CN106971803A - 一种全致密各向异性NdFeB/MnBi混合永磁的制备方法 - Google Patents
一种全致密各向异性NdFeB/MnBi混合永磁的制备方法 Download PDFInfo
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Abstract
本发明公开一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，首先制备MnBi合金粉末，按质量比计算，将20‑30％的MnBi合金粉末和70‑80％的NdFeB粉末混合后得到NdFeB/MnBi混合粉末，将该NdFeB/MnBi混合粉末放入磁场中取向成型，然后将成型后的NdFeB/MnBi混合粉末烧结即得NdFeB/MnBi混合永磁，采用本发明所制备的各向异性NdFeB/MnBi混合永磁，密度可达到7.75‑7.95g/cm3，样品中两种硬磁相都具有较好取向，且退磁曲线表现出单相退磁特征，适量MnBi的加入可保证磁体磁性能的同时，改善NdFeB磁体在高温下的矫顽力。
Description
技术领域
本发明涉及大块永磁技术领域，具体涉及一种全致密各向异性NdFeB/MnBi混合永磁的制备方法。
背景技术
钕铁硼永磁合金是当今磁能积最高的永磁，且生产工艺成熟、成本较低，被广泛应用，然而钕铁硼永磁的居里温度较低，磁性能随温度增加会大幅下降，不适宜应用在高温工作环境领域。
近年来一种不含稀土的永磁锰铋合金引起人们的注意，锰铋合金虽然磁能积远小于钕铁硼永磁，但也具有独特的优势：不含稀土元素，矫顽力较高，且矫顽力随温度升高而升高。由以前的公开报道可知，已有人将MnBi和NdFeB制作为混合磁体，如将MnBi和NdFeB磁粉混合制作成各向同性粘结磁体，或利用烧结法将混合粉末烧结为各向异性块体。前者，磁体密度较低且为各向同性，磁体磁性能较低；而后者，尽管磁体为各向异性，但由于采用的烧结法，磁体无法实现全致密，密度较低，造成磁体磁性能较低。因此，为利用MnBi磁粉的优势，改善NdFeB磁体的综合磁性能，如何制得全致密各向异性NdFeB/MnBi混合永磁具有重要的意义。
发明内容
为解决以上技术问题，本发明提供一种全致密各向异性NdFeB/MnBi混合永磁的制备方法。
技术方案如下：一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其关键在于：制备MnBi合金粉末，按质量比计算，将20-30％的MnBi合金粉末和70-80％的NdFeB粉末混合后得到NdFeB/MnBi混合粉末，将该NdFeB/MnBi混合粉末放入磁场中取向成型，然后将成型后的NdFeB/MnBi混合粉末烧结即得NdFeB/MnBi混合永磁。
制备MnBi合金粉末的步骤如下：配置MnBi合金原料，然后采用真空电弧熔炼将MnBi合金原料制成合金铸锭，接着将合金铸锭破碎并真空甩带制成MnBi合金薄带，最后将MnBi合金薄带进行真空热处理并破碎即得所述MnBi合金粉末。
制备所述NdFeB/MnBi混合粉末的方法为首先将MnBi合金粉末放入球磨罐中进行首次滚动球磨，然后再加入NdFeB粉末进行二次滚动球磨即得所述NdFeB/MnBi混合粉末。
上述首次滚动球磨是在正庚烷的保护下进行，按质量比计算，球料比为10:1球磨120min；所述二次滚动球磨的时间为60min。
上述磁场为脉冲磁场，磁场强度为2.5T，所述取向成型过程中在氩气氛围下进行。
上述真空热处理的条件为真空度10-2Pa，温度300℃，保温处理8h。
上述烧结条件为在3min内将温度升温至300℃，然后保温5min，接着在1min内将温度升温至600℃，最后在60min内快速降温至50℃即可，整个烧结过程中施加1GPa压力。
上述MnBi合金原料中按摩尔比计算Mn:Bi的摩尔比为1:1；所述NdFeB粉末为经HDDR处理后的各向异性NdFeB磁性粉末；所述MnBi合金粉末为80目。
有益效果：采用本发明所制备的各向异性NdFeB/MnBi混合永磁，密度可达到7.75-7.95g/cm3，混合永磁中两种硬磁相都具有较好取向(各向异性)，且退磁曲线表现出单相退磁特征，适量MnBi的加入可保证磁体磁性能的同时，改善NdFeB磁体在高温下的矫顽力。
附图说明
图1为实施例1的退磁曲线；
