CN108298972B - 一种软磁铁氧体片材的制备方法 - Google Patents

一种软磁铁氧体片材的制备方法 Download PDF

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CN108298972B
CN108298972B CN201810156938.0A CN201810156938A CN108298972B CN 108298972 B CN108298972 B CN 108298972B CN 201810156938 A CN201810156938 A CN 201810156938A CN 108298972 B CN108298972 B CN 108298972B
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顾正青
汤会香
计建荣
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Suzhou Shihua New Material Polytron Technologies Inc
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Abstract

一种软磁铁氧体片材的制备方法，包含粉末制备、浆料制备、流延成型和烧结步骤，在烧结前将含有铝盐或锆盐的醇水混合液喷涂于待烧结生料片的表面。通过上述方式，本发明能够实现多层铁氧体片材的共烧，而不会产生粘粘，良品率达到90%及以上，降低了生产成本。

Description

一种软磁铁氧体片材的制备方法
技术领域
本发明公开了一种软磁铁氧体的制备方法，特别涉及软磁铁氧体片材在烧结步骤前的一种预处理的方法。
背景技术
智能手机在使用的锂电池技术已经几十年了，电池低容量和智能手机高耗能之间的矛盾越来越突出，而无线充电是解决这个矛盾的方法之一。目前，无线充电主要有三种方式，磁感应技术，磁共振技术和无线电波射频技术，而商业化应用的主要是磁感应技术。
利用磁感应技术进行充电的无线充电器在发射端和接收端各有一个线圈，发射端线圈连接有线电源产生电磁信号，接收端线圈感应发射端的电磁信号从而产生电流给电池充电。在发射端线圈上贴上铁氧体隔磁片一方面可以提高单位面积内的磁通量，从而提高磁场强度；在接收端线圈上添加铁氧体隔磁片可减小或者消除充电时电磁场对手机的不良影响，尤其是手机电池。当发射端线圈发射出来的磁场通过电池时，电池里面的金属就会产生感应电流，通常叫做涡流。此涡流会产生一个与发射线圈的磁场方向相反的磁场，抵消掉发射线圈的磁场，使得接收端线圈收到的感应电压下降，并且该涡流会转变成热量，使手机非常热。因此，在手机端（接收端）的线圈上需要放置高磁导率的铁氧体片材作为隔磁片，降低能量损失，提高充电效率，并且降低发热量。
铁氧体片材的制作工艺是：混料-球磨-预烧-配置浆料-流延成型-切片-烧结。在烧结过程中，为了提高生产效率，一般会多层叠放。同种材料在高温下会发生固相反应，因此会发生粘粘。现有技术中采用的方法有，在铁氧体生料片上刷一层氧化铝或者氧化锆粉，但是氧化铝/氧化锆会发生团聚，很容易形成小颗粒，会导致烧成后的铁氧体片产生变形，凸点，裂纹等缺陷，并且由于铁氧体片材非常薄脆，不容易去除。以上缺陷都会使铁氧体片材的外观不合格，烧结的良率一般在70%左右。
发明内容
鉴于以上所述现有技术的缺点，本发明目的在于提供一种软磁铁氧体片材的制备方法，尤其是烧结工艺，用于提高铁氧体片的生产良率，降低生产成本。
软磁铁氧体片材制造工艺一般包括以下步骤：混料-球磨-预烧-配置浆料-流延成型-切片-烧结。为了实现上述目的，本发明提供如下技术方案。
