CN110853854A - 一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法 - Google Patents

一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法 Download PDF

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CN110853854A
CN110853854A CN201911111736.5A CN201911111736A CN110853854A CN 110853854 A CN110853854 A CN 110853854A CN 201911111736 A CN201911111736 A CN 201911111736A CN 110853854 A CN110853854 A CN 110853854A
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刘卫强
陈昊
岳明
李智
尹彦涛
李玉卿
张红国
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Beijing University of Technology
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Abstract

一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，属于稀土磁性材料制备技术领域。两种主相合金的成分分别为RE‑Fe‑B(RE为Nd或Pr)和(Nd,MM)‑Fe‑B，MM为混合稀土。本发明工艺，先以PrHoFe合金速凝片为扩散源，在(Nd,MM)‑Fe‑B氢破碎的粉末颗粒表面均匀地包覆一层富PrHo的化合物，利用Pr2Fe14B、Ho2Fe14B较高的各向异性场来提高矫顽力；然后以ZrCu合金速凝片为扩散源，在经第一步扩散后的粉末颗粒表面均匀地包覆一层富Zr层，阻止烧结过程中含MM主相晶粒的长大以及抑制与双主相中另一主相之间的互扩散，从而获得高矫顽力。

Description

一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的 方法
技术领域：
本发明提供了一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，属于稀土磁性材料制备技术领域。
背景技术：
作为备受关注的第三代稀土永磁材料，烧结钕铁硼磁体因其具有优异的综合磁性能，在电子、电力机械、航天航空、交通运输等领域得到了广泛的应用，已经成为当今最重要的基础功能材料之一。然而，随着烧结钕铁硼磁体需求量的不断增加，消耗了大量的紧缺稀土元素Pr、Nd、Dy、Tb等，这也导致了其价格的上涨。因此使用高丰度稀土特别是未经分离的混合稀土来制备磁体，对于实现成本的控制、环境的保护和资源的平衡利用具有重大意义。混合稀土(MM,Misch-metal)是稀土原矿经初步处理后得到的产物，由La、Ce、Pr、Nd等元素组成，由于混合稀土中含有大量的La、Ce，而La2Fe14B、Ce2Fe14B的内禀磁性能远低于Pr和Nd，因此采用混合稀土制备磁体时，会导致磁体性能的恶化，特别是矫顽力严重下降。
对于提高钕铁硼磁体的矫顽力，主要是通过细化晶粒、晶界调控和晶界扩散技术。目前应用最广泛的是晶界扩散技术，主要是对烧结后的磁体扩散重稀土Dy、Tb或低熔点稀土合金。但是在扩散过程中，重稀土元素或低熔点合金在块状磁体基体中的扩散深度有限，使得晶界扩散技术存在一定的缺陷。因此通过一定的技术在粉末颗粒表面引入扩散元素来实现扩散源在粉末表面形成元素的扩散对于提高矫顽力效果更好，目前报道的主要是对气流磨细粉扩散Dy、Tb等重稀土元素，包括热阻蒸发沉积法(如专利201710624106.2)、磁控溅射法(如专利201110242847.7)和旋转蒸发扩散法(如专利201710852677.1)，但是这些方法都是对气流磨粉末进行扩散，由于气流磨粉末颗粒细小容易导致粉末严重氧化影响磁体性能，同时扩散Dy、Tb等重稀土元素成本太高，对于热阻蒸发沉积法和磁控溅射法对设备要求较高且不易于控制成本和实现产业化；而对于旋转蒸发扩散法由于扩散源和被扩散的气流磨细粉距离较远，同时在加热时气流磨细粉团聚更加严重，因此会导致扩散效果变差，对提高最终磁体的性能有限。