图2为实施例1的垂直于磁化方向平面的XRD图；
图3为实施例2的退磁曲线；
图4为实施例2的垂直于磁化方向平面的XRD图。
具体实施方式
下面结合实施例和附图对本发明作进一步说明。
实施例1，步骤一、首先制备MnBi合金粉末
配制摩尔比为1:1的MnBi的合金原料，利用真空电弧熔炼反复熔炼三次，从而得到成分均匀的合金铸锭，接着将合金铸锭破碎并以30m/s的甩带速度进行真空甩带，得到MnBi合金薄带，将MnBi合金薄带在真空热处理炉中进行真空热处理，真空热处理条件为：真空度为10-2Pa、加热温度为300℃，保温时间8h，然后将经真空热处理后的MnBi薄带放入手套箱中并破碎至80目，获得所述MnBi合金粉末；
步骤二、制备NdFeB/MnBi混合粉末
按质量比计算，将20％的MnBi合金粉末和80％的经HDDR处理后的市售各向异性NdFeB粉末混合均匀得到NdFeB/MnBi混合粉末。为获得混合均匀的NdFeB/MnBi混合粉末，采用两步球磨法，即：将所述MnBi合金粉末放入球磨罐中，并在正庚烷保护下进行首次滚动球磨，首次滚动球磨的球料比为10:1；球磨120min后放入NdFeB粉末进行二次滚动球磨，二次滚动球磨时间为60min，然后将球磨后的混合粉末真空干燥去除正庚烷液体即得所述NdFeB/MnBi混合粉末；
步骤三、制备NdFeB/MnBi混合永磁
在手套箱中将步骤二中制得的NdFeB/MnBi混合粉末放入硬质合金无磁模具中，然后将该无磁模具放入磁场强度为2.5T的脉冲磁场成型机中在氩气氛围下对NdFeB/MnBi混合粉末取向成型，将成型后的NdFeB/MnBi混合粉末连同无磁模具一起放入放电等离子烧结炉中进行真空热压烧结，烧结工艺为：在1GPa压力下，3min内温度由室温升至300℃，然后保温5min，接着在1min内快速升温至600℃，之后在60min内快速降温至50℃，即制得各向异性的NdFeB/MnBi混合永磁，该NdFeB/MnBi混合永磁的密度为7.75g/cm3，如图1所示，制得的NdFeB/MnBi混合永磁在室温(25℃)及高温(100℃)下均具有较好磁性能，如图2所示，NdFeB/MnBi混合永磁还具有较好的取向。
实施例2，步骤一、首先制备MnBi合金粉末
配制摩尔比为1:1的MnBi的合金原料，利用真空电弧熔炼反复熔炼三次，从而得到成分均匀的合金铸锭，接着将合金铸锭破碎并以30m/s的甩带速度进行真空甩带，得到MnBi合金薄带，将MnBi合金薄带在真空热处理炉中进行真空热处理，真空热处理条件为：真空度为10-2Pa、加热温度为300℃，保温时间8h，然后将经真空热处理后的MnBi薄带放入手套箱中并破碎至80目，获得所述MnBi合金粉末；
步骤二、制备NdFeB/MnBi混合粉末
按质量比计算，将30％的MnBi合金粉末和70％的经HDDR处理后的市售各向异性NdFeB粉末混合均匀得到NdFeB/MnBi混合粉末。为获得混合均匀的NdFeB/MnBi混合粉末，采用两步球磨法，即：将所述MnBi合金粉末放入球磨罐中，并在正庚烷保护下进行首次滚动球磨，首次滚动球磨的球料比为10:1；球磨120min后放入NdFeB粉末进行二次滚动球磨，二次滚动球磨时间为60min，然后将球磨后的混合粉末真空干燥去除正庚烷液体即得所述NdFeB/MnBi混合粉末；
步骤三、制备NdFeB/MnBi混合永磁
在手套箱中将步骤二中制得的NdFeB/MnBi混合粉末放入硬质合金无磁模具中，然后将该无磁模具放入磁场强度为3T的脉冲磁场成型机中在氩气氛围下对NdFeB/MnBi混合粉末取向成型，将成型后的NdFeB/MnBi混合粉末连同无磁模具一起放入放电等离子烧结炉中进行真空热压烧结，烧结工艺为：在1GPa压力下，3min内温度由室温升至300℃，然后保温5min，接着在1min内快速升温至600℃，之后在60min内快速降温至30℃，即制得各向异性的NdFeB/MnBi混合永磁，该NdFeB/MnBi混合永磁的密度为7.95g/cm3，如图3所示，制得的NdFeB/MnBi混合永磁在室温(25℃)及高温(100℃)下均具有较好磁性能，如图4所示，NdFeB/MnBi混合永磁还具有较好的取向。