将用于制备铁氧体的原材料（CuO，Fe2O3，ZnO，NiO/Mn3O4）按比例混合，各组分含量如下：对于MnZn铁氧体来说，CuO：0～12wt%，Fe2O3：65～75wt%，ZnO：5~10wt%，Mn3O4：15～25%；对于NiZn铁氧体来说，CuO：0～10wt%，Fe2O3：67～72wt%，ZnO：18~23wt%，NiO：5～10wt%。
所述的球磨工艺可以采用干法球磨或者是湿法球磨，干法球磨的设备是振动球磨机，物料和球的重量比控制在1:1～3:1范围内。湿法球磨可以采用卧式球磨机或者立式行星式球磨机，物料和球的重量比控制在1:1～4:1范围内。
所述的预烧工艺是为了控制原料的反应活性，因此反应温度控制在800~900℃之间。
所述的配置浆料工艺是通过将铁氧体粉末与粘结剂、增塑剂、溶剂和分散剂混合来形成铁氧体浆料。此步工艺可使用球磨机或者砂磨机。一般是先将铁氧体粉末，溶剂和分散剂混合，充分分散后，再添加增塑剂和粘结剂等其他微量添加剂，这样可以获得均匀的铁氧体浆料。为了防止在涂布和干燥过程中出现裂纹或者是孔洞，需将所得浆料在真空容器中充分脱泡后，进行下一道工艺。
所述的流延成型工艺是通过使用流延法将铁氧体浆料涂覆在PET硅胶离型膜或者图案化的离型膜上，并且需要在60～80℃温度范围内使铁氧体浆料干燥来获得铁氧体生料片，铁氧体生料片的厚度控制为60-400μm。
所述的烧结工艺是首先把PET硅胶离型膜或者图案化的离型膜剥离，然后将MnZn/MnCuZn生料片在1200～1380℃下烧结2～10个小时，NiZn/NiCuZn生料片在900～1000℃下烧结1～4个小时。为了提高产能，通常是多层叠烧。
本发明通过在生料片表面喷涂一层铝盐或锆盐的醇水混合液后再进行高温烧结，实现了多层共烧。
所述的醇水混合液为乙二醇、乙醇、丙三醇中的至少一种与水的混合液，醇与水的比例为1:3～3:1。
所述的铝盐为氯化铝、硝酸铝、硫酸铝中的任意一种，醇水混合液中铝盐的浓度为0.10～0.46 mol/L。
所述的锆盐为二氯氧化锆或硝酸氧锆中的任意一种，醇水混合液中锆盐的浓度为0.15～0.50 mol/L。
通过上述本发明提供一种软磁铁氧体片材的制备方法，实现多层铁氧体片材的共烧，而不会产生粘粘，良品率达到90%及以上，降低了生产成本。
具体实施例
下面将结合具体实施例对本发明的技术方案进行清楚、完整地解释。显然，所描述的实施例仅是本发明的一部分优选实施例，而不是全部的实施例。
实施例1。
铁氧体粉末的制备：制备具有以下成分的MnZn铁氧体粉末：Fe2O3：72wt%，ZnO：8wt%，Mn3O4：20wt%，粉末的颗粒直径分布在0.4~3μm。
铁氧体浆料的制备：使用球磨机把上述铁氧体粉末，乙醇和分散剂按照重量比：70:29:1球磨10个小时，得到产物A浆料；向A浆料中添加铁氧体粉末重量的7wt%的粘结剂，4wt%的增塑剂和其他添加剂2wt%，继续球磨2～5小时。真空脱泡30min～60min后待用。
在流延机上以1～5m/min的线速度在PET硅胶保护膜或者是图案化的离型膜上进行涂布，干燥温度在60℃～80℃之间。生料片的厚度控制在150±5μm。
涂布完成后，在生料片上喷涂一层二氯氧化锆的醇水混合液，醇与水的比例为：1:1.8~2:5，其中二氯氧化锆在混合液中的浓度为0.32mol/L，喷涂线速度为5～10m/min，干燥温度为110℃。按照140mmx140mm的尺寸切成片状，把离型膜剥离，放置于氧化铝板上，叠放层数为10层。
在1280℃下烧结4个小时，随炉冷却后取出，10层片子不会发生粘粘，不会有凸点，翘曲等不良外观，良品率为92%。切成圆环测试磁导率，在100KHz的初始磁导率实部μ’ 为510~640。
