CN109576609B - 软磁性FeCoNiBCP高熵非晶合金及其制备方法 - Google Patents
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Abstract
本发明公开了一种软磁性能的FeCoNiBCP高熵非晶合金,其原子百分比组成为FeaCobNicBdCePf,其中,30<a≤45,10≤b≤25,15≤c≤30,0≤d≤20,0<e≤20,0<f≤20,15≤d+e+f≤30。本发明还公开了该高熵非晶合金的制备方法。与现有的技术相比,本发明的优点是:具有高的饱和磁感应强度Bs(多数合金Bs大于1.0T,可达到1.24T),极低的矫顽力(可达到0.5A/m),良好的热稳定性,因此是一种优异的软磁材料,在磁性功能器件中的应用具有优良的前景。
Description
技术领域
本发明属于高熵非晶合金材料及其制备技术领域,特别涉及具有软磁性的FeCoNiBCP高熵非晶合金及其制备方法。
背景技术
有别于传统的晶态合金,非晶合金是长程无序的合金。因此,非晶合金具有一些晶态合金不具备的优异性能。其中,非晶合金的软磁性能在1967年被首次报道,并立刻引起了科研及工业界的极大重视,成为了几十年来软磁材料研究的热点之一。
对于具有软磁性能的非晶合金而言,因原子呈无序排列,没有晶界阻碍磁畴壁的移动,使得其具有小的矫顽力,因此磁滞损耗小;同时,原子的无序排列,使Fe基非晶合金具有较大的电阻率,导致涡流损耗较小。综上所述,软磁非晶合金具有优异的综合软磁性能。
高熵合金同样是一类特殊的新型合金。其特征为体系的混合熵ΔSmix≥1.5R,在成分上表现为各组元的原子百分比相等或基本相等。这与传统合金仅含1至2种主要组成元素的成分的设计思路差别很大。这种成分特点,使得高熵合金具有一些传统合金无法比拟的优异性能,如高硬度、高强度、高耐磨、高耐蚀、高电阻、高热阻等。
近年来的研究成果表明,部分高熵合金成分在一定条件下,可以制备成具有非晶态结构的合金材料,即高熵非晶合金。例如,2002年,日本东北大学的Ma等人制备出了Ti20Zr20Hf20Cu20M20(M=Fe,Co,Ni)非晶合金条带。2011年,中科院物理所的Wang等人制备出Zn20Ca20Sr20Yb20(Li0.55Mg0.45)20的高熵块体非晶合金。此外日本东北大学的Takeuchi等人通过玻璃包覆提纯法制备出了临界尺寸达到厘米量级的Pd20Pt20Cu20Ni20P20高熵块体非晶合金。随后,清华大学姚可夫研究组研发出多个有大非晶形成能力的高熵块体非晶合金系。近年来,对于高熵非晶合金而言,研究者们更多研究的是其力学性能,而对于其功能特性,如光、电、磁学性能,相关的研究却较少。最近,高熵合金及高熵非晶合金的磁学性能,特别是软磁性能,开始受到关注:大连理工大学的Zhang等人制备了一系列Fe25Co25Ni25(B,C,Si,P)25具有软磁性能的高熵非晶合金[Journal of Alloys and Compounds,2017,693(25-31);Intermetallics,2015,66(8-12);Journal of Non-Crystalline Solids,2018,487(60-64)],具有较低的矫顽力(0.8-6.4A/m),但由于其铁磁性元素Fe,Co,Ni含量相对较低(原子百分比含量75%),故饱和磁感应强度偏低(0.71-0.87T)。因此,开发兼具低矫顽力和较高饱和磁感应强度的高熵非晶合金是很有必要的。
发明内容
本发明提供了具有较高饱和磁感应强度、极低矫顽力、较大非晶形成成分范围的高熵非晶合金及其制备方法。具体技术方案如下。
一种具有优异软磁性能的FeCoNiBCP高熵非晶合金,分子式为FeaCobNicBdCePf,下标a、b、c、d、e、f为各对应元素的原子百分比,满足30<a≤45,10≤b≤25,15≤c≤30,0≤d≤20,0<e<20,0<f<20,15≤d+e+f≤30。
进一步,所述高熵非晶合金,其饱和磁感应强度Bs≥0.8T,优选Bs≥1.0T,更优选1.24T。
进一步,所述非晶合金在低温去应力热处理后(即在低于非晶转变温度Tg或低于晶化温度Tx约50-100度以下热处理后),非晶合金的矫顽力Hc低于15-22A/m,优选Hc≤5.0-6.0A/m,更优选Hc≤0.5A/m。
