CN109111219A - 一种永磁铁氧体材料的制备方法 - Google Patents
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
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- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种永磁铁氧体材料的制备方法，主要解决现有永磁铁氧体材料在成型时料浆脱水困难、成型难度大、容易发生粘模的技术问题。本发明方法包括以下步骤：湿法混料；一次预烧；粗粉碎；湿磨制浆；湿压磁场成型；二次烧结；熟坯打磨。本发明通过控制主原料中Fe2O3和SrCO3的摩尔比为6.2—6.5和预烧料粗粉的pH值为7—9，降低了永磁铁氧体材料的制备成本，制得永磁铁氧体材料的剩余磁感应强度Br为420±10mT，矫顽力Hcb为266±12kA/m，内禀矫顽力Hcj≥305kA/m。
Description
技术领域
本发明涉及一种永磁材料的制备方法，特别涉及一种永磁铁氧体材料的方法，属于磁性材料的制造领域。
背景技术
铁氧体永磁材料是以Fe2O3为主要组元的复合氧化物永磁材料，铁氧体属于功能材料中的磁性材料大类，目前永磁铁氧体材料应用较为广泛的有钡铁氧体和锶铁氧体两种。
器件厂将铁氧体永磁材料制备成瓦形器件，然后电机厂将瓦型器件粘贴在金属壳体上，与转子一起组装成各式电机。
铁氧体永磁材料质量决定了后续器件产品的制备难易，现有铁氧体永磁材料存在料浆脱水难，压制成型难、粘模等问题，导致器件成品率低，这推高了制备成本，压缩了器件利润空间。
发明内容
本发明的目的是提供一种永磁铁氧体材料的制备方法，主要解决现有永磁铁氧体材料在成型时料浆脱水困难、成型难度大、容易发生粘模的技术问题。
本发明采用的技术方案是，一种永磁铁氧体材料的制备方法，包括以下步骤：
1)湿法混料，以水为湿磨分散介质，将主原料和一次添加剂同时加入球磨机中，进行1～10小时的湿磨混料，获得湿磨料浆，湿磨料浆烘干后粉体粒度为0.7～1.5μm，所述主原料的组分及比例为：氧化铁粉84-88wt％，碳酸锶为11-15wt％，主原料中Fe2O3和SrCO3的摩尔比为6.2—6.5，氧化铁粉中Fe2O3的重量百分含量≥98％，碳酸锶中SrCO3的重量百分含量≥97％，所述一次添加剂为工业纯二氧化硅，一次添加剂以主原料重量计的添加比例为CaCO30-0.5wt％，SiO20.1-0.4wt％；
2)一次预烧，将经湿磨混料得到的料浆在空气中进行预烧，温度为1150～1350℃，保温1～5小时，获得一次预烧料；
3)粗粉碎，将一次预烧料利用球磨机粉碎后进行粒级筛分获得粒度为1～10μm预烧料粗粉；
4)检测预烧料粗粉的pH值，当预烧料粗粉的pH值>9或pH值<7，则重复步骤1)—3)；当预烧料粗粉的pH值为7—9时，转入步骤5)；
5)湿磨制浆，在粗粉碎得到的粗粉中添加二次添加剂后用球磨机进行细磨，以水为分散介质，获得细磨料浆，细磨料浆烘干后粉体粒度为0.2～1.0μm，比表面积为1～12m2/g，所述的二次添加剂以粗粉重量计的添加比例为：CaCO30.05-1.5wt％，SiO20-0.25wt％，Al2O30-3.0wt％；
6)湿压磁场成型，将细磨得到的细磨料浆浓缩为含水为25～50wt％的成型料浆，在外加磁场为3～30kOe、成型压力为19.6～78.4Mpa的条件下压制成生坯；
7)二次烧结，将成型所得生坯在空气中进行烧结，温度为1150～1250℃，保温2～6小时，获得熟坯；
8)熟坯打磨，采用自动磨床将熟坯进行打磨后获得样品。
进一步；步骤4)中，检测预烧料粗粉的pH值，包括，取100g预烧料粗粉试样置于容积为500mL的烧杯中，向烧杯内加入200mL蒸馏水并混匀预烧料粗粉，将烧杯内预烧料粗粉溶液煮沸，烧杯内的液位下降至175mL时，用pH试纸热测烧杯内上层清液的pH值。
本发明备的永磁铁氧体材料为M型六角晶系铁氧体，基本分子组成可以表示为：SrO·χFe2O3，式中χ为摩尔比。
本发明方法通过控制主原料中Fe2O3和SrCO3的摩尔比为6.2—6.5以及预烧料粗粉的pH值为7—9，制得剩余磁感应强度Br为420±10mT，矫顽力Hcb为266±12kA/m，内禀矫顽力Hcj≥305kA/m的高性能永磁铁氧体材料。
本发明相比现有技术具有如下积极效果：本发明方法通过控制主原料中Fe2O3和SrCO3的摩尔比为6.2—6.5和预烧料粗粉的pH值为7—9，减少了杂相的产生，降低了料浆黏度，解决了料浆脱水困难、成型难度大、粘模的难题；制得剩余磁感应强度Br为420±10mT，矫顽力Hcb为266±12kA/m，内禀矫顽力Hcj≥305kA/m的高性能永磁铁氧体材料，降低了永磁铁氧体材料的制备成本。
具体实施方式
下面结合具体实施方式，进一步阐明本发明，应理解下述具体实施方式仅用于说明本发明而不用于限制本发明的范围。
