CN113929445B - 一种永磁铁氧体预烧料的制备方法 - Google Patents

一种永磁铁氧体预烧料的制备方法 Download PDF

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CN113929445B
CN113929445B CN202111123603.7A CN202111123603A CN113929445B CN 113929445 B CN113929445 B CN 113929445B CN 202111123603 A CN202111123603 A CN 202111123603A CN 113929445 B CN113929445 B CN 113929445B
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丁伯明
胡良权
叶华
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Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

本发明涉及永磁铁氧体制造领域，为了克服现有预烧料的制备方法离子交换率低、对预烧料性能提升不足，提供一种永磁铁氧体预烧料的制备方法。通过预压增大混合原料间的接触面积，提升离子交换率，提高离子分散均匀性，再控制预烧的温度和氧气浓度，最优化条件下进行预烧，提升预烧料的性能，为后续制得性能优良的永磁铁氧体打下基础。

Description

一种永磁铁氧体预烧料的制备方法
技术领域
本发明涉及永磁铁氧体制造领域，尤其是一种永磁铁氧体预烧料的制备方法。
背景技术
预烧是氧化物法生产永磁铁氧体的重要工序之一，对产品的质量起到重要的作用，预烧的目的是将混合料在一定温度下保温数小时，使混合料颗粒间产生初步的固相反应，生成部分铁氧体。其作用主要体现在降低化学活性的不均匀性、降低烧结产品的收缩率、提高产品的烧结密度和易于成型等方面。气氛以及气氛和温度的相互匹配是预烧的关键，总的来说，需要氧化气氛，在烘干、排出水分初步氧化分解、预烧、以及无机盐的分解和亚铁的氧化阶段都需要在氧化气氛中完成。
中国专利公开号CN 106747390B，公开了一种锶铁氧体预烧料及其制备方法，其特征在于，包括以下步骤：a、按摩尔比Fe2O3﹕SrO＝6.2～6.3﹕1进行计算，称取原料铁鳞和碳酸锶，加入高岭土，混合均匀后加水球磨2.5～3.5h，得到混合浆料，高岭土的添加量为铁鳞和碳酸锶总量的0.25～0.3％；b、将步骤a中的混合浆料烘干，于电炉中进行预烧；c、预烧结束后，将预烧产物破碎至60目筛以下，加入碳酸钙和硼酸，球磨14～18h，过滤，碳酸钙和硼酸加入量分别预烧产物总量的0.5～0.7％和0.15～0.25％；d、将步骤c中过滤得到的固体物质进行烧结，制得锶铁氧体预烧料。其不足之处在于，混合浆料未经处理直接预烧，固相-固相之间接触面积有限，离子交换率低，且该方法对预烧料的性能提升效果有限，后续制得的永磁铁氧体磁学性能较差。
发明内容
本发明是为了克服现有预烧料的制备方法离子交换率低、对预烧料性能提升不足，制得永磁铁氧体磁学性能较差的不足，公开一种离子交换率高、预烧料性能提升大，制得的永磁铁氧体磁学性能优良的一种永磁铁氧体预烧料的制备方法。
为了实现上述发明目的，本发明采用的技术方案如下：
一种永磁铁氧体预烧料的制备方法，永磁铁氧体预烧料具有CayLaxSr1-x-yFe2n- zCozO19主相，其中0.3≤x≤0.6、0.1≤y≤0.5、0.2≤z≤0.4、5.1≤n≤5.6，永磁铁氧体预烧料的制备方法包括以下步骤：
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3，混合后加入助熔剂进行球磨，烘干得混合粉料；
B.对步骤A所得混合粉料进行预压、有氧预烧得预烧料。
原料中各氧化物和碳酸盐经球磨混合均匀后烘干，在经预压后，减少了原料颗粒间空隙，增大原料间的接触面积，有利于固相反应的发生，有利于离子的交换，在得到的预烧料体系中，离子分布也就更均匀，再经有氧预烧，控制预烧过程中的升温和含氧量，最大化提升预烧料的性能。
进一步的，步骤A中，助熔剂为SiO2。
进一步的，步骤A中，助熔剂的添加量为Fe2O3、CaCO3、La2O3、CoCO3、SrCO3总质量的0.1％～0.2％。
进一步的，步骤A中，球磨方法为湿法球磨，球磨时间为4～8小时，球磨后的平均粒度为0.5～1μm。
进一步的，步骤B中，预压压力为5～10MPa。
进一步的，步骤B中，有氧预烧温度为1180～1230℃。
进一步的，步骤B中，有氧预烧的氧气浓度为22％～25％。
进一步的，步骤B中，有氧预烧的时间为2～4小时。
由于采用以上的技术方案，本发明具有这样的有益效果：通过预压和控制有氧预烧的条件，提升了原料间的离子交换，均匀了预烧料中的离子分布，并提升了预烧料的性能，为后续制备性能优良的永磁铁氧体提供基础。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
总实施例
一种永磁铁氧体预烧料的制备方法，永磁铁氧体预烧料具有CayLaxSr1-x-yFe2n- zCozO19主相，其中0.3≤x≤0.6、0.1≤y≤0.5、0.2≤z≤0.4、5.1≤n≤5.6，永磁铁氧体预烧料的制备方法包括以下步骤：
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3，混合后加入混合物重量0.1％～0.2％的SiO2进行湿法球磨，球磨4～8小时后，球磨后的平均粒度为0.5～1μm，烘干得混合粉料；