为了制备高性能的混合稀土铁硼磁体，我们采用双合金法来制备磁体，但对于混合稀土取代量较高的(MM,Nd)-Fe-B主相来说，由于高的混合稀土含量导致其性能较差，特别是由于MM替代后磁晶各向异性场明显降低而导致矫顽力低，同时在烧结过程中晶粒也更容易长大，最重要的是双主相磁体在后续的烧结和热处理过程中会发生严重的互扩散导致磁体性能严重恶化。因此本发明首先对混合稀土取代量较高的(MM,Nd)-Fe-B氢破碎粉末进行两步扩散处理，第一步扩散PrHoFe合金，在粉末颗粒表面均匀的包覆一层富PrHo的化合物，利用Pr2Fe14B、Ho2Fe14B较高的各向异性场来提高矫顽力；第二步扩散ZrCu合金，在粉末颗粒表面均匀的包覆一层富Zr的高熔点合金，阻止烧结过程中含MM的晶粒长大以及抑制与双主相中的另一主相Pr/Nd2Fe14B之间的互扩散，从而获得高矫顽力；采用该方法制备的磁体性价比高，且有望实现对中高档磁体的替代。
发明内容：
本发明提供了一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，目的是通过对性能较差的(MM,Nd)-Fe-B氢破碎粉末先进行两步扩散处理再通过双合金法来提高最终磁体的磁性能，得到低成本高性能的磁体。
一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，其特征在于主相A为Pr/Nd2Fe14B相，主相B为(MM,Nd)2Fe14B相，主相B的氢破碎粗粉经两次旋转扩散处理后再与主相A氢破碎粗粉混合均匀，主相A和主相B的质量比例为1:9～5:5(两者之和为10)。
主相A的名义成分为Pr/NdxFe100-x-y-zMyBz(wt.％)(即代表PrxFe100-x-y-zMyBz或NdxFe100-x-y-zMyBz)，主相B的名义成分为[MMaNd1-a]xFe100-x-y-zMyBz(wt.％)，MM为混合稀土，其中各成分的质量百分比为Ce:48-58％，La:20-30％，Pr:4-6％，Nd:15-17％；M为Nb、Ti、V、Co、Cr、Mn、Ni、Zr、Ga、Ag、Ta、Al、Au、Pb、Cu、Si中的一种或者几种；x、x1、y、z满足以下关系：0≤a≤1，25≤x≤35，0.5≤y≤3，0.3≤z≤1.5。
一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，其步骤如下：
(1)根据主相A的名义成分为Pr/NdxFe100-x-y-zMyBz、B的名义成分[MMaNd1-a]xFe100-x-y-zMyBz选择金属镨、混合稀土金属MM、其他金属M、金属钕、铁、铁硼合金放入坩埚中，真空下烘料完毕后充入氩气进行熔炼，然后浇到旋转的水冷铜辊上，铜辊转速1-4m/s，分别得到厚度为180-400μm的A、B两种成分的速凝薄带；
(2)采用真空感应速凝炉将PrHoFe合金和ZrCu合金分别制备成速凝薄带，然后粗破碎为(0.5-1.5)cm*(0.5-1.5)cm小方片；
(3)将步骤(1)中得到的A、B两种成分的速凝薄带分别进行氢破碎，脱氢后得到粗破碎的粗粉；
