CN112341181A - 一种提高永磁铁氧体磁性能的方法 - Google Patents
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Abstract
一种提高永磁铁氧体磁性能的方法，包括以下步骤：（1）将永磁铁氧体预烧料加入球磨机中，同时向球磨机中加入添加剂碳酸钙、石英砂、金属铬粉和葡萄糖酸钙；（2）向球磨机中加入水，进行球磨，得永磁铁氧体料浆；（3）将步骤（2）所得永磁铁氧体料浆进行沉淀，过滤，得永磁铁氧体过滤料浆；（4）将步骤（3）所得永磁铁氧体过滤料浆注入模具，在磁场下加压成型，得永磁铁氧体生坯；（5）将步骤（4）所得永磁铁氧体生坯升温烧结，得永磁铁氧体产品。本发明方法选择金属铬粉作为添加剂之一，与传统的方法相比，提高了永磁铁氧体的磁性能，且降低了生产成本。
Description
技术领域
本发明涉及一种永磁铁氧体的制造方法，尤其涉及一种提高永磁铁氧体磁性能的方法。
背景技术
永磁铁氧体是一种用途广泛的基础功能材料，其具有较高的居里温度，耐腐蚀性，且原料来源广泛，价格低廉。目前永磁铁氧体主要用于各种永磁电机和扬声器等设备制造，但是随着设备小型化、轻量化的需求的不断增加，提升永磁铁氧体材料的磁性能也变得尤为迫切。
永磁铁氧体磁性能指标主要有剩磁（Br）和内禀矫顽力（Hcj），这两个指标越高，表明磁体的磁性能越好。其中剩磁正比于磁体的密度、晶粒取向度以及材料的饱和磁化强度（Ms）等，而内禀矫顽力与磁体中晶粒大小和磁晶各向异性参数有关。
目前传统的不添加稀土材料的永磁铁氧体，一般采用的添加剂包括：碳酸钙、石英砂、硼酸、氧化铝、氧化铬、分散剂（葡萄糖酸钙）等，但采用这些添加剂很难获得剩磁超过410mT和内禀矫顽力超过320 Oe的高性能永磁铁氧体产品。但现有高性能永磁铁氧体材料需要添加昂贵的稀土及钴类金属氧化物作为添加剂，导致高端永磁铁氧体产品的成本较高，降低了其市场竞争力。
发明内容
本发明要解决的技术问题是，克服现有技术存在的上述缺陷，提供一种在不添加稀土元素和氧化钴等昂贵添加剂的条件下，提高永磁铁氧体磁性能的方法。
本发明解决其技术问题所采用的技术方案是，一种提高永磁铁氧体磁性能的方法，包括以下步骤：
（1）将永磁铁氧体预烧料加入球磨机中，同时向球磨机中加入添加剂碳酸钙、石英砂、金属铬粉和葡萄糖酸钙；
（2）向球磨机中加入水，进行球磨，得永磁铁氧体料浆；
（3）将步骤（2）所得永磁铁氧体料浆进行沉淀，过滤，得永磁铁氧体过滤料浆；
（4）将步骤（3）所得永磁铁氧体过滤料浆注入模具，在磁场下加压成型，得永磁铁氧体生坯；
（5）将步骤（4）所得永磁铁氧体生坯升温烧结，得永磁铁氧体产品。
进一步，步骤（1）中，所述碳酸钙的添加量为永磁铁氧体预烧料质量的0.3~1.0%，优选为0.7~0.9%，最优选0.8 %。
进一步，步骤（1）中，所述石英砂的添加量为永磁铁氧体预烧料质量的0.20~0.4%，优选为0.2~0.3%，最优选0.25%。适量的碳酸钙和石英砂的添加有利于提高磁体的密度同时抑制晶粒的过度生长。
进一步，步骤（1）中，所述金属铬粉的添加量为永磁铁氧体预烧料质量的0.1~1.5%，优选0.5~0.7%，最优选0.6%。研究表明，添加适量的金属铬粉有利于提高磁体密度的同时，改善磁体的围观结构，因此可以使得磁体的矫顽力获得大幅度的提高的情况下，保持高剩磁。不过金属铬粉添加过多，磁体的内禀矫顽力虽然仍会继续大幅度提高，但是剩磁会明显下降。
进一步，步骤（1）中，所述葡萄糖酸钙的添加量为永磁铁氧体预烧料质量的0.1~0.5%。葡萄糖酸钙的添加有助于改善球磨过程中料浆的粒度分布，同时改善成型阶段颗粒的取向性，从而提高材料的剩磁和内禀矫顽力。
