CN109111220A - 一种高松装密度镁锌软磁铁氧体粉料制备方法 - Google Patents

一种高松装密度镁锌软磁铁氧体粉料制备方法 Download PDF

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CN109111220A
CN109111220A CN201711445357.0A CN201711445357A CN109111220A CN 109111220 A CN109111220 A CN 109111220A CN 201711445357 A CN201711445357 A CN 201711445357A CN 109111220 A CN109111220 A CN 109111220A
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廖晓舟
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ZHAOQING CHAMPION FERRITE TECHNOLOGY Co Ltd
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Abstract

一种高松装密度镁锌软磁铁氧体粉料制备方法，所得未经预烧的镁锌铁氧体喷雾干燥颗粒具有高的松装密度特点，可有效提高后道成型、烧结的产品质量。采用重质氧化镁为原料，并加入适当的镍锌铁氧体、锰锌铁氧体或镁锌铁氧体废磁芯粉末，采用高铝陶瓷内衬球磨机研磨，加入磁性材料专用分散剂、消泡剂，得到高固含量、流动性好的料浆，喷雾干燥造粒而成。

Description

一种高松装密度镁锌软磁铁氧体粉料制备方法
技术领域
本发明涉及一种高松装密度镁锌软磁铁氧体粉料制备方法，尤其是一种采用重质氧化镁为原料，并加入适当的镍锌铁氧体、锰锌铁氧体或镁锌铁氧体废磁芯粉末，采用高铝陶瓷内衬球磨机研磨，加入磁性材料专用分散剂、消泡剂，制得高固含量，流动性好的料浆，经过喷雾干燥造粒得到不经过预烧的具有高松装密度的镁锌软磁铁氧体粉料，属于新材料技术领域。
背景技术
软磁铁氧体具有高导磁率、高电阻率、低损耗等特点，同时还具有陶瓷的坚硬性，因而被广泛用于计算机、通信设备、消费电子产品等，起功率传输、抗电磁干扰、电磁振荡等作用。目前，软磁铁氧体中应用最多的是锰锌铁氧体和镍锌铁氧体。锰锌铁氧体适合在低频段使用，其烧结时需要气氛保护的缺点；镍锌铁氧体更加适合高频段使用，高频损耗小，同时烧结时不需要气氛保护。然而， 镍锌铁氧体需要使用昂贵的氧化镍为原料，生产成本高。由于镁锌铁氧体不含镍元素，研究采用镁锌铁氧体替代镍锌铁氧体的技术成果越来越多，镁锌铁氧体性能大幅提高，并且部分镁锌铁氧体采用不经过预烧的一次烧结工艺制备，已经能取代常规镍锌铁氧体。但未经预烧的镁锌铁氧体粉料制备过程中，容易出现料浆变稠，颗粒松装密度难以提高的工艺难点，过低的松装密度，成型装料高度增加，容易造成单重高度变化和压力增大，导致卡模和模具损耗增加，更不利于生坯成型密度的提高，对烧结后磁芯机械强度不利。因此解决未经预烧的镁锌铁氧体材料松装密度才能解决其在实际应用在的不足，提高后道成型、烧结的产品质量。
现有镁锌软磁铁氧体粉料制备主要以轻质氧化镁为原料，采用砂磨工艺研磨，由于轻质氧化镁质地轻浮，在研磨时料浆容易出现气泡，并且变稠，导致料浆流动性下降，因此无法减少水添加量，固含量无法提高，在进行喷雾干燥造粒得到的颗粒料，其松装密度一般低于1.2g/cm3，如果要提高其松装密度，大多采用预烧工艺，通过提高预烧温度，实现材料松装密度的提高。本发明一种高松装密度镁锌软磁铁氧体粉料制备方法，材料不经过预烧，而是从原材料选取，研磨工艺以及辅助添加剂等方面进行创新，采用该方法喷雾干燥造粒得到的颗粒料，可以与预烧工艺的颗粒料相媲美，适合高速旋转压制高精度成型，同时烧结时磁芯没有变形现象。
发明内容
本发明的目的在于针对用现有镁锌软磁铁氧体，在不经过预烧工艺，制备得到的颗粒料松装密度低的不足，提供一种采用重质氧化镁为原料，并加入适当的镍锌、锰锌或镁锌铁氧体废磁芯粉末，采用高铝陶瓷内衬球磨机研磨，加入磁性材料专用分散剂、消泡剂，喷雾干燥造粒制备得具有高松装密度的镁锌软磁铁氧体粉料制备方法。
本发明的技术方案为：一种高松装密度镁锌软磁铁氧体粉料制备方法。本发明采用重质氧化镁为原料，相对于轻质氧化镁，重质氧化镁质地重，能明显改善料浆流动，不容易产生气泡，料浆不容易变稠，同时适当加入的镍锌、锰锌或镁锌铁氧体废磁芯粉末，也能明显改善料浆的流动性。采用这两种方法配制的没经过预烧的镁锌铁氧体料浆具有极佳的流动性，可以减少水加入量，提高料浆固含量，从而提高喷雾造粒颗粒松装密度。
由于重质氧化镁活性比轻质氧化镁低，磁体烧结外观不光亮，本发明采用高铝陶瓷内衬球磨机，进行材料研磨，由于是刚性坚硬内衬，磨球碰撞产生的摩擦效果远远优于软性聚氨酯内衬球磨机，可以实现重质氧化镁和废磁芯粉末的充分研磨细化，高铝陶瓷内衬中的氧化铝研磨损耗极少，将与配方中加入的二氧化硅反应形成硅酸铝，存在磁体晶界，可以提高磁体强度，且不影响材料性能。同时采用高铝陶瓷内衬球磨机研磨，可以少于搅拌砂磨工艺的水添加量的情况下，物料和研磨介质在球磨机转动过程中依然能实现翻滚碰撞，从而提高料浆固含量，提高喷雾干燥颗粒松装密度。