(4)将步骤(3)中成分B的氢破碎粗粉与步骤(2)中破碎的PrHoFe速凝片分别放置于一个同轴双层圆形料筒内层空腔和外层空腔中进行第一步扩散处理，两者的质量比为2∶1至1∶2，内层空腔和外层空腔采用金属钼网隔开，放入旋转热处理炉中以一定转速(1-10r/min)和500-700℃下进行扩散热处理3-6h，得到第一步扩散粗粉；所述的同轴双层圆形料筒的外层桶壁为料筒外壁，采用实料板材制成，同轴内层为金属钼网组成的金属钼网筒，金属钼网筒与料筒外壁之间的环形空腔结构为外层空腔，金属钼网筒内的腔体为内层空腔；金属钼网的网孔直径小于5μm；
(5)将步骤(4)中经第一步扩散处理后得到的第一步扩散粗粉与步骤(2)中破碎的ZrCu速凝片分别放置于所述的同轴双层圆形料筒内层空腔和外层空腔中进行第二步扩散处理得到第二步扩散粗粉，两者质量比为2∶1至1∶2，放入旋转热处理炉中以一定转速(1-10r/min)和800-950℃下进行扩散热处理2-5h，所述旋转热处理炉连接有手套箱，并充有惰性气体，使原料进出旋转热处理炉在手套箱进行操作；
(6)将步骤(3)中A成分氢破碎粗粉和步骤(5)中经两步扩散处理后的第二步扩散粗粉混合，使得主相A和主相B的质量比例为1:9～5:5(两者之和为10)；并添加0.01～5％质量比的润滑剂和0.01～5％质量比的防氧化剂，混合均匀后进行气流磨制粉，得到1～5μm的细粉；上述所述的质量百分比为占步骤(3)中A成分氢破碎粗粉和步骤(5)中经两步扩散处理后的第二步扩散粗粉两者之和的质量百分比；
(7)将步骤(6)制备的细粉再次添加0.01～5％质量比的润滑剂和0.01～5％质量比的防氧化剂混合均匀，在惰性气体保护下，将混合均匀的细粉在磁场强度为1.5-2.0T的磁场中取向成型，得到压坯，将压坯真空封装后进行冷等静压；上述所述的质量百分比为占步骤(6)细粉的质量百分比；
(8)将步骤(7)中得到的生坯放入真空烧结炉中进行烧结，在烧结温度980-1080℃保温1-4小时后通氩气风冷；为了抑制两相之间的互扩散对双主相磁体只进行低温回火热处理，回火温度为400-600℃，时间为2-5h。
PrHoFe合金的组成及质量百分比为：Pr的质量分数为40-80％，Ho的质量分数为10-40％，Fe的质量分数为10-20％；ZrCu合金的组成及质量百分比为：Zr的质量分数为35-65％，Cu的质量分数为35-65％。
润滑剂为本领域常规的润滑剂，防氧化剂为本领域常规的防氧化剂。
本发明与现有技术相比具有的优势：
(1)本发明采用混合稀土(MM)制备烧结磁体，实现了稀土资源的综合利用，减轻了分离提纯带来的环境污染，降低了生产成本；
(2)本发明采用两步旋转扩散的方法对含混合稀土(MM)的氢破碎粗粉扩散PrHoFe合金和ZrCu合金，既能在粉末颗粒的表面均匀包覆一层富PrHo的化合物，利用Pr2Fe14B、Ho2Fe14B较高的各向异性场来提高矫顽力，又能在粉末颗粒表面均匀的包覆一层富Zr的高熔点合金，阻止烧结过程中含MM的晶粒长大以及抑制与双主相中的另一主相Pr/Nd2Fe14B之间的互扩散，也有利于获得高矫顽力；
(3)本发明采用经两步旋转扩散后的(MM,Nd)-Fe-B氢破碎粗粉与Pr/Nd-Fe-B氢破碎粗粉混合制备双主相磁体，解决了(MM,Nd)-Fe-B合金磁晶各向异性场低的问题，双主相磁体中两相晶粒尺寸大小不均匀的问题，以及两种主相晶粒在后续烧结和热处理过程中的互扩散问题，最终制备的双主相磁体磁性能得到了明显的提高；
(4)本发明采用旋转扩散的方法对含混合稀土(MM)的氢破碎粗粉扩散PrHoFe合金和ZrCu合金，可以实现大批量生产提高生产效率，并且操作简单，极易实现工业化生产，而PrHoFe合金速凝片和ZrCu合金速凝片也可重复使用，大幅降低生产成本。
附图说明：
图1为本发明中扩散所使用的双层圆形料筒示意图；
图中：1-料筒外壁，2-内层金属钼网，3-(MM,Nd)-Fe-B氢破碎粗粉，4-扩散所用的PrHoFe或ZrCu速凝片；
具体实施方式：
下面结合实施例和对比例对本发明作进一步说明，但本发明并不限于以下实施例。
对比例1：