进一步，步骤（2）中，所述水的添加量为永磁铁氧体预烧料质量的1.3~1.5倍，所述球磨为球磨至料浆中的固体颗粒的粒度为达到0.70 ~0.80μm。加水量过少会导致球磨效率降低，同时会造成球磨时间大幅度延长，加水量过多会造成粒度分布范围宽，影响产品合格率；当球磨所得的料浆中的固体颗粒的粒度低于0.70μm时，料浆成型的难度过大；球磨所得的料浆中的固体颗粒的粒度大于0.80μm时，葡萄糖酸钙对料浆的分散做用会降低，从而导致料浆无法在成型阶段获得良好的取向性。
进一步，步骤（3）中，所述永磁铁氧体过滤至料浆的含水量为30~40 wt%。含水量过高，会导致成型阶段排水困难，造成产品出现裂纹等不良缺陷，含水量过低，则会造成填料困难，导致产品烧结后外观一致性差。
进一步，步骤（4）中，所述磁场的强度范围为450~950kA/m。磁场强度过低会导致料浆中的一定比例的细粒度颗粒无法取向，磁场强度过高并不会获得更高的取向度且会导致高能耗。
进一步，步骤（5）中，所述升温的速率≤5℃/min。
进一步，步骤（5）中，所述烧结的温度为1140~1200℃；所述烧结的时间为0.5~3.0h。升温速率控制在3℃/min，同时烧结温度控制在1160℃最为优选。升温速度过低会导致烧结效率低下，升温速度过高会导致磁体开裂，添加的金属铬粉具有助熔作用，可以有效降低烧结温度。
本发明具有以下有益效果：与传统的单独或者复合添加氧化铬和氧化铝的方法相比，采用复合添加碳酸钙、石英砂、金属铬粉和葡萄糖酸钙的方法，对永磁铁氧体的磁性能进行明显改善，选用金属铬粉作为添加剂之一，能在获得高内禀矫顽力的前提下，避免剩磁的大幅度下降，从而获得剩磁和内禀矫顽力均较高的永磁铁氧体产品，且生产成本较低。
具体实施方式
下面结合实施例对本发明作进一步说明。
实施例1-3
（1）将1000g永磁铁氧体预烧料、碳酸钙、石英砂、葡萄糖酸钙、金属铬粉加入球磨机中，其中添加剂的添加量见表1。
（2）然后加入1400g水，球磨至粒度为0.75μm，得永磁铁氧体料浆；
（3）将步骤（2）所得永磁铁氧体料浆沉淀过滤至含水量为32wt%，得永磁铁氧体过滤料浆；
（4）将步骤（3）所得永磁铁氧体过滤料浆注入模具，在磁场强度为480kA/m的条件下加压成型，得直径Φ30.1mm的永磁铁氧体生坯；
（5）将步骤（4）所得永磁铁氧体生坯以3℃/min速率升温，然后在1160℃下烧结2h，得永磁铁氧体。
将所得永磁铁氧体的上下两表面磨削抛光，采用TYU-2000型磁性材料自动测量装置对其进行磁性能测试，测试结果参见表2。
对比例1
本对比例中的原料和工艺参数与对比例1相同，其区别仅在于：步骤（1）中添加氧化铬替代金属铬粉。
对比例2
本对比例中的原料和工艺参数与对比例1相同，其区别仅在于：步骤（1）中添加氧化铬和氧化铝替代金属铬粉。
将所得永磁铁氧体的上下两表面磨削抛光，采用TYU-2000型磁性材料自动测量装置对其进行磁性能测试，测试结果参见表2。
表1 实施例1-3和对比例1、2所采用的添加剂
注：“-”表示未添加。
表2 实施例1-3和对比例1、2的测试结果
与对比例1相比，本发明实施例中添加金属铬粉后，材料的Br和Hcj均有所提高。当金属铬粉添加量为0.6wt%、碳酸钙添加量为0.8 wt%时，石英砂添加量0.25%、葡萄糖酸钙添加量0.3%的情况下，Br高13.1mT，Hcj高6.2 kA/m。
与对比例2相比，当金属铬粉添加量为0.6wt%、碳酸钙添加量为0.8 wt%时，石英砂添加量0.25%、葡萄糖酸钙添加量0.3%的情况下，Br高17.3mT，Hcj高3.8 kA/m；
