CN111916285A - 一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法 - Google Patents
一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法 Download PDFInfo
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Abstract
本发明公开了一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法，包括：采用气相沉积的方法，在钕铁硼粉末上同步进行M金属和R‑R或R‑H金属的沉积而形成金属混合镀层，其中M金属为Mo/W/Zr/Ti/Nb中的至少一种,R为Pr/Nd/La/Ce中的至少一种,H为Cu/Al/Ga中的一种,之后取向压制成型、真空烧结时效处理，最终获得高矫顽力烧结钕铁硼磁体。本发明利用烧结时效过程中，钕铁硼粉末表面的混合镀层中的高熔点的M金属作为支撑部分，将不同主相晶粒支撑起来形成晶界通道，混合镀层中低熔点的R‑R/R‑H在晶界通道内液相流动扩散形成网状晶界相，使得钕铁硼磁体的矫顽力显著提高。
Description
技术领域
本发明涉及稀土材料制备技术领域，具体是涉及一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法。
背景技术
钕铁硼永磁材料是我国稀土行业最为关注的稀土应用产业，随着科学技术的发展和技术的进步对高性能钕铁硼永磁材料的需求日益广泛。烧结钕铁硼的矫顽力是一个十分重要的磁参量，且是组织结构敏感参量，其主要受磁体的主相晶粒的HA影响和主相晶粒间的晶界影响，主相晶粒的HA越大磁体的最终矫顽力越大，主相晶粒间的晶界越宽，越连续，磁体的矫顽力越高。
轻稀土辅助合金的双合金方法利用轻稀土合金熔点低，在高于其熔点的某一温度热处理，发生液态扩散，在主相晶粒周围呈薄层网格状分布，可以实现主相晶粒的良好隔离和去磁耦合作用，从而提高磁体矫顽力。然而传统的双合金技术，由于不能实现晶界相完全的分割主相晶粒，进而导致钕铁硼磁体矫顽力增加幅度不大。
磁粉表面扩散法，在钕铁硼磁粉表面镀上一层轻稀土膜层，之后再对其进行压型，烧结可以很好的提高钕铁硼磁体的矫顽力。例如专利文件CN104124052A 公布了使用磁控溅射的方法在钕铁硼磁体粉末上沉积轻稀土合金后，之后再进行压型，烧结，利用烧结过程中磁粉表面的轻稀土合金的液态扩散，扩宽晶界相和连接晶界相并形成网状晶界分布，制备高性能钕铁硼烧结磁体。然而上述专利中由于磁粉表面的镀层全部为低熔点金属，在烧结时效过程中，磁粉表面的镀层全部参与了液态扩散中的流动等，导致不同主相晶粒之间由于晶界相的流动而极易发生直接的接触，因此不能保证所制备的烧结钕铁硼磁体中，不同主相晶粒之间的完全隔离，因此采用上述磁粉表面扩散法制备的烧结钕铁硼磁体的矫顽力较未采用磁粉表面扩散法的所制备的烧结钕铁硼磁体的矫顽力提高幅度不高。
发明内容
本发明的目的在于解决传统磁粉表面扩散法存在的难以形成均匀网状晶界相，而导致钕铁硼磁体矫顽力提升幅度较低的问题，而提供一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法。
本发明提供的技术方案，其特出之处在于，包括如下步骤：
a、按照成分设计配制钕铁硼合金原料，将配制好的原料经熔炼，速凝甩片，制备钕铁硼合金薄片，将钕铁硼合金薄片在氢处理炉内，进行吸氢处理和高温脱氢处理，之后经气流磨制备钕铁硼合金粉末；
b、采用气相沉积的方法，在钕铁硼粉末上同步进行M金属和R-R或R-H金属的沉积而形成混合金属镀层，其中M金属为Mo/W/Zr/Ti/Nb中的至少一种, R为Pr/Nd/La/Ce中的至少一种， H为Cu/Al/Ga中的一种。
c、将所得沉积有混合金属层的钕铁硼粉末在磁场取向压制成型、冷等静压、真空烧结时效，获得高矫顽力钕铁硼磁体。
上述制备方法中，步骤a 中所述钕铁硼合金粉末的平均粒径为2-6μm，作为优选的实施例中，钕铁硼合金粉末的平均粒径为3-5μm。
上述制备方法中，步骤b中所述气相沉积方法为磁控溅射方法。
上述制备方法中，步骤b中所述混合金属镀层的厚度3-100nm，作为优选的实施例中，混合金属镀层的厚度为20-50nm。
上述制备方法中，混合金属镀层中R-R金属或者R-H金属与M金属的重量比范围为5:1到50:1，作为优选的实施例中，混合金属镀层中R-R金属或者R-H金属与M金属的重量比范围为10:1到30:1。
上述制备方法中，工艺步骤c中的烧结时效阶段中，烧结温度的范围1000℃-1150℃，烧结时间为2-10h,作为优选的实施例中,烧结温度范围为1050℃-1100℃，烧结时间为4-6h.