实施例1，一种永磁铁氧体材料的制备方法，包括以下步骤：
1)湿式混料，以水为湿磨分散介质，将主原料和一次添加剂同时加入球磨机中，进行2.5小时的湿磨混料，获得湿磨料浆，湿磨料浆烘干后粉体粒度为0.7～1.5μm，所述主原料的组分及比例为：氧化铁粉86.6wt％，碳酸锶为13.4wt％，主原料中Fe2O3和SrCO3的摩尔比为6.25，氧化铁粉中Fe2O3含量为99wt％，碳酸锶中SrCO3含量为97.5wt％，所述一次添加剂为工业纯二氧化硅，一次添加剂以主原料重量计的添加比例为CaCO30.35wt％，SiO20.1wt％；
2)一次预烧，将经湿磨混料得到的料浆在空气中进行预烧，温度为1250℃，保温2小时，获得一次预烧料；
3)粗粉碎，将一次预烧料利用球磨机粉碎后进行粒级筛分获得粒度为2.5μm预烧料粗粉；取100g料粉，加入200mL蒸馏水，煮沸，在液位下降至175mL时，使用pH试纸热测烧杯内上层清液的pH值，控制pH值为7～9；
4)检测预烧料粗粉的pH值，取100g预烧料粗粉试样置于容积为500mL的烧杯中，向烧杯内加入200mL蒸馏水并混匀预烧料粗粉，将烧杯内预烧料粗粉溶液煮沸，烧杯内的液位下降至175mL时，用pH试纸热测烧杯内上层清液的pH值为8，转入步骤5)；
5)湿磨制浆，在粗粉碎得到的粗粉中添加二次添加剂后用球磨机进行细磨，以水为分散介质，获得细磨料浆，细磨料浆烘干后粉体粒度为0.65μm，比表面积为1～12m2/g，所述的二次添加剂以粗粉重量计的添加比例为：CaCO30.65wt％，SiO20.15wt％；
6)湿压磁场成型，将细磨得到的细磨料浆浓缩为含水为40wt％的成型料浆，在外加磁场为15kOe、成型压力为34.3Mpa的条件下压制成尺寸为Φ28.5×15mm的圆柱形生坯；
7)二次烧结，将成型所得生坯在空气中进行烧结，温度为1250℃，保温2.5小时，获得熟坯；
8)熟坯打磨，采用自动磨床将熟坯进行打磨后获得样品。
除上述实施例外，本发明还可以有其他实施方式。凡采用等同替换或等效变换形成的技术方案，均落在本发明要求的保护范围。
Claims (2)
1.一种永磁铁氧体材料的制备方法，其特征是，所述的方法包括以下步骤：
1)湿法混料，以水为湿磨分散介质，将主原料和一次添加剂同时加入球磨机中，进行1～10小时的湿磨混料，获得湿磨料浆，湿磨料浆烘干后粉体粒度为0.7～1.5μm，所述主原料的组分及比例为：氧化铁粉84-88wt％，碳酸锶为11-15wt％，主原料中Fe2O3和SrCO3的摩尔比为6.2—6.5，氧化铁粉中Fe2O3的重量百分含量≥98％，碳酸锶中SrCO3的重量百分含量≥97％，所述一次添加剂为工业纯二氧化硅，一次添加剂以主原料重量计的添加比例为CaCO30-0.5wt％，SiO20.1-0.4wt％；
2)一次预烧，将经湿磨混料得到的料浆在空气中进行预烧，温度为1150～1350℃，保温1～5小时，获得一次预烧料；
3)粗粉碎，将一次预烧料利用球磨机粉碎后进行粒级筛分获得粒度为1～10μm预烧料粗粉；
4)检测预烧料粗粉的pH值，当预烧料粗粉的pH值>9或pH值<7，则重复步骤1)—3)；当预烧料粗粉的pH值为7—9时，转入步骤5)；
5)湿磨制浆，在粗粉碎得到的粗粉中添加二次添加剂后用球磨机进行细磨，以水为分散介质，获得细磨料浆，细磨料浆烘干后粉体粒度为0.2～1.0μm，比表面积为1～12m2/g，所述的二次添加剂以粗粉重量计的添加比例为：CaCO30.05-1.5wt％，SiO20-0.25wt％，Al2O30-3.0wt％；
6)湿压磁场成型，将细磨得到的细磨料浆浓缩为含水为25～50wt％的成型料浆，在外加磁场为3～30kOe、成型压力为19.6～78.4Mpa的条件下压制成生坯；
7)二次烧结，将成型所得生坯在空气中进行烧结，温度为1150～1250℃，保温2～6小时，获得熟坯；
8)熟坯打磨，采用自动磨床将熟坯进行打磨后获得样品。
2.如权利要求1所述的一种永磁铁氧体材料的制备方法，其特征是，步骤4)中，检测预烧料粗粉的pH值，包括，取100g预烧料粗粉试样置于容积为500mL的烧杯中，向烧杯内加入200mL蒸馏水并混匀预烧料粗粉，将烧杯内预烧料粗粉溶液煮沸，烧杯内的液位下降至175mL时，用pH试纸热测烧杯内上层清液的pH值。
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| CN112321294A (zh) * | 2020-11-04 | 2021-02-05 | 重庆凌达磁材科技有限公司 | 一种铁氧体永磁材料及其制备方法 |
| CN112694337A (zh) * | 2020-12-09 | 2021-04-23 | 南京梅宝新型建材有限公司 | 一种永磁铁氧体材料料浆可成型特性控制方法 |
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