综上所述，采用金属铬粉作为添加剂与传统的采用氧化铬和氧化铝作为添加剂相比，更能够有效地提高永磁铁氧体材料的磁性能。
Claims (10)
1.一种提高永磁铁氧体磁性能的方法，其特征在于，包括以下步骤：
（1）将永磁铁氧体预烧料加入球磨机中，同时向球磨机中加入添加剂碳酸钙、石英砂、金属铬粉和葡萄糖酸钙；
（2）向球磨机中加入水，进行球磨，得永磁铁氧体料浆；
（3）将步骤（2）所得永磁铁氧体料浆进行沉淀，过滤，得永磁铁氧体过滤料浆；
（4）将步骤（3）所得永磁铁氧体过滤料浆注入模具，在磁场下加压成型，得永磁铁氧体生坯；
（5）将步骤（4）所得永磁铁氧体生坯升温烧结，得永磁铁氧体产品。
2.根据权利要求1所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（1）中，所述碳酸钙的添加量为永磁铁氧体预烧料质量的0.3~1.0%，优选为0.7~0.9%，最优选0.8 %。
3.根据权利要求1或2所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（1）中，所述石英砂的添加量为永磁铁氧体预烧料质量的0.20~0.4%，优选为0.2~0.3%，最优选0.25%。
4.根据权利要求1~3之一所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（1）中，所述金属铬粉的添加量为永磁铁氧体预烧料质量的0.1~1.5%，优选0.5~0.7%，最优选0.6%。
5.根据权利要求1~4之一所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（1）中，所述葡萄糖酸钙的添加量为永磁铁氧体预烧料质量的0.1~0.5%。
6.根据权利要求1~5所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（2）中，所述水的添加量为永磁铁氧体预烧料质量的1.3~1.5倍，所述球磨为球磨至料浆中的固体颗粒的粒度达到0.70 ~0.80μm。
7.根据权利要求1~6之一所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（3）中，所述永磁铁氧体过滤至料浆的含水量为30~40 wt%。
8.根据权利要求1~7之一所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（4）中，所述磁场的强度范围为450~950kA/m。
9.根据权利要求1~8之一所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（5）中，所述升温的速率≤5℃/min。
10.根据权利要求1~9之一所述的提高永磁铁氧体磁性能的方法，其特征在于，步骤（5）中，所述烧结的温度为1140~1200℃，烧结的时间为0.5~3.0h。
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| CN113562769A (zh) * | 2021-06-07 | 2021-10-29 | 北矿磁材（阜阳）有限公司 | 一种提高粘结永磁铁氧体材料磁性能的分散剂及方法 |
| WO2022105390A1 (zh) * | 2020-11-17 | 2022-05-27 | 湖南航天磁电有限责任公司 | 一种提高永磁铁氧体磁性能的方法 |
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