根据主相A的名义成分Pr31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)，主相B的名义成分(Nd0.5MM0.5)31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)(MM中La：27.49wt.％、Ce：53.93wt.％、Pr：1.86wt.％、Nd：16.72wt.％)，采用l.25m/s的铜辊转速，制备得到厚度为210μm的A、B两种成分速凝薄带。
将A、B两种成分的速凝薄带分别进行氢破碎，脱氢后得到粗破碎磁粉，然后分别加入质量比为0.05％的润滑剂和0.1％的防氧化剂充分混合均匀后在惰性气体保护气氛下，进行气流磨，得到A、B两种成分的气流磨细粉，平均粒度X50为2.10μm。
在手套箱中对A、B两种成分的气流磨细粉再次分别添加质量比为0.1％的润滑剂和0.2％的防氧化剂后充分混合均匀，在惰性气体保护气氛下，将A、B两种成分的磁粉在磁场强度为2.0T的磁场中取向成型，得到压坯，将压坯真空封装进行冷等静压后放入真空烧结炉中进行烧结，分别在烧结温度1060℃和1050℃保温2小时后通氩气风冷，然后进行一级回火和二级回火两步回火热处理，一级回火温度为900℃，时间3h；二级回火温度为450℃，时间4h。
将制备好的A、B两种成分的磁体放入BH测试仪中测试磁性能，结果如下:
磁体A：Br＝13.69kG，Hcj＝20.18kOe，(BH)max＝45.72MGOe，Hk/Hcj＝97.7％
磁体B：Br＝12.29kG，Hcj＝9.02kOe，(BH)max＝36.86MGOe，Hk/Hcj＝92.0％
对比例2：
根据主相A的名义成分Pr31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)，主相B的名义成分(Nd0.5MM0.5)31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)(MM中La：27.49wt.％、Ce：53.93wt.％、Pr：1.86wt.％、Nd：16.72wt.％)，采用l.25m/s的铜辊转速，制备得到厚度为210μm的A、B两种成分速凝薄带。
将A、B两种成分的速凝薄带进行氢破碎，脱氢后得到粗破碎磁粉。
将A、B两种成分氢破碎粗粉按质量比1:9和3:7分别混合，并加入质量比为0.05％的润滑剂和0.1％的防氧化剂充分混合均匀后在惰性气体保护气氛下进行气流磨，分别对应得到C、D两种成分的气流磨细粉，平均粒度X50为2.10μm。
在手套箱中对C、D两种成分的气流磨细粉再次分别添加质量比为0.1％的润滑剂和0.2％的防氧化剂充分混合均匀，在惰性气体保护气氛下，将C、D两种成分的磁粉在磁场强度为2.0T的磁场中取向成型，得到生坯，将生坯真空封装进行冷等静压后放入真空烧结炉中进行烧结，在烧结温度1050℃保温2小时后通氩气风冷，然后只进行低温回火热处理，回火温度为450℃，时间4h。
将制备好的C、D两种成分的双主相磁体放入BH测试仪中测试磁性能，结果如下:
双主相磁体C：Br＝12.53kG，Hcj＝9.53kOe，(BH)max＝38.11MGOe，Hk/Hcj＝93.4％
双主相磁体D：Br＝12.68kG，Hcj＝12.05kOe，(BH)max＝39.50MGOe，Hk/Hcj＝94.2％
实施例1：
根据主相A的名义成分Pr31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)，主相B的名义成分(Nd0.5MM0.5)31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)(MM中La：27.49wt.％、Ce：53.93wt.％、Pr：1.86wt.％、Nd：16.72wt.％)，采用l.25m/s的铜辊转速，制备得到厚度为210μm的A、B两种成分速凝薄带。
采用真空感应速凝炉分别制备名义成分为Pr65Ho20Fe15和Zr55Cu45的速凝薄带，并粗破碎为1cm*1cm左右的小方片。
将A、B两种成分的速凝片进行氢破碎，脱氢后得到粗破碎磁粉。