与现有技术相比，本发明有益之处在于：
通过在钕铁硼磁粉表面沉积混合金属镀层，并利用烧结时效过程中，钕铁硼磁粉表面混合镀层中高熔点的Mo/W/Zr/Ti/Nb金属部分作为支撑部分，将不同主相晶粒之间支撑起来形成晶界通道，混合镀层中低熔点的轻稀土合金在晶界通道内液相流动扩散形成均匀的网状晶界相，使得钕铁硼磁体的矫顽力显著提高。本专利与现有技术相比，本专利所制备的钕铁硼磁体组织结构均匀，网状晶界相均匀明显且磁体矫顽力高。
附图说明
图1为钕铁硼合金粉末表面沉积混合金属镀层的示意图。
标记说明： 1、钕铁硼合金粉末颗粒，2、M金属颗粒，3、H-L/H-H金属颗粒。
具体实施方式
下述实施例是对本发明内容的进一步说明以作为对本发明技术内容的阐释，但本发明的实质内容并不限于下述实施例所述，本领域的普通技术人员可以且应当知晓任何基于本发明实质精神的简单变化或者替换均应属于本发明所要求的保护范围。
对于本申请以下实施例，钕铁硼合金粉末的形成均采用同一原料及同样的工艺制作，便于进行性能比较，每个实施例仅在于钕铁硼合金粉末的粒度不同，每个实施例对于选取的钕铁硼合金粉末，均分为A组、B组，其中A钕铁硼合金粉末不进行任何处理，B组采用本申请的气相沉积方法形成混合金属镀层,在钕铁硼粉末上同步进行M金属和R-R或R-H金属的沉积而形成混合金属镀层，同步进行是指同时开启和同时关闭，气象沉积镀膜的过程中可以同时在钕铁硼粉末上面进行两种膜层的沉积，形成混合镀层。
钕铁硼合金粉末的制作具体为，熔炼制备成分为质量分数为Nd:23.4%，Pr:5.1%，AL:0.45%，Co:0.5%，Cu:0.15%，Ga:0.2%，B:0.93%，Ho:2.0%，Ti:0.15% 剩余成分为Fe的钕铁硼速凝薄片。将母合金速凝薄片氢爆破碎后，在粉料中添加占合金总重量为1%的专用防氧化剂和0.2%的润滑剂，充分混合后置于气流磨中进一步破碎，制成平均钕铁硼合金粉末。
实施例1
制作平均粒度为2μm的钕铁硼合金粉末均匀的分成A,B两份，其中A钕铁硼合金粉末不进行任何处理，使用磁控溅射设备并同时开启磁控设备内的W靶材和Pr靶材,在B钕铁硼磁粉表面同时进行W金属和Pr金属膜层的沉积，并控制Pr靶材和W靶材的沉积速度比例为5:1，并控制混合膜层厚度为3nm左右。
之后将处理后的A钕铁硼合金粉末和B钕铁硼合金粉末分别在1.8T的磁场中取向成型，再经180Mpa冷等静压压制成胚料。
将压胚在1000℃真空烧结10h,再经850℃一级回火6h和500℃二级回火处理5h,制成烧结钕铁硼磁体。
将经过上述工艺制作的A烧结钕铁硼烧结钕铁硼磁体和B烧结钕铁硼磁体切割后测试磁性能（温度20℃±3℃），并将测试结果记录在表1中。
表1
| 磁体品名 | Br（KGs) | Hcj（KOe) | Hk/Hcj |
| A磁体 | 13.45 | 17.9 | 0.98 |
| B磁体 | 13.41 | 19.7 | 0.98 |
由表1可见，实施例1中在钕铁硼合金粉末成分相同的情况下，经过本申请所述方式制备的烧结钕铁硼磁体的矫顽力Hcj增加了1.8koe，增加效果明显。
实施例2
制作平均粒度为3μm的钕铁硼合金粉末均匀的分成A,B两份，其中A钕铁硼合金粉末不进行任何处理，使用磁控溅射设备并同时开启磁控设备内的Mo靶材和NdCu靶材,在B钕铁硼磁粉表面同时进行Mo金属和NdCu金属膜层的沉积，并控制NdCu靶材和Mo靶材的沉积速度比例为20:1，并控制混合膜层厚度为20nm左右。
之后将处理后的A钕铁硼合金粉末和B钕铁硼合金粉末分别在1.8T的磁场中取向成型，再经180Mpa冷等静压压制成胚料。
将压胚在1100℃真空烧结4h,再经850℃一级回火6h和500℃二级回火处理5h,制成烧结钕铁硼磁体。
将经过上述工艺制作的A烧结钕铁硼烧结钕铁硼磁体和B烧结钕铁硼磁体切割后测试磁性能（温度20℃±3℃），并将测试结果记录在表2中。
表2
| 磁体品名 | Br（KGs) | Hcj（KOe) | Hk/Hcj |
| A磁体 | 13.44 | 18.2 | 0.98 |
| B磁体 | 13.35 | 21.3 | 0.98 |
由表2可见，实施例2中在钕铁硼合金粉末成分相同的情况下，经过本申请所述方式制备的烧结钕铁硼磁体的矫顽力Hcj增加了3.1 koe，增加效果明显。
实施例3
