CN108298971A - 一种磁铁氧体的制备方法 - Google Patents

一种磁铁氧体的制备方法 Download PDF

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CN108298971A
CN108298971A CN201810119851.6A CN201810119851A CN108298971A CN 108298971 A CN108298971 A CN 108298971A CN 201810119851 A CN201810119851 A CN 201810119851A CN 108298971 A CN108298971 A CN 108298971A
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年四虎
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Chuzhou Boruite Industry & Trade Co Ltd
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Abstract

本发明公开了一种磁铁氧体的制备方法，包括以下步骤，配料：按如下重量份数的原料进行配料：钡铁氧体料粉：200份，氯化聚乙烯CPE：28.9‑29.6份、硬脂酸：0.2‑0.5、二辛酯：0.1‑0.15份、石蜡：0.2‑0.3份、工业大豆油：0.7份、铁红：11‑14份、轻质氧化镁：100‑110份；经过混料、造球预烧结、粉碎、成型、烧结、冷却处理：烧结后进行冷却，冷却分为两个阶段：第一阶段：以510℃/h的冷却速度将烧结后的成型体冷却到925℃，第二阶段，在110000e‑130000e磁场作用下成型，得到永磁铁氧体生坯，接着通过自然冷却将成型体冷却至室温，即得到磁铁氧体。应用本发明实施例，提高生产出来体贴的应用范围。