针对镁锌铁氧体研磨过程中容易变粘稠和气泡产生，与厂家合作研发出铁氧体料浆专用助剂，包括非氨水型铁氧体研磨专用分散剂A及铁氧体料浆专用消泡剂B。该分散剂不同于常用的氨水型分散剂，没有刺激气味，其分散效果更佳持久，提高料浆流动性更佳，分别在研磨开始和结束时加入，研磨开始时加入分散剂A可以大幅度减少水添加量，防止料浆团聚，提高研磨效率，在研磨结束前再加入该铁氧体研磨专用分散剂A，其作用是进一步提高料浆流动性，获得极佳的固含量，固含量提高到70%以上。在研磨结束添加铁氧体料浆专用消泡剂B，与常用的正辛醇消泡剂或含硅类消泡剂相比，专用的消泡剂用量小，消泡效果明显，可以拟制泡沫产生，料浆更佳沉实，并且流动性更佳。两种添加剂的配合使用，进一步提高了料浆流动性和固含量，可以明显提高颗粒松装密度。
制备得到的料浆，在离心喷雾干燥塔进行喷雾干燥造粒，进口温度控制在300~400℃，出口温度控制在90~130℃，雾化盘转速在10000~12000转/分钟，取其中60~220目之间的颗粒，得到松装密度将在1.3~1.6镁锌铁氧体颗粒料。
一种高松装密度镁锌软磁铁氧体粉料制备方法，包括采用重质氧化镁为原料，并加入适当的镍锌铁氧体、锰锌铁氧体或镁锌铁氧体废磁芯粉末，其添加量重量百分比可以在5~90%，采用高铝陶瓷内衬球磨机研磨，钢球或锆球为磨介，按料：水：球=1:0.3~0.4:2~3的比例进行投料。配料研磨同时添加0.2~0.6%磁性材料专用分散剂A，球磨8~16小时后，加入15~20%浓度为8%的1799聚乙烯醇溶液、0.3~1%磁性材料料浆专用分散剂A和0.01~0.3%铁氧体料浆专用消泡剂B，球磨30分钟，得到待喷雾干燥造粒的铁氧体浆料，然后在离心喷雾干燥塔进行喷雾干燥造粒，进口温度控制在300~400℃，出口温度控制在90~130℃，雾化盘转速在10000~12000转/分钟，取其中60~200目之间的颗粒，得到一种具有高松装密度的镁锌软磁铁氧体粉料。以下是工艺指标参数：
浆料固含量：60%~70%
浆料粘度为：<300（mPa.s，25℃）
浆料平均粒度：1.0-1.3μm。
喷雾干燥造粒后取60目-200目之间的颗粒。
本发明的有益效果为：本发明使用重质氧化镁为原料，并加入适当的镍锌铁氧体、锰锌铁氧体或镁锌铁氧体废磁芯粉末，采用高铝陶瓷内衬球磨机研磨，改善研磨效果，提高了上述材料的活性，同时加入磁性材料专用分散剂、消泡剂，制得固含量高，流动性好的料浆，喷雾干燥造粒制备得具有高松装密度的镁锌软磁铁氧体粉料，解决了镁锌铁氧体松装密度低，不利于提高生坯成型密度和烧结磁体强度的缺点，扩大了镁锌铁氧体的应用领域。
具体实施方式
具体实施例一，称取重质氧化镁9.7 Kg，氧化铁66.8Kg，氧化锌21.5 Kg，氧化铜2Kg，镍锌废磁芯过200目粉末10Kg，配制成镁锌铁氧体110 Kg，加水40 Kg ，磁性材料专用分散剂A 0.3 Kg ，上述材料采用200Kg高铝陶瓷内衬球磨机（研磨介质钢球200 Kg），球磨8小时，然后加入浓度为8%的1799PVA溶液20 Kg，磁性材料专用分散剂A 0.4 Kg，铁氧体料浆专用消泡剂B 0.06 Kg，球磨30分钟，得到流动性好、固含量高的待喷雾干燥造粒浆料，然后在离心喷雾干燥塔进行喷雾干燥造粒，进口温度控制在330℃，出口温度控制在110℃，雾化盘转速在11000转/分钟，取其中60~200目之间的颗粒，得到一种松装密度约为1.4g/cm3，磁导率500左右的镁锌软磁铁氧体粉料。
具体实施例二，称取重质氧化镁8 Kg，氧化铁67.5Kg，氧化锌21.5 Kg，氧化铜3Kg，镁锌废磁芯200目粉末20Kg，配制成镁锌铁氧体120 Kg，加水40 Kg ，磁性材料专用分散剂A 0.3 Kg ，上述材料采用200Kg高铝陶瓷内衬球磨机（研磨介质钢球200 Kg），球磨8小时，然后加入浓度为8%的1799PVA溶液20 Kg，磁性材料专用分散剂A 0.5 Kg，铁氧体料浆专用消泡剂B 0.06 Kg，球磨30分钟得到流动性好、固含量高的待喷雾干燥造粒浆料，然后在离心喷雾干燥塔进行喷雾干燥造粒，进口温度控制在350℃，出口温度控制在100℃，雾化盘转速在11000转/分钟，取其中60~200目之间的颗粒，得到一种松装密度约为1.5g/cm3，磁导率800左右的镁锌软磁铁氧体粉料。
具体实施例三，称取重质氧化镁9 Kg，氧化铁12Kg，氧化锌10 Kg，氧化铜5 Kg，锰锌废磁芯200目粉末64Kg，配制成镁锌铁氧体100 Kg，加水30 Kg ，磁性材料专用分散剂A0.4 Kg ，上述材料采用300Kg高铝陶瓷内衬球磨机（研磨介质钢球400 Kg），球磨10小时，然后加入浓度为8%的1799PVA溶液20 Kg，磁性材料专用分散剂A 0.3 Kg，铁氧体料浆专用消泡剂B 0.04Kg，球磨40分钟得到流动性好、固含量高的待喷雾干燥造粒浆料，然后在离心喷雾干燥塔进行喷雾干燥造粒，进口温度控制在330℃，出口温度控制在110℃，雾化盘转速在11000转/分钟，取其中60~200目之间的颗粒，得到一种松装密度约为1.55g/cm3，磁导率600左右的镁锌软磁铁氧体粉料。