制作平均粒度为4μm的钕铁硼合金粉末均匀的分成A,B两份，其中A钕铁硼合金粉末不进行任何处理，使用磁控溅射设备并同时开启磁控设备内的Zr靶材和Nd靶材,在B钕铁硼磁粉表面同时进行Zr金属和Nd金属膜层的沉积，并控制Nd靶材和Zr靶材的沉积速度比例为30:1，并控制混合膜层厚度为30nm左右。
之后将处理后的A钕铁硼合金粉末和B钕铁硼合金粉末分别在1.8T的磁场中取向成型，再经180Mpa冷等静压压制成胚料。
将压胚在1050℃真空烧结8h,再经850℃一级回火6h和500℃二级回火处理5h,制成烧结钕铁硼磁体。
将经过上述工艺制作的A烧结钕铁硼烧结钕铁硼磁体和B烧结钕铁硼磁体切割后测试磁性能（温度20℃±3℃），并将测试结果记录在表3中。
表3
| 磁体品名 | Br（KGs) | Hcj（KOe) | Hk/Hcj |
| A磁体 | 13.46 | 18.00 | 0.98 |
| B磁体 | 13.4 | 21.9 | 0.98 |
由表3可见，实施例3中在钕铁硼合金粉末成分相同的情况下，经过本申请所述方式制备的烧结钕铁硼磁体的矫顽力Hcj增加了3.9koe，增加效果明显。
实施例4
制作平均粒度为5μm的钕铁硼合金粉末均匀的分成A,B两份，其中A钕铁硼合金粉末不进行任何处理，使用磁控溅射设备并同时开启磁控设备内的Nb靶材和PrAl靶材,在B钕铁硼磁粉表面同时进行Nb金属和PrAl金属膜层的沉积，并控制PrAl靶材和Nb靶材的沉积速度比例为10:1，并控制混合膜层厚度为50nm左右。
之后将处理后的A钕铁硼合金粉末和B钕铁硼合金粉末分别在1.8T的磁场中取向成型，再经180Mpa冷等静压压制成胚料。
将压胚在1150℃真空烧结2h,再经850℃一级回火6h和500℃二级回火处理5h,制成烧结钕铁硼磁体。
将经过上述工艺制作的A烧结钕铁硼烧结钕铁硼磁体和B烧结钕铁硼磁体切割后测试磁性能（温度20℃±3℃），并将测试结果记录在表4中。
表4
| 磁体品名 | Br（KGs) | Hcj（KOe) | Hk/Hcj |
| A磁体 | 13.44 | 17.9 | 0.98 |
| B磁体 | 13.34 | 23.8 | 0.98 |
由表4可见，实施例4中在钕铁硼合金粉末成分相同的情况下，经过本申请所述方式制备的烧结钕铁硼磁体的矫顽力Hcj增加了5.9koe，增加效果明显。
实施例5
制作平均粒度为6μm的钕铁硼合金粉末均匀的分成A,B两份，其中A钕铁硼合金粉末不进行任何处理，使用磁控溅射设备并同时开启磁控设备内的Ti靶材和LaGa靶材,在B钕铁硼磁粉表面同时进行Ti金属和LaGa金属膜层的沉积，并控制LaGa靶材和Ti靶材的沉积速度比例为50:1，并控制混合膜层厚度为100nm左右。
之后将处理后的A钕铁硼合金粉末和B钕铁硼合金粉末分别在1.8T的磁场中取向成型，再经180Mpa冷等静压压制成胚料。
将压胚在1020℃真空烧结8h,再经850℃一级回火6h和500℃二级回火处理5h,制成烧结钕铁硼磁体。
将经过上述工艺制作的A烧结钕铁硼烧结钕铁硼磁体和B烧结钕铁硼磁体切割后测试磁性能（温度20℃±3℃），并将测试结果记录在表5中。
表5
| 磁体品名 | Br（KGs) | Hcj（KOe) | Hk/Hcj |
| A磁体 | 13.46 | 17.8 | 0.98 |
| B磁体 | 13.12 | 21.2 | 0.97 |
由表5可见，实施例5中在钕铁硼合金粉末成分相同的情况下，经过本申请所述方式制备的烧结钕铁硼磁体的矫顽力Hcj增加了3.4koe，增加效果明显。
以上描述仅是示例性和解释性的，并不限制本发明。以上实施例表明，在钕铁硼粉末相同成分的情况下，本专利所公布的通过在钕铁硼沉积混合金属膜层后再进行压制成型，烧结时效所制备的烧结钕铁硼磁体的矫顽力增加效果明显。
Claims (6)
1.一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法，其特征在于，包括下述步骤：
a、将配制好的钕铁硼合金原料经熔炼、速凝甩片，形成钕铁硼合金薄片，将钕铁硼合金薄片在氢处理炉内，进行吸氢处理和高温脱氢处理，之后经气流磨制备钕铁硼合金粉末；
b、采用气相沉积的方法，在钕铁硼粉末上同步进行M金属和R-R或R-H金属的沉积而形成混合金属镀层，其中M金属为Mo/W/Zr/Ti/Nb中的至少一种, R为Pr/Nd/La/Ce中的至少一种，H为Cu/Al/Ga中的一种；
c、将所得沉积有混合金属镀层的钕铁硼粉末在磁场取向压制成型、冷等静压、真空烧结时效，获得高矫顽力钕铁硼磁体。