对比例1，将经HDDR处理后的市售各向异性的NdFeB粉末直接制备成致密各向异性磁体，具体步骤为：在手套箱中将NdFeB粉末放入硬质合金无磁模具中，然后将该无磁模具放入磁场强度为2.5T的脉冲磁场成型机中在氩气氛围下对NdFeB粉末取向成型，将成型后的样品连同无磁模具一起放入放电等离子烧结炉中进行真空热压烧结，烧结工艺为：在1GPa压力下，3min内温度由室温升至300℃，然后保温5min，接着在1min内快速升温至600℃，之后在60min内快速降温至50℃，即制得各向异性的NdFeB永磁，该NdFeB永磁的密度为7.53g/cm3。
在100℃下，分别测定实施例1、2中制得的NdFeB/MnBi混合永磁和对比例1中制得NdFeB永磁的磁性能，测试结果见表1。
表1
| 组别 | 剩磁(kGs) | 矫顽力(kOe) |
| 实施例1 | 7.4 | 8.4 |
| 实施例2 | 8.2 | 8.1 |
| 对比例1 | 9.1 | 7.2 |
从表1可以看出，添加了MnBi粉末的实施例1和实施例2制得的NdFeB/MnBi混合永磁的矫顽力显著高于未添加MnBi粉末的对比实施例1的矫顽力，结合图1-4可知实施例1和实施例2制得的NdFeB/MnBi混合永磁还具有较好的取向，且其退磁曲线表现出单向退磁特性，因此采用本发明提供的方法可显著改善NdFeB磁体的磁性能。
最后需要说明的是，上述描述仅仅为本发明的优选实施例，本领域的普通技术人员在本发明的启示下，在不违背本发明宗旨及权利要求的前提下，可以做出多种类似的表示，这样的变换均落入本发明的保护范围之内。
Claims (8)
1.一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于：制备MnBi合金粉末，按质量比计算，将20-30％的MnBi合金粉末和70-80％的NdFeB粉末混合后得到NdFeB/MnBi混合粉末，将该NdFeB/MnBi混合粉末放入磁场中取向成型，然后将成型后的NdFeB/MnBi混合粉末烧结即得NdFeB/MnBi混合永磁。
2.根据权利要求1所述的一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于制备MnBi合金粉末的步骤如下：配置MnBi合金原料，然后采用真空电弧熔炼将MnBi合金原料制成合金铸锭，接着将合金铸锭破碎并真空甩带制成MnBi合金薄带，最后将MnBi合金薄带进行真空热处理并破碎即得所述MnBi合金粉末。
3.根据权利要求1或2所述的一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于：制备所述NdFeB/MnBi混合粉末的方法为首先将MnBi合金粉末放入球磨罐中进行首次滚动球磨，然后再加入NdFeB粉末进行二次滚动球磨即得所述NdFeB/MnBi混合粉末。
4.根据权利要求3所述的一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于：所述首次滚动球磨是在正庚烷的保护下进行，按质量比计算，球料比为10:1球磨120min；所述二次滚动球磨的时间为60min。
5.根据权利要求1所述的一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于：所述磁场为脉冲磁场，磁场强度为2.5T，所述取向成型过程中在氩气氛围下进行。
6.根据权利要求2所述的一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于：所述真空热处理的条件为真空度10-2Pa，温度300℃，保温处理8h。
7.根据权利要求1、2、5或6所述的一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于：所述烧结条件为在3min内将温度升温至300℃，然后保温5min，接着在1min内将温度升温至600℃，最后在60min内快速降温至50℃即可，整个烧结过程中施加1GPa压力。
8.根据权利要求2所述的一种全致密各向异性NdFeB/MnBi混合永磁的制备方法，其特征在于：所述MnBi合金原料中按摩尔比计算Mn:Bi的摩尔比为1:1；所述NdFeB粉末为经HDDR处理后的各向异性NdFeB磁性粉末；所述MnBi合金粉末为80目。
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