将成分B的氢破碎粗粉与破碎的Pr65Ho20Fe15速凝片以1∶1的质量比分别放置于一个双层圆形料筒内外层，料筒内外层用直径小于5μm的金属钼网隔开，放入旋转热处理炉中以5r/min的转速在630℃保温4h进行第一步扩散热处理；然后将第一步扩散热处理后的氢破碎粗粉与破碎的Zr55Cu45速凝片再次以1∶1的质量比放入旋转热处理炉中以5r/min的转速在885℃保温3h进行第二步扩散热处理，上述热处理过程先将热处理炉抽真空至5×10- 3Pa以下再充氩气至65kPa，在氩气保护气氛中进行，所述旋转热处理炉连接有手套箱，并充有惰性气体，使原料进出旋转热处理炉在手套箱中进行。
将成分A的氢破碎粗粉与扩散后成分B的氢破碎粗粉分别按质量比1:9和3:7混合，并分别加入质量比为0.05％的润滑剂和0.1％的防氧化剂充分混合均匀后在惰性气体保护气氛下，进行气流磨，得到C1、D1两种成分的气流磨细粉，平均粒度X50为2.10μm。
在手套箱中对C1、D1两种成分的气流磨细粉再次分别添加质量比为0.1％的润滑剂和0.2％的防氧化剂充分混合均匀，在惰性气体保护气氛下，将C1、D1两种成分的磁粉在磁场强度为2.0T的磁场中取向成型，得到压坯，将压坯真空封装进行冷等静压后放入真空烧结炉中进行烧结，在烧结温度1050℃保温2小时后通氩气风冷，然后只进行低温回火热处理，回火温度为450℃，时间4h。
将制备好的C1、D1两种成分的双主相磁体放入BH测试仪中测试磁性能，结果如下:
双主相磁体C1：Br＝12.65kG，Hcj＝14.87kOe，(BH)max＝39.76MGOe，Hk/Hcj＝96.7％
双主相磁体D1：Br＝12.92kG，Hcj＝16.95kOe，(BH)max＝41.31MGOe，Hk/Hcj＝96.5％
实施例2：
根据主相A的名义成分Pr31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)，主相B的名义成分(Nd0.5MM0.5)31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)(MM中La：27.49wt.％、Ce：53.93wt.％、Pr：1.86wt.％、Nd：16.72wt.％)，采用l.25m/s的铜辊转速，制备得到厚度为210μm的A、B两种成分速凝薄带。
采用真空感应速凝炉分别制备名义成分为Pr65Ho20Fe15和Zr55Cu45的速凝薄带，并粗破碎为1cm*1cm左右的小方片。
将A、B两种成分的速凝片进行氢破碎，脱氢后得到粗破碎磁粉。
将成分B的氢破碎粗粉与破碎的Pr65Ho20Fe15速凝片以1∶1的质量比分别放置于一个双层圆形料筒内外层，料筒内外层用直径小于5μm的金属钼网隔开，放入旋转热处理炉中以5r/min的转速在630℃保温4h进行第一步扩散热处理；然后将第一步扩散热处理后的氢破碎粗粉与破碎的Zr55Cu45速凝片再次以1∶1的质量比放入旋转热处理炉中以5r/min的转速在915℃保温3h进行第二步扩散热处理，上述热处理过程先将热处理炉抽真空至5×10- 3Pa以下再充氩气至65kPa，在氩气保护气氛中进行，所述旋转热处理炉连接有手套箱，并充有惰性气体，使原料进出旋转热处理炉在手套箱中进行。
将成分A的氢破碎粗粉与扩散后成分B的氢破碎粗粉按质量比1:9和3:7混合，并加入质量比为0.05％的润滑剂和0.1％的防氧化剂充分混合均匀后在惰性气体保护气氛下，进行气流磨，得到C2、D2两种成分的气流磨细粉，平均粒度X50为2.10μm。
在手套箱中对C2、D2两种成分的气流磨细粉再次添加质量比为0.1％的润滑剂和0.2％的防氧化剂充分混合均匀，在惰性气体保护气氛下，将C2、D2两种成分的磁粉在磁场强度为2.0T的磁场中取向成型，得到压坯，将压坯真空封装进行冷等静压后放入真空烧结炉中进行烧结，在烧结温度1050℃保温2小时后通氩气风冷，然后只进行低温回火热处理，回火温度为450℃，时间4h。