所述高熵非晶合金的制备方法,包括以下步骤:
(1)将合金原料按化学式配比转换成质量百分比后进行称量配料,使用的原料为纯度大于99.5wt%的Fe、Co、Ni、B、C及纯度大于99.0wt%的Fe3P;
(2)采用感应熔炼炉,在抽真空后,充入保护气体,再将配好的合金元素原料进行多次熔炼,以保证成分均匀,最后得到母合金锭;
(3)将母合金锭进行破碎;
(4)将破碎后的小母合金块熔化,然后采用单辊旋淬法制备出高熵非晶合金条带;
(5)将所述高熵非晶合金条带在热处理炉内进行热处理,其中,所述热处理时间大于15min,所述热处理温度为400℃。
进一步,采用X射线衍射仪检测热处理前及热处理后样品的结构,采用振动样品磁强计(VSM)测量样品的饱和磁感应强度Bs(最大外加磁场为800kA/m),软磁直流测试装置测量样品的B800和Hc(最大外加磁场为800A/m)。
本发明的有益效果:与现有的技术相比,本发明的高熵非晶合金具有高的饱和磁感应强度(可达到1.24T),极低的矫顽力(可达到0.5A/m),良好的热稳定性,因此是一种优异的软磁材料,在磁性功能器件中的应用具有优良的前景。
附图说明
图1是以本发明实施例1-12中各合金成分通过单辊旋淬法获得的条带的X射线衍射图谱。
图2是本发明实施例典型成分非晶合金晶化过程的DSC曲线。
图3是本发明实施例1–12成分的非晶条带的饱和磁感应强度Bs随着成分变化的分布情况图。
图4是本发明实施例1–12中成分的非晶条带的矫顽力Hc随着成分变化的分布情况图。
图5是以本发明实施例13-14中各合金成分通过单辊旋淬法获得的条带对应的X射线衍射图谱。
具体实施方式
下面通过附图和实施例对本发明进行具体说明,但本发明并不局限于此。
表1实施例1-12及对比例的磁学性能
实施例1-12:制备Fe40Co20Ni20(B,C,P)20高熵非晶合金
设计的高熵合金成分分别为:Fe40Co20Ni20C7P13(实施例1)、Fe40Co20Ni20C10P10(实施例2)、Fe40Co20Ni20B3C7P10(实施例3)、Fe40Co20Ni20B5C5P10(实施例4)、Fe40Co20Ni20B5C7P8(实施例5)、Fe40Co20Ni20B7C3P10(实施例6)、Fe40Co20Ni20B7C5P8(实施例7)、Fe40Co20Ni20B7C7P6(实施例8)、Fe40Co20Ni20B9C1P10(实施例9)、Fe40Co20Ni20B9C3P8(实施例10)、Fe40Co20Ni20B9C5P6(实施例11)、Fe40Co20Ni20B9C7P4(实施例12),合金成分见表一所示。实施例1-12首先根据化学成分配比进行配料,再采用感应熔炼炉,在抽真空后,充入保护气体,再将配好的原料进行多次熔炼,以保证成分均匀,最后得到母合金锭。将母合金锭进行破碎。将破碎后的小母合金块熔化,然后采用单辊旋淬法制备出高熵非晶合金条带。将所述高熵非晶合金条带在热处理炉内进行去应力低温热处理,其中,所述热处理时间约为15min以上,所述热处理温度约为400℃。
采用X射线衍射仪检测热处理前及热处理后条带样品的结构。图1为实施例1-12中各合金成分通过单辊旋淬法获得的条带的X射线衍射图谱,图谱为非晶合金典型的漫散射峰,没有与晶态材料相对应的尖锐衍射峰,表明制备的高熵非晶合金具有完全非晶结构。经低温(400℃)热处理15min后,各条带的X射线衍射图谱与图1相似,也是典型的非晶合金X射线衍射图谱。
采用热分析仪(DSC)测试了典型成分Fe40Co20Ni20B9C3P8(实施例10)非晶合金条带的升温晶化过程的DSC曲线,如图2所示。可见其非晶转变温度Tg=436℃,起始晶化温度Tx=472℃。
采用振动样品磁强计(VSM)测量样品的饱和磁感应强度Bs(最大外加磁场为800kA/m),采用软磁直流测试装置测量样品的B800和Hc(最大外加磁场为800A/m)。所测得的磁学性能如表1所示。图3所示为实施例1-12中不同B、C、P含量的各成分非晶合金的Bs分布图。可见各合金的Bs为0.86-1.24T,多数合金的Bs约大于1.0T。