B.对步骤A所得粉料在5～10MPa下进行预压，于管式炉中1180～1230℃预烧2～4小时，控制管式炉中氧气含量在22～25％之间，得预烧料。
实施例中使用的原料规格如下：Fe2O3纯度≥99.3wt％，Cl-≤0.1wt％，颗粒的原始平均粒度≤1.5μm；CaCO3纯度≥98.5wt％，颗粒的原始平均粒度≤1.0μm；La2O3纯度≥99.2wt％，颗粒的原始平均粒度≤5μm；氧化钴Co含量≥72.2％，颗粒的原始平均粒度≤3μm；SrCO3纯度≥97.2wt％，颗粒的原始平均粒度≤1.5μm。
实施例1
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料在8MPa下进行预压成圆饼状，于管式炉中升温预烧，在温度达到1200℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在23％，煅烧3小时后，停止充氧，停止加热，冷却得预烧料。
实施例2
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.2％的SiO2进行湿法球磨，球磨8小时后，烘干得平均粒度0.5μm的混合粉料；
B.对步骤A所得混合粉料在5MPa下进行预压成圆饼状，于管式炉中升温预烧，在温度达到1180℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在22％，煅烧4小时后，停止充氧，停止加热，冷却得预烧料。
实施例3
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨4小时后，烘干得平均粒度1μm的混合粉料；
B.对步骤A所得混合粉料在10MPa下进行预压成圆饼状，于管式炉中升温预烧，在温度达到1230℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在25％，煅烧2小时后，停止充氧，停止加热，冷却得预烧料。
对比例1
对比例1相较于实施例1，未对混合粉料进行预压；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1200℃后停止升温，开始持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在23％，煅烧3小时后，停止充氧，停止加热，冷却得预烧料。
对比例2
对比例2相较于实施例1，在温度达到1200℃后持续充空气煅烧；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1200℃后停止升温，开始持续充空气煅烧3小时后，停止充空气，停止加热，冷却得预烧料。
对比例3
对比例3相较于实施例1，有氧预烧过程中氧气含量稳定在30％；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1200℃后停止升温，持续充氧气，检测氧气分压，使管式炉中氧气含量保持稳定在30％，煅烧3小时后，停止充氧，停止加热，冷却得预烧料。
对比例4
对比例4相较于实施例1，在1250℃进行有氧预烧；
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3混合，混合后加入混合物中质量0.1％的SiO2进行湿法球磨，球磨6小时后，烘干得平均粒度0.8μm的混合粉料；
B.对步骤A所得混合粉料于管式炉中升温预烧，在温度达到1250℃后停止升温，开始充氧气，检测氧气分压，使管式炉中氧气含量保持在23％，煅烧3小时后停止加热，停止充氧气，冷却得预烧料。
称取实施例1～3及对比例1～4的预烧料各500g，分别添加2.5gSiO2、7.2gCaCO3，5g葡萄糖酸钙混合物投入到球磨机，再添加750mL去离子水作为球磨介质研磨30小时至料浆平均粒度为0.60μm。
湿法粉碎之后，对成型用料浆进行离心脱水，各个料浆的浓度调整为68％，然后在5MPa下成型，在压制的同时，在压制方向施加15000Oe的成型磁场。得到成型体直径为45mm、高度为10mm的圆柱体。
在400℃下对成型体进行热处理，彻底去除水分，然后在空气中进行烧结，升温速度为150℃/小时，在1190℃保温60分钟，获得烧结体。对各个烧结体的上下表面研磨，测量其剩余磁感应强度(Br)、矫顽力(Hcb)、内禀矫顽力(Hcj)、最大磁能积(BH)max，结果如下表所示。
编号 Br(Gs) Hcb(Oe) Hcj(Oe) (BH)max(MGOe) 矫顽力温度系数
实施例1 4560 4230 5440 4.997 0.12
实施例2 4573 4238 5560 5.001 0.12
实施例3 4523 5128 5249 4.687 0.13
对比例1 4490 4029 4850 4.654 0.26
对比例2 4520 4060 4960 4.885 0.2
对比例3 4450 4145 5021 4.747 0.18
对比例4 4390 4179 4941 4.702 0.16
可见，由实施例1～3的预烧料制得的永磁铁氧体，具有明显优于对比例1～4的磁学特性，由对比例1可见，预压过程对提高预烧料性能有着极大提升，且矫顽力系数有明显下降；由对比例2、对比例3可见，过低及过高的氧浓度预烧，都不利于固相反应的进行，对最终烧结体的磁学特性也会产生影响；由对比例4可见，有氧预烧的温度过高，也会导致最终烧结体性能下降。