将制备好的C2、D2两种成分的双主相磁体放入BH测试仪中测试磁性能，结果如下:
双主相磁体C2：Br＝12.71kG，Hcj＝14.89kOe，(BH)max＝39.92MGOe，Hk/Hcj＝96.3％
双主相磁体D2：Br＝12.94kG，Hcj＝17.06kOe，(BH)max＝41.57MGOe，Hk/Hcj＝96.4％
实施例3：
根据主相A的名义成分Pr31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)，主相B的名义成分(Nd0.5MM0.5)31.5FebalAl0.4Cu0.2Co1Ga0.2Zr0.22B0.98(wt.％)(MM中La：27.49wt.％、Ce：53.93wt.％、Pr：1.86wt.％、Nd：16.72wt.％)，采用l.25m/s的铜辊转速，制备得到厚度为210μm的A、B两种成分速凝薄带。
采用真空感应速凝炉分别制备名义成分为Pr65Ho20Fe15和Zr55Cu45的速凝薄带，并粗破碎为1cm*1cm左右的小方片。
将A、B两种成分的速凝片进行氢破碎，脱氢后得到粗破碎磁粉。
将成分B的氢破碎粗粉与破碎的Pr65Ho20Fe15速凝片以1∶1的质量比分别放置于一个双层圆形料筒内外层，料筒内外层用直径小于5μm的金属钼网隔开，放入旋转热处理炉中以5r/min的转速在630℃保温4h进行第一步扩散热处理；然后将第一步扩散热处理后的氢破碎粗粉与破碎的Zr55Cu45速凝片再次以1∶1的质量比放入旋转热处理炉中以10r/min的转速在915℃保温3h进行第二步扩散热处理，上述热处理过程先将热处理炉抽真空至5×10- 3Pa以下再充氩气至65kPa，在氩气保护气氛中进行，所述旋转热处理炉连接有手套箱，并充有惰性气体，使原料进出旋转热处理炉在手套箱中进行。
将成分A的氢破碎粗粉与扩散后成分B的氢破碎粗粉按质量比1:9和3:7混合，并加入质量比为0.05％的润滑剂和0.1％的防氧化剂充分混合均匀后在惰性气体保护气氛下，进行气流磨，得到C3、D3两种成分的气流磨细粉，平均粒度X50为2.10μm。
在手套箱中对C3、D3两种成分的气流磨细粉再次添加质量比为0.1％的润滑剂和0.2％的防氧化剂充分混合均匀，在惰性气体保护气氛下，将C3、D3两种成分的磁粉在磁场强度为2.0T的磁场中取向成型，得到压坯，将压坯真空封装进行冷等静压后放入真空烧结炉中进行烧结，在烧结温度1050℃保温2小时后通氩气风冷，然后只进行低温回火热处理，回火温度为450℃，时间4h。
将制备好的C3、D3两种成分的双主相磁体放入BH测试仪中测试磁性能，结果如下:
双主相磁体C3：Br＝12.76kG，Hcj＝15.04kOe，(BH)max＝40.13MGOe，Hk/Hcj＝97.3％
双主相磁体D3：Br＝13.03kG，Hcj＝17.31kOe，(BH)max＝42.05MGOe，Hk/Hcj＝97.8％
上述所有的对比例和实施例中所用润滑剂均为本领域常规的润滑剂，所用防氧化剂均为本领域常规的防氧化剂。
表1对比例和实施例中各磁体的剩磁、矫顽力、最大磁能积和方形度。
Figure BDA0002271629940000081

Claims (5)

1.一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，其特征在于，主相A为Pr/Nd2Fe14B相，主相B为(MM,Nd)2Fe14B相，主相B的氢破碎粗粉经两次旋转扩散处理后再与主相A氢破碎粗粉混合均匀，主相A和主相B的质量比例为1:9～5:5，两者之和为10。
2.按照权利要求1所述的一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，其特征在于，主相A的名义成分为Pr/NdxFe100-x-y-zMyBz(wt.％)，主相B的名义成分为[MMaNd1-a]xFe100-x-y-zMyBz(wt.％)，MM为混合稀土，其中各成分的质量百分比为Ce:48-58％，La:20-30％，Pr:4-6％，Nd:15-17％；M为Nb、Ti、V、Co、Cr、Mn、Ni、Zr、Ga、Ag、Ta、Al、Au、Pb、Cu、Si中的一种或者几种；x、x1、y、z满足以下关系：0≤a≤1，25≤x≤35，0.5≤y≤3，0.3≤z≤1.5。
