CN109482880B - 一种同时提升Ni-Mn-In合金力学性能和磁热性能的制备方法 - Google Patents
一种同时提升Ni-Mn-In合金力学性能和磁热性能的制备方法 Download PDFInfo
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Abstract
本发明提供了一种同时提升Ni‑Mn‑In合金力学性能和磁热性能的制备方法,该合金由以下设计工艺制成:按照原料配比称取Ni、Mn、In原料,利用真空电弧多次反复熔炼,制备多晶铸锭,通过机械研磨,制成粉末,然后用标准试验筛筛出15~200um左右的合金粉末,去应力退火温度在300℃~700℃之间。置于石墨模具中,然后在放电等离子烧结系统中进行烧结,真空度小于20Pa,升温速率为20~100℃/min,压力为20~80MPa,烧结温度为550~930℃,保温时间为1~30min,去应力退火温度在300℃~700℃之间。通过本发明设计的制备工艺,同时提升了Ni‑Mn‑In合金的力学性能和磁热性能。本工艺具有普遍性规律,同样适用于所有的Ni‑Mn‑x(In、Sn、Sb)合金。
Description
技术领域
本发明属于磁制冷材料技术领域,尤其涉及一种功能金属材料的设计方案和制备方法。
背景技术
近年来,Ni-Mn-x(x=In、Sn、Sb)合金作为一类新型磁制冷材料,一直被广泛关注。除了磁晶各向异性能,在磁场作用下,塞曼能发挥着至关重要的作用,能够显著影响相的稳定性并诱导逆马氏体相变发生,塞曼能可以随外加磁场增加而增加。但是,Ni-Mn-x(Ga、In、Sn、Sb)合金力学性能较脆的本质,导致机械加工成型性比较差,一直阻碍着工业化生产。
为了改善NiMn基合金的力学性能,相关学者作出了大量尝试,目前,主要有定向凝固工艺,合金化,复合材料,粉末冶金等途径。其中定向凝固(Huang Y J,Hu Q D,Liu J,etal.Banded-like morphology and martensitic transformation of dual-phase Ni–Mn–In magnetic shape memory alloy with enhanced ductility[J].Acta Materialia,2013,61(15):5702-5712.)和合金化,例如B(Yang Z,Cong D Y,Sun X M,et al.Enhancedcyclability of elastocaloric effect in boron-microalloyed Ni-Mn-In magneticshape memory alloys[J].Acta Materialia,2017,127:33-42.)、Ti(Sánchezalarcos V,Pérezlandazábal J I,Recarte V,et al.Effect of Ti addition on the mechanicalproperties and the magnetocaloric effect of Ni-Mn-In metamagnetic shapememory alloys[J].Journal of Physics D Applied Physics,2015,48(44):445006.)等,尽管改善了NiMn基合金的力学性能,但是,定向凝固以及合金化产生的第二相,钉扎位错,阻碍了马氏体相变,增加了滞后,同时提高了相变应力平台。而通过SPS烧结制备了Ni-Mn-Ga/Mg复合材料(Tian B,Tong Y X,Chen F,et al.Microstructure,phasetransformation and mechanical property of Ni-Mn-Ga particles/Mg composites[J].Materials Science&Engineering A,2014,615(615):273-277.),力学性能显著改善,但是,马氏体转变的磁化率非常弱,降低了磁性能。
粉末冶金是一种有效的改善合金强度和塑性的成型工艺,通过SPS烧结制备了Ni-Co-Mn-In合金(Tian B,Ren D C,Tong Y X,et al.Microstructure,PhaseTransformation and Mechanical Property of Ni-Co-Mn-In Alloy Prepared by SparkPlasma Sintering[J].Materials Science Forum,2015,815(4):222-226.),烧结合金的抗压强度和断裂应变分别达到了1900MPa和18%,这是目前通过熔炼和合金化无法达到的,但是DSC没有观测到吸放热峰,合金的马氏体相变彻底被抑制。尽管通过以上途径都改善了NiMn基合金的力学性能,但是,其相关磁性能都不同程度的下降甚至彻底丧失。至今为止,还没有文献报道能够同时提升NiMn基变磁性形状记忆合金的力学性能和磁热性能。
本发明通过适当的烧结工艺并结合相应的热处理工艺,消除机械研磨和烧结过程中粒子塑性变形所产生的内应力,使得烧结合金恢复马氏体转变,结果,同时提升了合金的力学性能和磁热性能,本工艺具有普遍性规律,同样适用于所有的Ni-Mn-x(In、Sn、Sb)合金。
发明内容
本发明提供了一种Ni-Mn-In变磁性形状记忆合金的烧结成型工艺,通过一系列工艺流程,同时提升NiMn基合金的力学性能和磁热性能。更有利于实际应用,而且该合金的的工艺制备简单、高效率、易于实现工业化生产。