Claims (4)

1.一种高松装密度镁锌软磁铁氧体粉料制备方法，其特征在于：采用重质氧化镁为原料，并加入适当的镍锌铁氧体、锰锌铁氧体或镁锌铁氧体废磁芯粉末，采用高铝陶瓷内衬球磨机研磨，加入磁性材料专用分散剂、消泡剂，得到高固含量、流动性好料浆，喷雾干燥造粒而成。
2.如权利要求1所述的一种高松装密度镁锌软磁铁氧体粉料制备方法，其特征在于采用重质氧化镁为原料，并加入适当的镍锌铁氧体、锰锌铁氧体或镁锌铁氧体废磁芯粉末，其添加量重量百分比可以在5~90%。
3.如权利要求1所述的一种高松装密度镁锌软磁铁氧体粉料制备方法，其特征在于采用高铝陶瓷内衬球磨机研磨，浆料平均粒度1.0-1.3μm。
4.如权利要求1所述的一种高松装密度镁锌软磁铁氧体粉料制备方法，其特征在于采用磁性材料料浆专用分散剂A和铁氧体料浆专用消泡剂B为助剂，得到的铁氧体浆料，喷雾干燥造粒而成。
CN201711445357.0A 2017-12-27 2017-12-27 一种高松装密度镁锌软磁铁氧体粉料制备方法 Pending CN109111220A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111943659A (zh) * 2020-07-06 2020-11-17 南昌大学 一种高频低损耗高电阻率镍锌铁氧体材料的制备工艺
CN113860865A (zh) * 2021-11-04 2021-12-31 无锡斯贝尔磁性材料有限公司 MnZn铁氧体粉料颗粒的制粉线工艺管控方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111943659A (zh) * 2020-07-06 2020-11-17 南昌大学 一种高频低损耗高电阻率镍锌铁氧体材料的制备工艺
CN113860865A (zh) * 2021-11-04 2021-12-31 无锡斯贝尔磁性材料有限公司 MnZn铁氧体粉料颗粒的制粉线工艺管控方法

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