2.如权利要求1所述的一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法，其特征在于：步骤a中所述钕铁硼合金粉末的粒径范围为2-6μm。
3.如权利要求1所述的一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法，其特征在于：步骤b中所述气相沉积方法为磁控溅射方法。
4.如权利要求1所述的一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法，其特征在于：步骤b中所述混合金属镀层的厚度3-100nm。
5.如权利要求1或4所述的一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法，其特征在于：步骤b中所述混合金属镀层中R-R金属或者R-H金属与M金属的重量比范围为5:1到50:1。
6.如权利要求1所述的一种低重稀土高矫顽力烧结钕铁硼磁体的制备方法，其特征在于：步骤c中所述烧结时效过程中烧结温度范围为1000℃-1150℃，烧结时间范围为2-10h。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112863848A (zh) * | 2021-01-15 | 2021-05-28 | 烟台首钢磁性材料股份有限公司 | 高矫顽力烧结钕铁硼磁体的制备方法 |
| CN113380528A (zh) * | 2021-06-15 | 2021-09-10 | 中钢天源股份有限公司 | 一种烧结钕铁硼晶界重塑的方法 |
| EP4156210A1 (en) * | 2021-09-24 | 2023-03-29 | Yantai Dongxing Magnetic Materials Inc. | A low-cost rare earth magnet and corresponding manufacturing method thereof |
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| CN114455600B (zh) * | 2020-11-10 | 2023-02-21 | 海南热带海洋学院 | 一种稀土或碱土六硼化物纳米粉体的制备方法及应用 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130266471A1 (en) * | 2012-04-04 | 2013-10-10 | GM Global Technology Operations LLC | Vibration Machines for Powder Coating |
| CN103456452A (zh) * | 2013-09-12 | 2013-12-18 | 南京理工大学 | 低镝耐腐蚀烧结钕铁硼制备方法 |
| CN106783130A (zh) * | 2016-12-21 | 2017-05-31 | 包头稀土研究院 | 制备低重稀土高矫顽力钕铁硼磁体的方法 |
| CN108470615A (zh) * | 2018-05-11 | 2018-08-31 | 包头稀土研究院 | 高磁能积高矫顽力烧结钕铁硼磁体的制备方法 |
| CN108735494A (zh) * | 2018-05-24 | 2018-11-02 | 北京京磁电工科技有限公司 | 高矫顽力钕铁硼磁体的制备方法 |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101456841B1 (ko) * | 2006-09-14 | 2014-11-03 | 가부시키가이샤 알박 | 영구자석 및 영구자석의 제조방법 |
| WO2011070847A1 (ja) * | 2009-12-09 | 2011-06-16 | 愛知製鋼株式会社 | 希土類異方性磁石粉末およびその製造方法とボンド磁石 |
| WO2012114530A1 (ja) * | 2011-02-21 | 2012-08-30 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