为实现前述发明目的,本发明采用的技术方案包括如下步骤:
1、通过电弧熔炼制备出多晶Ni-Mn-In块体,机械研磨,制成粉体。然后用90目和1000目的标准试验筛,获取一定粒径的合金粉末,粒径在15um~160um之间。
2、上述材料由放电等离子烧结工艺合成,其包括以下步骤:
(1)去应力退火:将电弧熔炼的Ni-Mn-In合金粉末放入充有氩气的石英管当中,密封,然后退火温度在300℃~700℃之间,退火时间在0~24h之间,最佳退火参数为600℃,5h去应力退火。
(2)烧结:称取3~9g合金粉末,置于Ф15的石墨磨具中,在放电等离子烧结系统,真空环境中进行烧结,真空度为小于20Pa;以20~100℃/min的升温速率升至550~930℃,保温1-30分钟,压力为20~80MPa,最佳烧结参数为:升温速率为100℃/min,烧结温度为900℃,保温时间15min,加载压力为50MPa。
(3)去应力退火:将选取的合金粉末放入充有氩气的石英管当中,密封,然后退火温度在300℃~700℃之间,退火时间在0~24h之间,最佳退火参数为500℃,5h去应力退火。
本发明的一种三元Ni-Mn-In变磁性形状记忆合金,从实际应用角度出发,提升了Ni-Mn-In变磁性形状记忆合金的力学性能和磁热性能,解决了力学性能差的缺点,同时又保持了良好的磁热性能。更有利于实际应用。此外,该工艺通过放电等离子烧结成型,具有环保,节能,高效等优良特点,本工艺具有普遍性规律,同样适用于所有的Ni-Mn-x(In、Sn、Sb)合金。
附图说明
附图1烧结Ni50Mn34.7In15.3合金的工艺流程图。
附图2烧结Ni50Mn34.7In15.3合金的磁熵变随温度的变化曲线。
附图3烧结Ni50Mn34.7In15.3合金的工程应力应变曲线。
具体实施方式
实施例1
Ni-Mn-In合金中元素的原子比之和为100,原子比为n(Ni):n(Mn):n(In)=50:34.7:15.3。
Ni50Mn34.7In15.3合金靶材的制备方法,包括以下步骤:
步骤1,Ni-Mn-In合金粉末的制备:
(1)原料配比:按照化学式Ni50Mn34.7In15.3配料;
(2)制备多晶铸锭:将步骤(1)称取的原料盛放至真空电弧熔炼炉水冷铜坩埚中,电弧熔炼炉腔体抽真空至3×10-3后,通入惰性保护气体0.05MPa,反复熔炼4~5次,熔炼时间为2~2.5小时。电磁搅拌下进行电弧熔炼,得到成分均匀的合金铸锭;
(3)将熔炼的多晶块体合金放入充有氩气的石英管当中,密封,然后在900℃,48h均匀化退火,水淬;
(4)机械研磨:将退火后的Ni-Mn-In合金铸锭打磨干净后,通过机械研磨机研磨成粉,得到所述Ni50Mn34.7In15.3合金粉末,然后用100目和120目的标准试验筛,获取一定粒径的合金粉末,粒径在125um~150um之间。
步骤2,Ni-Mn-In合金粉末的烧结成型:
(1)去应力退火:将选取的合金粉末放入充有氩气的石英管当中,密封,然后在600℃,5h去应力退火。
(2)称取7g合金粉末,放入石墨磨具中,在放电等离子烧结系统中进行烧结,真空度为10Pa。在7分钟内升温至600℃,600℃以后,以100℃/min的升温速率,烧结温度900℃,保温15分钟,压力为50MPa。
(3)去应力退火:将选取的合金粉末放入充有氩气的石英管当中,密封,然后在500℃,5h去应力退火。
其性能指标:
磁热性能:在5T磁场下的磁熵变为19.3J·kg-1K-1。
力学性能:合金的抗压强度和断裂应变分别为1050MPa和12.5%。
Claims (2)
1.一种Ni-Mn-In合金材料,其特征在于,包括以下步骤:
(1)通过电弧熔炼制备出多晶Ni-Mn-In块体,机械研磨,制成粉体;然后用90目和1000目的标准试验筛,获取粒径在13um~160um之间的合金粉末;
(2)对步骤(1)获取的材料采用放电等离子烧结工艺合成
1)去应力退火:将经步骤(1)电弧熔炼、机械研磨、筛选的Ni-Mn-In合金粉末放入充有氩气的石英管当中,密封,然后退火温度在300℃~700℃之间,退火时间不大于24h;
2)烧结:称取3~9g合金粉末,置于内径Ф15的石墨磨具中,在放电等离子烧结系统,真空环境中进行烧结,真空度为小于20Pa;以20~100℃/min的升温速率升至550~930℃,保温1~30分钟,压力为20~80Mpa;
3)去应力退火:将烧结的合金粉末放入充有氩气的石英管当中,密封,然后退火温度在300℃~700℃之间,退火时间不大于24h。
2.根据权利要求1所述的一种Ni-Mn-In合金材料,其特征在于以下步骤:
(1)通过电弧熔炼制备出多晶Ni-Mn-In块体,机械研磨,制成粉体;然后用90目和1000目的标准试验筛,获取粒径在13um~160um之间的合金粉末;
(2)对步骤(1)获取的材料采用放电等离子烧结工艺合成如下:
1)去应力退火:将经步骤(1)电弧熔炼、机械研磨、筛选的Ni-Mn-In合金粉末放入充有氩气的石英管当中,密封,然后退火温度在600℃,退火时间在5h;
2)烧结:称取3~9g合金粉末,置于Ф15的石墨磨具中,在放电等离子烧结系统,真空环境中进行烧结,真空度为小于20Pa;以100℃/min的升温速率升至900℃,保温15min,压力为50MPa;
3)去应力退火:将烧结的合金粉末放入充有氩气的石英管当中,密封,然后退火温度在500℃,退火时间在5h。
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