3.按照权利要求1或2所述的一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，其特征在于，具体包括以下步骤：
(1)根据主相A的名义成分为Pr/NdxFe100-x-y-zMyBz、B的名义成分[MMaNd1-a]xFe100-x-y-zMyBz选择金属镨、混合稀土金属MM、其他金属M、金属钕、铁、铁硼合金放入坩埚中，真空下烘料完毕后充入氩气进行熔炼，然后浇到旋转的水冷铜辊上，铜辊转速1-4m/s，分别得到厚度为180-400μm的A、B两种成分的速凝薄带；
(2)采用真空感应速凝炉将PrHoFe合金和ZrCu合金分别制备成速凝薄带，然后粗破碎为(0.5-1.5)cm*(0.5-1.5)cm小方片；
(3)将步骤(1)中得到的A、B两种成分的速凝薄带分别进行氢破碎，脱氢后得到粗破碎的粗粉；
(4)将步骤(3)中成分B的氢破碎粗粉与步骤(2)中破碎的PrHoFe速凝片分别放置于一个同轴双层圆形料筒内层空腔和外层空腔中进行第一步扩散处理，两者的质量比为2∶1至1∶2，内层空腔和外层空腔采用金属钼网隔开，放入旋转热处理炉中以一定转速(1-10r/min)和500-700℃下进行扩散热处理3-6h，得到第一步扩散粗粉；所述的同轴双层圆形料筒的外层桶壁为料筒外壁，采用实料板材制成，同轴内层为金属钼网组成的金属钼网筒，金属钼网筒与料筒外壁之间的环形空腔结构为外层空腔，金属钼网筒内的腔体为内层空腔；金属钼网的网孔直径小于5μm；
(5)将步骤(4)中经第一步扩散处理后得到的第一步扩散粗粉与步骤(2)中破碎的ZrCu速凝片分别放置于所述的同轴双层圆形料筒内层空腔和外层空腔中进行第二步扩散处理得到第二步扩散粗粉，两者的质量比为2∶1至1∶2，放入旋转热处理炉中以一定转速(1-10r/min)和800-950℃下进行扩散热处理2-5h，所述旋转热处理炉连接有手套箱，并充有惰性气体，使原料进出旋转热处理炉在手套箱进行操作；
(6)将步骤(3)中A成分氢破碎粗粉和步骤(5)中经两步扩散处理后的第二步扩散粗粉混合，使得主相A和主相B的质量比例为1:9～5:5；并添加0.01～5％质量比的润滑剂和0.01～5％质量比的防氧化剂，混合均匀后进行气流磨制粉，得到1～5μm的细粉；上述所述的质量百分比为占步骤(3)中A成分氢破碎粗粉和步骤(5)中经两步扩散处理后的第二步扩散粗粉两者之和的质量百分比；
(7)将步骤(6)制备的细粉再次添加0.01～5％质量比的润滑剂和0.01～5％质量比的防氧化剂混合均匀，在惰性气体保护下，将混合均匀的细粉在磁场强度为1.5-2.0T的磁场中取向成型，得到压坯，将压坯真空封装后进行冷等静压；上述所述的质量百分比为占步骤(6)细粉的质量百分比；
(8)将步骤(7)中得到的生坯放入真空烧结炉中进行烧结，在烧结温度980-1080℃保温1-4小时后通氩气风冷；为了抑制两相之间的互扩散对双主相磁体只进行低温回火热处理，回火温度为400-600℃，时间为2-5h。
4.按照权利要求3所述的一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，其特征在于，PrHoFe合金的组成及质量百分比为：Pr的质量分数为40-80％，Ho的质量分数为10-40％，Fe的质量分数为10-20％。
5.按照权利要求3所述的一种两步扩散法制备高性能双主相烧结混合稀土铁硼磁体的方法，其特征在于，ZrCu合金的组成及质量百分比为：Zr的质量分数为35-65％，Cu的质量分数为35-65％。
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