding method, thus it can provide the experiment foundations for preparing the materials with high quality. Furthermore, the surface-modified treatment for Tb-Dy-Fe material is also investigated in this paper.
The effects of directional solidification rate, alloy composition and heat treatment systems used in the "one-step" directional solidification process on the microstructures and properties are studied, and the preferred processing parameters are obtained. When the directional solidification rate is 70mm/h, the crystal growth mode is a cellular morphology, and the material has a<110> preferred orientation and thus can obtain better properties. When the directional solidification rate is 110-150mm/h, the crystal growth mode is still a cellular morphology, but the<110> orientation becomes weak while the<113> orientation enhance. When the directional solidification rate is 200mm/h, the crystal growth mode is a developed dendrite morphology, thus the material fails to get a preferred orientation and thereby obtain an inferior performance. For the (TbxDy1-x)Fe1.95 alloys, the anisotropism of the magnetocrystalline is the lowest when x=0.3, and the properties of materials in which x is deviated from the value are worsened to some extent. By increasing the ratio of Tb/Dy, the anisotropy constant can be increased and the spinning reorientation temperature Tr can be decreased, thus the material has better properties at lower temperature. When x is 0.3, the magnetic field is 160kA/m and there is no compression stress, the temperature coefficients for this magnetostrictive material is very small(-1.9×10-6/℃), so this material is suitable for0 using in the specific working circumstance which has lower and sharply changed temperature(e.g.-50℃-40℃). After the heat-treatment at 900℃and 950℃, the RE-riched phase in this alloy is changed from netlike distribution to spherical distribution, thus the phase interface between this phase and the main phase is decreased, and the magnetostrictive performance is markedly enchanced. The heat-treatment at higher temperature (e.g.>1000℃) can lead to a segregation of the second-phase REFey(y=3-5) in the alloy, and the performance is barely enchanced. By using the metal with higher purity and the preferred processing parameters(e.g.V=70-85mm/h, heat-treatment at 950℃for 2hs), a rod-shaped (Tb0.3Dy0.7)Fe1.95 material (φ50mm) with advanced world standard is obtained, wherein, it'sλis up to 1380×10-6 under lOMPa and 80kA/m, and it can be used in high power underwater-acoustic-transducer and magnetostrictive driving-valve etc..
Moreover, the relationship between the casting-powder sintering producing process and the material properties therefrom is also studied. When the particle size is smaller than 0.147mm, the performance and the density of the sintered sample is higher, and the magnetic field has the most effect on the orientation of<111> crystal orientation, furthermore, the degree of the orientation is up to 40.56%. Increasing the isostatic-pressure and extending the pressing time are helpful to improve the performance and the density of the sample. When the sintering is carried out at 1200℃, the material with higher performance can be obtained. With the external magnetic field of 240kA/m and the pre-stressing force of 8.0MPa, the magnetostriction for this sample can up to 1613×10-6 which is the leading national level.
The strip-casting technology for preparing TbDyFe bonded magnetostrictive material is put forward in this paper. And the relationship between the process and the material properties is studied. As the cooling speed increase, the crystal growth mode will transform from the dendrite morphology to the cellar morphology, and the preferred orientation changes from<112> to<110>, wherein, the sample with a preferred orientation<112> has the better performance than that with a preferred orientation<110>. The binder with small elastic modulus (e.g. epoxy resin) is helpful for the performance, and the optimized concentration of it is 4%.The particle size of the powder has some effect on the performance, and the preferred particle size of the powder is≤100-150μm. The optimized curing temperature is 150℃and the curing time is 2hs. The reorientation resulted by the magnetic field has a good effect on the performance. The binding material with higher performance is obtained through this research, and theλis up to 1380×10-6 under the magnetic field of 240kA/m.
The surface modifying on the magnetostrictive material by ion nitriding process is performed for the first time. By ion nitriding process, a FeN compound layer is formed on the surface of the material, and thus it can delay the corrosion speed of RE-riched phase under acid circumstance. And the anti-corrosion property, surface hardness and wearable property of the sample are remarkablely improved, wherein, the said surface hardness can be increased. from 587HV to 622HV. Ion nitriding process on the surface nearly has no effect on the property of the material, so it is a better surface-treating method to modifying Tb-Dy-Fe magnetostrictive material.
引文
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