Description

一种磁铁氧体的制备方法
技术领域
本发明涉及磁铁氧体制备技术领域，特别涉及一种磁铁氧体的制备方法。
背景技术
永磁材料是电子行业中不可或缺的材料，广泛应用于家电、汽车、计算机、通讯、医疗、航天、军事等领域。近年来，永磁铁氧体磁性材料以其原料来源广、价格低廉和优异的磁性能在磁性材料的研究与发展中占有重要地位，具有相对较高的剩磁(Br)、矫顽力(jHc)及磁能积(BH)max。工业上永磁铁氧体以铁红或铁鳞与碳酸锶、碳酸钡或者碳酸钙等为主要原料通过传统陶瓷工艺制备，理论上Fe2O3与MCO3(M为Ba、Sr或Ca等元素)的摩尔比为6，但实际操作中，为了使反应更加完全，往往提高MCO3的配比，使Fe2O3与MCO3的摩尔比在5-6之间。
添加剂的选择对永磁铁氧体性能起重要作用，生产中通常加入适量H3BO3、SiO2等改善永磁铁氧体性能。其中，SiO2的作用是细化晶粒，提高永磁铁氧体矫顽力，但SiO2的量并非越多越好，过量掺杂会在反应中生成MSiO3相，严重破坏永磁铁氧体性能，因此生产中，SiO2的添加量一般控制在0.3w％左右。但有些廉价原料中往往Si含量很高，严重影响了永磁铁氧体的磁性能。
发明内容
本发明所要解决的技术问题是提供一种磁铁氧体的制备方法，旨在提高生产出来的磁铁的应用范围。
为实现上述目的，本发明提供以下的技术方案：
一种磁铁氧体的制备方法，包括以下步骤，
(1)配料：按如下重量份数的原料进行配料：钡铁氧体料粉：200份，氯化聚乙烯CPE：28.9-29.6份、硬脂酸：0.2-0.5、二辛酯：0.1-0.15份、石蜡：0.2-0.3份、工业大豆油：0.7份、铁红：11-14份、轻质氧化镁：100-110份；
(2)混料：在真空条件下将配料投入到行星球磨机进行超细球磨，球磨20-25小时，使得原料粉末的粒度小于2μm；然后对原料粉末进行烘干处理；
(3)造球预烧结：将烘干处理后的原料粉末在空气中进行预烧结，预烧结温度为1000-12000℃，保温时间为1-2小时，得到预烧结球团；
(4)粉碎：对预烧结球团进行干式球磨粉碎至平均粒度4-6μm，得到预烧结粗粉；在真空环境下用滚磨机来进行二次球磨，球磨转速为350r/min，球磨时间为12-14小时；
(5)成型：将球磨后所得的料浆采用离心方式进行脱水处理，调整至料浆浓度在70-85wt％，然后进行磁场成型，成型压力为1吨/cm2，采用5万安匝的直流磁场，叠加7.2万安匝的脉冲磁场；压制成型后的毛坯直径为200mm，长度为50mm的圆饼；
(6)烧结：将上述成型体先在200℃的温度进行热处理，除去水分，然后在空气中进行烧结，其中升温速度是140℃/小时，烧结温度为1150℃，保温时间为2.5小时，获得烧结体；
(7)冷却处理：烧结后进行冷却，冷却分为两个阶段：第一阶段：以510℃/h的冷却速度将烧结后的成型体冷却到925℃，
第二阶段，在110000e-130000e磁场作用下成型，得到永磁铁氧体生坯，接着通过自然冷却将成型体冷却至室温，即得到磁铁氧体。
作为上述方案的进一步优化，在对预烧结球团进行干式球磨粉碎至平均粒度4-6μm之前，加入碳酸钙、氧化硅。
作为上述方案的进一步优化，所述磁铁氧体的规格为：2㎜×8.8㎜，或2.2*9.2。
作为上述方案的进一步优化，所述配料中还包括：铁的氧化物和锶盐混合而成的氧化铁组合物与锶铁氧体，氧化铁组合物的重量为混合物总重量的5％。
本发明提供的一种磁铁氧体的制备方法，具有如下有益效果：
1、本发明的一种磁铁氧体的制备方法，通过配料：按如下重量份数的原料进行配料：钡铁氧体料粉：200份，氯化聚乙烯CPE：28.9-29.6份、硬脂酸：0.2-0.5、二辛酯：0.1-0.15份、石蜡：0.2-0.3份、工业大豆油：0.7份、铁红：11-14份、轻质氧化镁：100-110份，经过混料、造球预烧结、粉碎、成型、烧结、冷却处理：烧结后进行冷却后形成的磁铁，可以应用于冰箱、冰柜的磁铁应用领域。
2、本发明的一种磁铁氧体的制备方法制备的磁条，适用规格尺寸2㎜×8.8㎜、吸力60-70g、硬度小于等于96A、延伸率小于等于24％。
具体实施方式
为使发明的目的、技术方案和优点更加清楚明了，下面通过实施例，对本发明技术方案进行进一步详细说明。但是应该理解，此处所描述的具体实施例仅仅用以解释本发明技术方案，并不用于限制本发明技术方案的范围。
实施例1
一种磁铁氧体的制备方法，包括以下步骤，
(1)配料：按如下重量份数的原料进行配料：钡铁氧体料粉：200份，氯化聚乙烯CPE：29.6份、硬脂酸：0.2份、二辛酯：0.15份、石蜡：0.2份、工业大豆油：0.7份、铁红：14份、轻质氧化镁：110份，铁的氧化物和锶盐混合而成的氧化铁组合物与锶铁氧体，氧化铁组合物的重量为混合物总重量的5％；
(2)混料：在真空条件下将配料投入到行星球磨机进行超细球磨，球磨20小时，使得原料粉末的粒度小于2μm；然后对原料粉末进行烘干处理；
(3)造球预烧结：将烘干处理后的原料粉末在空气中进行预烧结，预烧结温度为1000℃，保温时间为1小时，得到预烧结球团；
(4)粉碎：对预烧结球团进行干式球磨粉碎至平均粒度4μm，得到预烧结粗粉；在真空环境下用滚磨机来进行二次球磨，球磨转速为350r/min，球磨时间为12小时，在对预烧结球团进行干式球磨粉碎至平均粒度4μm之前，加入碳酸钙、氧化硅；
(5)成型：将球磨后所得的料浆采用离心方式进行脱水处理，调整至料浆浓度在70-85wt％，然后进行磁场成型，成型压力为1吨/cm2，采用5万安匝的直流磁场，叠加7.2万安匝的脉冲磁场；压制成型后的毛坯直径为200mm，长度为50mm的圆饼；
(6)烧结：将上述成型体先在200℃的温度进行热处理，除去水分，然后在空气中进行烧结，其中升温速度是140℃/小时，烧结温度为1150℃，保温时间为2.5小时，获得烧结体；
(7)冷却处理：烧结后进行冷却，冷却分为两个阶段：第一阶段：以510℃/h的冷却速度将烧结后的成型体冷却到925℃，
第二阶段，在110000e磁场作用下成型，得到永磁铁氧体生坯，接着通过自然冷却将成型体冷却至室温，即得到磁铁氧体，所述磁铁氧体的规格为：2㎜×8.8㎜。
实施例2
(1)配料：按如下重量份数的原料进行配料：钡铁氧体料粉：200份，氯化聚乙烯CPE：28.9份、硬脂酸：0.5、二辛酯：0.1份、石蜡：0.3份、工业大豆油：0.7份、铁红：11份、轻质氧化镁：100份，配料中还包括：铁的氧化物和锶盐混合而成的氧化铁组合物与锶铁氧体，氧化铁组合物的重量为混合物总重量的5％；
(2)混料：在真空条件下将配料投入到行星球磨机进行超细球磨，球磨20-25小时，使得原料粉末的粒度小于2μm；然后对原料粉末进行烘干处理；
(3)造球预烧结：将烘干处理后的原料粉末在空气中进行预烧结，预烧结温度为12000℃，保温时间为2小时，得到预烧结球团；
(4)粉碎：对预烧结球团进行干式球磨粉碎至平均粒度6μm，得到预烧结粗粉；在真空环境下用滚磨机来进行二次球磨，球磨转速为350r/min，球磨时间为14小时，在对预烧结球团进行干式球磨粉碎至平均粒度6μm之前，加入碳酸钙、氧化硅；
(5)成型：将球磨后所得的料浆采用离心方式进行脱水处理，调整至料浆浓度在70-85wt％，然后进行磁场成型，成型压力为1吨/cm2，采用5万安匝的直流磁场，叠加7.2万安匝的脉冲磁场；压制成型后的毛坯直径为200mm，长度为50mm的圆饼；
(6)烧结：将上述成型体先在200℃的温度进行热处理，除去水分，然后在空气中进行烧结，其中升温速度是140℃/小时，烧结温度为1150℃，保温时间为2.5小时，获得烧结体；
(7)冷却处理：烧结后进行冷却，冷却分为两个阶段：第一阶段：以510℃/h的冷却速度将烧结后的成型体冷却到925℃，
第二阶段，在130000e磁场作用下成型，得到永磁铁氧体生坯，接着通过自然冷却将成型体冷却至室温，即得到磁铁氧体；所述磁铁氧体的规格为：2.2*9.2。
表1
实施例1 规格尺寸 吸力 硬度 延伸率
效果 2㎜×8.8㎜ 50-60g ≤96A ≤24％
实施例2 规格尺寸 吸力 硬度 延伸率
效果 2.2㎜×9.2㎜ 60-72g ≤96A ≤24％
应用本发明实施例，本发明的一种磁铁氧体的制备方法，能够通过配料：按如下重量份数的原料进行配料：钡铁氧体料粉：200份，氯化聚乙烯CPE：28.9-29.6份、硬脂酸：0.2-0.5、二辛酯：0.1-0.15份、石蜡：0.2-0.3份、工业大豆油：0.7份、铁红：11-14份、轻质氧化镁：100-110份，经过混料、造球预烧结、粉碎、成型、烧结、冷却处理：烧结后进行冷却后形成的磁铁，可以应用于冰箱、冰柜的磁铁应用领域。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。