图4为实施例1-12中不同B、C、P含量的各成分高熵非晶合金条带在经过400℃热处理15min后的矫顽力Hc分布图。可见各合金的Hc为0.5-21.2A/m,多数合金的Hc约小于5.6A/m,甚至达0.5A/m。
比较例1:Fe25Co25Ni25B7.5C7.5P10
该成分选自中国专利CN104878324A,由于该专利的合金铁磁性元素Fe,Co,Ni含量较低,原子百分比含量为75%,因此Bs不高,典型的Fe25Co25Ni25B7.5C7.5P10饱和磁化强度(Bs)为0.80T,矫顽力为3.4A/m。较低的Bs将导致制作出来的器件体积增大,限制了设备向小型化、高效化方向发展。
比较例2:Fe25Co25Ni25Al25
该高熵合金成分选自文献[Journal of Magnetism and Magnetic Materials,2014,371(60-68)],为纯晶态的高熵合金,因此矫顽力较大,为224.5A/m,软磁性能较差。
实施例13-14:制备Fe31Co20Ni30B6C3P10及Fe44Co18Ni18B7C3P10高熵非晶合金
设计了高熵合金成分Fe31Co20Ni30B6C3P10(实施例13)和Fe44Co18Ni18B7C3P10(实施例14)。并根据化学成分配比进行配料,再采用感应熔炼炉,在抽真空后,充入保护气体,再将配好的原料进行多次熔炼,以保证成分均匀,最后得到母合金锭。将母合金锭进行破碎。将破碎后的小母合金块熔化,然后采用单辊旋淬法制备出高熵非晶合金条带。将所述高熵非晶合金条带在热处理炉内进行热处理。其中,所述热处理时间约为15min,所述热处理温度约为400℃。
表2实施例13-14的磁学性能
采用X射线衍射仪检测热处理前及热处理后条带样品的结构,图5为实施例13-14中各成分合金通过单辊旋淬法制备的条带退火前的X射线衍射图谱,图谱为非晶合金典型的漫散射峰,没有与晶态材料相对应的尖锐衍射峰,表明制备的高熵非晶合金具有完全非晶结构。经低温(400℃)退火15min后,各条带的X射线衍射图谱与图1相似,也是典型的非晶合金X射线衍射图谱。
采用软磁直流测试装置测量了退火条带样品的B800和Hc(最大外加磁场为800A/m)。所测得的磁学性能如表2所示。可见Fe31Co20Ni30B6C3P10(实施例13)和Fe44Co18Ni18B7C3P10(实施例14)非晶合金条带的B800分别为0.7T和0.97T、Hc分别为2.2A/m和1.2A/m(见表二)。
上述实施例对本发明的技术方案进行了详细说明。显然,本发明并不局限于所描述的实施例。基于本发明中的实施例,熟悉本技术领域的人员还可据此做出多种变化,但任何与本发明等同或相类似的变化都属于本发明保护的范围。
Claims (5)
1.一种具有软磁性能的FeCoNiBCP高熵非晶合金,其特征在于,所述合金的分子式为Fe40Co20Ni20BdCePf,下标d、e、f为各对应元素的原子百分比,满足d为0、5、7,e为3、5、10, f为10,d+e+f为20。
2.权利要求1所述的高熵非晶合金的制备方法,其特征在于,包括以下步骤:
(1)采用纯度大于99.5 wt%的Fe、Co、Ni、B、C及纯度大于99.0 wt%的Fe3P按权利要求1所述的合金元素进行配料;
(2)采用感应熔炼炉,在抽真空后,充入保护气体,再将配好的合金元素原料进行熔炼,得到母合金锭;
(3)将母合金锭进行破碎,得到小母合金块;
(4)将破碎后的小母合金块熔化,然后采用单辊旋淬法制备出高熵非晶合金条带;
(5)将所得高熵非晶合金条带进行热处理,得到所述高熵非晶合金。
3.根据权利要求2所述的制备方法,其特征在于:步骤(2)中所述熔炼为进行多次熔炼,以保证成分均匀。
4.根据权利要求2所述的制备方法,其特征在于:步骤(5)中所述热处理在热处理炉内进行,其中,所述热处理时间大于15 min,所述热处理温度为400℃。
5.根据权利要求2所述的制备方法,其特征在于:还包括步骤(6)采用X射线衍射仪检测热处理前及热处理后样品的结构,采用振动样品磁强计测量样品的饱和磁感应强度B s,采用软磁直流测试装置测量样品的B 800和H c。
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