| CN104124052A (zh) | 2014-07-25 | 2014-10-29 | 安徽大地熊新材料股份有限公司 | 一种高性能稀土－铁－硼系烧结永磁体的制备方法 |
| CN106384639B (zh) * | 2016-10-28 | 2018-04-03 | 北京科技大学 | 一种高性能粘结钕铁硼永磁材料的制备方法 |
| WO2018113717A1 (zh) * | 2016-12-21 | 2018-06-28 | 包头稀土研究院 | 钕铁硼永磁材料的制备方法 |
| CN114974874B (zh) * | 2022-06-28 | 2023-09-12 | 安徽大地熊新材料股份有限公司 | 利用废旧烧结钕铁硼磁体制备再生磁体的方法 |
-
2020
- 2020-08-08 CN CN202010792279.7A patent/CN111916285A/zh active Pending
-
2021
- 2021-08-05 EP EP21189825.9A patent/EP3955268A1/en active Pending
- 2021-08-06 US US17/395,494 patent/US20220044853A1/en active Pending
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130266471A1 (en) * | 2012-04-04 | 2013-10-10 | GM Global Technology Operations LLC | Vibration Machines for Powder Coating |
| CN103456452A (zh) * | 2013-09-12 | 2013-12-18 | 南京理工大学 | 低镝耐腐蚀烧结钕铁硼制备方法 |
| CN106783130A (zh) * | 2016-12-21 | 2017-05-31 | 包头稀土研究院 | 制备低重稀土高矫顽力钕铁硼磁体的方法 |
| CN108470615A (zh) * | 2018-05-11 | 2018-08-31 | 包头稀土研究院 | 高磁能积高矫顽力烧结钕铁硼磁体的制备方法 |
| CN108735494A (zh) * | 2018-05-24 | 2018-11-02 | 北京京磁电工科技有限公司 | 高矫顽力钕铁硼磁体的制备方法 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112863848A (zh) * | 2021-01-15 | 2021-05-28 | 烟台首钢磁性材料股份有限公司 | 高矫顽力烧结钕铁硼磁体的制备方法 |
| CN112863848B (zh) * | 2021-01-15 | 2023-04-11 | 烟台东星磁性材料股份有限公司 | 高矫顽力烧结钕铁硼磁体的制备方法 |
| US11854736B2 (en) | 2021-01-15 | 2023-12-26 | Yantai Dongxing Magnetic Materials Inc. | Method of preparing a high-coercivity sintered NdFeB magnet |
| CN113380528A (zh) * | 2021-06-15 | 2021-09-10 | 中钢天源股份有限公司 | 一种烧结钕铁硼晶界重塑的方法 |
| EP4156210A1 (en) * | 2021-09-24 | 2023-03-29 | Yantai Dongxing Magnetic Materials Inc. | A low-cost rare earth magnet and corresponding manufacturing method thereof |
| JP2023047305A (ja) * | 2021-09-24 | 2023-04-05 | 煙台東星磁性材料株式有限公司 | Ｎｄ－Ｆｅ－Ｂ系磁性体及びその製造方法 |
| JP7325921B2 (ja) | 2021-09-24 | 2023-08-15 | 煙台東星磁性材料株式有限公司 | Ｎｄ－Ｆｅ－Ｂ系磁性体及びその製造方法 |
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