Claims (4)

1.一种磁铁氧体的制备方法，其特征在于，包括以下步骤，
(1)配料：按如下重量份数的原料进行配料：钡铁氧体料粉：200份，氯化聚乙烯CPE：28.9-29.6份、硬脂酸：0.2-0.5、二辛酯：0.1-0.15份、石蜡：0.2-0.3份、工业大豆油：0.7份、铁红：11-14份、轻质氧化镁：100-110份；
(2)混料：在真空条件下将配料投入到行星球磨机进行超细球磨，球磨20-25小时，使得原料粉末的粒度小于2μm；然后对原料粉末进行烘干处理；
(3)造球预烧结：将烘干处理后的原料粉末在空气中进行预烧结，预烧结温度为1000-12000℃，保温时间为1-2小时，得到预烧结球团；
(4)粉碎：对预烧结球团进行干式球磨粉碎至平均粒度4-6μm，得到预烧结粗粉；在真空环境下用滚磨机来进行二次球磨，球磨转速为350r/min，球磨时间为12-14小时；
(5)成型：将球磨后所得的料浆采用离心方式进行脱水处理，调整至料浆浓度在70-85wt％，然后进行磁场成型，成型压力为1吨/cm2，采用5万安匝的直流磁场，叠加7.2万安匝的脉冲磁场；压制成型后的毛坯直径为200mm，长度为50mm的圆饼；
(6)烧结：将上述成型体先在200℃的温度进行热处理，除去水分，然后在空气中进行烧结，其中升温速度是140℃/小时，烧结温度为1150℃，保温时间为2.5小时，获得烧结体；
(7)冷却处理：烧结后进行冷却，冷却分为两个阶段：第一阶段：以510℃/h的冷却速度将烧结后的成型体冷却到925℃，
第二阶段，在110000e-130000e磁场作用下成型，得到永磁铁氧体生坯，接着通过自然冷却将成型体冷却至室温，即得到磁铁氧体。
2.根据权利要求1所述的磁铁氧体的制备方法，其特征在于，在对预烧结球团进行干式球磨粉碎至平均粒度4-6μm之前，加入碳酸钙、氧化硅。
3.根据权利要求1所述的磁铁氧体的制备方法，其特征在于，所述磁铁氧体的规格为：2㎜×8.8㎜，或2.2*9.2。
4.根据权利要求1所述的磁铁氧体的制备方法，其特征在于，所述配料中还包括：铁的氧化物和锶盐混合而成的氧化铁组合物与锶铁氧体，氧化铁组合物的重量为混合物总重量的5％。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112876230A (zh) * 2021-03-02 2021-06-01 苏州工业园区凯艺精密科技有限公司 一种适用于5g环形器的铁氧体材料及其制备方法

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