Claims (6)

1.一种永磁铁氧体预烧料的制备方法，所述永磁铁氧体预烧料具有CayLaxSr1-x-yFe2n- zCozO19主相，其中0.3≤x≤0.6、0.1≤y≤0.5、0.2≤z≤0.4、5.1≤n≤5.6，其特征在于，所述永磁铁氧体预烧料的制备方法包括以下步骤：
A.按配比称取Fe2O3、CaCO3、La2O3、CoCO3、SrCO3，混合后加入助熔剂进行球磨，烘干得混合粉料；
B.对步骤A所得混合粉料进行预压、有氧预烧得预烧料；
所述步骤B中，有氧预烧的氧气浓度为22%~25%；
所述步骤B中，有氧预烧温度为1180~1230℃。
2.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤A中，助熔剂为SiO2。
3.根据权利要求1或2所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤A中，助熔剂的添加量为Fe2O3、CaCO3、La2O3、CoCO3、SrCO3总质量的0.1%~0.2%。
4.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤A中，球磨方法为湿法球磨，球磨时间为4~8小时，球磨后的平均粒度为0.5~1μm。
5.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤B中，预压压力为5~10MPa。
6.根据权利要求1所述的一种永磁铁氧体预烧料的制备方法，其特征在于，所述步骤B中，有氧预烧的时间为2~4小时。
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06151153A (ja) * 1992-11-06 1994-05-31 Nippon Steel Corp マンガン−亜鉛フェライト用仮焼粉およびその製造方法
CN102190501A (zh) * 2010-03-08 2011-09-21 无锡斯贝尔磁性材料有限公司 一种MnZn铁氧体粉料的预烧工艺
CN111004027A (zh) * 2019-12-09 2020-04-14 天长市华磁磁电有限公司 一种高磁导率软磁铁氧体及其制备方法
CN111362687A (zh) * 2019-12-17 2020-07-03 横店集团东磁股份有限公司 一种永磁铁氧体及其制备方法
WO2021057051A1 (zh) * 2019-09-25 2021-04-01 横店集团东磁股份有限公司 一种永磁材料及其制备方法
CN113185275A (zh) * 2021-04-23 2021-07-30 麦格磁电科技（珠海）有限公司 云计算用超高Bs低损耗锰锌铁氧体材料的制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102473499A (zh) * 2009-07-08 2012-05-23 Tdk株式会社 铁氧体磁性材料
CN103030388A (zh) * 2013-01-17 2013-04-10 北矿磁材科技股份有限公司 一种高性能永磁铁氧体材料及制造方法
CN105399411B (zh) * 2015-12-01 2019-01-25 横店集团东磁股份有限公司 一种锰锌铁氧体低温烧结工艺
CN110372365A (zh) * 2019-07-16 2019-10-25 横店集团东磁股份有限公司 一种永磁铁氧体材料的制备方法
CN111943658B (zh) * 2020-06-30 2022-06-03 天通控股股份有限公司 一种宽温低损耗MnZn铁氧体材料及其制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06151153A (ja) * 1992-11-06 1994-05-31 Nippon Steel Corp マンガン−亜鉛フェライト用仮焼粉およびその製造方法
CN102190501A (zh) * 2010-03-08 2011-09-21 无锡斯贝尔磁性材料有限公司 一种MnZn铁氧体粉料的预烧工艺
WO2021057051A1 (zh) * 2019-09-25 2021-04-01 横店集团东磁股份有限公司 一种永磁材料及其制备方法
CN111004027A (zh) * 2019-12-09 2020-04-14 天长市华磁磁电有限公司 一种高磁导率软磁铁氧体及其制备方法
CN111362687A (zh) * 2019-12-17 2020-07-03 横店集团东磁股份有限公司 一种永磁铁氧体及其制备方法
CN113185275A (zh) * 2021-04-23 2021-07-30 麦格磁电科技（珠海）有限公司 云计算用超高Bs低损耗锰锌铁氧体材料的制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
永磁铁氧体元件机械强度分析;王自敏;《机械强度》;第38卷(第04期);第729-733页 *

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