实施例2。
铁氧体粉末的制备：制备具有以下成分的MnCuZn铁氧体粉末：CuO：7wt%，Fe2O3：68wt%，ZnO：5wt%，Mn3O4：20wt%，粉末的颗粒直径分布在0.4~3μm。
铁氧体浆料的制备：使用球磨机把上述铁氧体粉末，乙醇和分散剂按照重量比：70:29:1球磨10个小时，得到产物B浆料；向B浆料中添加铁氧体粉末重量的12wt%的粘结剂，5wt%的增塑剂和其他添加剂2wt%，继续球磨2～5小时。真空脱泡30min～60min后待用。
在流延机上以1～5m/min的线速度在PET硅胶保护膜或者是图案化的离型膜上进行涂布，干燥温度在60℃～80℃之间。生料片的厚度控制在150±5μm。
涂布完成后，在生料片上喷涂一层硝酸氧锆的醇水混合液，醇与水的比例为：1:2.5~3:5，其中硝酸氧锆在混合液中的浓度为0.32mol/L，喷涂线速度为5～10m/min，干燥温度为110℃。按照140mmx140mm的尺寸切成片状，把离型膜剥离，放置于氧化铝板上，叠放层数为15层。
在1350℃下烧结7个小时，随炉冷却后取出，15层片子不会发生粘粘，不会有凸点，翘曲等不良外观，良品率为90%。切成圆环测试磁导率，在100KHz的初始磁导率实部μ’为520~660。
实施例3。
铁氧体粉末的制备：制备具有以下成分的NiZn铁氧体粉末：Fe2O3：70wt%，ZnO：22wt%，NiO：8wt%，粉末的颗粒直径分布在0.4~3μm。
铁氧体浆料的制备：使用球磨机把上述铁氧体粉末，乙醇和分散剂按照重量比：70:29:1球磨10个小时，得到产物C浆料；向C浆料中添加铁氧体粉末重量的9wt%的粘结剂，4wt%的增塑剂和其他添加剂3wt%，继续球磨2～5小时。真空脱泡30min～60min后待用。
在流延机上以1～5m/min的线速度在PET硅胶保护膜或者是图案化的离型膜上进行涂布，干燥温度在60℃～80℃之间。生料片的厚度控制在150±5μm。
涂布完成后，在生料片上喷涂一层氯化铝的醇水混合液，醇与水的比例为：1:2.5~1:1，其中氯化铝在混合液中的浓度为0.28mol/L，喷涂线速度为3～6m/min，干燥温度为110℃。按照140mmx140mm的尺寸切成片状，把离型膜剥离，放置于氧化铝板上，叠放层数为9层。
在1000℃下烧结3个小时，随炉冷却后取出，9层片子不会发生粘粘，不会有凸点，翘曲等不良外观，良品率为94%。切成圆环测试磁导率，在100KHz的初始磁导率实部μ’为750~880。
实施例4。
铁氧体粉末的制备：制备具有以下成分的NiCuZn铁氧体粉末：CuO：6wt%，Fe2O3：70wt%，ZnO：18wt%，NiO：6wt%，粉末的颗粒直径分布在0.4~3μm。
铁氧体浆料的制备：使用球磨机把上述铁氧体粉末，乙醇和分散剂按照重量比：70:29:1球磨10个小时，得到产物D浆料；向D浆料中添加铁氧体粉末重量的5wt%的粘结剂，4wt%的增塑剂和其他添加剂3wt%，继续球磨2～5小时。真空脱泡30min～60min后待用。
在流延机上以1～5m/min的线速度在PET硅胶保护膜或者是图案化的离型膜上进行涂布，干燥温度在60℃～80℃之间。生料片的厚度控制在150±5μm。
涂布完成后，在生料片上喷涂一层硝酸铝的醇水混合液，醇与水的比例为：1:2~2:1，其中硝酸铝在混合液中的浓度为0.33mol/L，喷涂线速度为3～6m/min，干燥温度为110℃。按照140mmx140mm的尺寸切成片状，把离型膜剥离，放置于氧化铝板上，叠放层数为12层。
在1000℃下烧结3个小时，随炉冷却后取出，12层片子不会发生粘粘，不会有凸点，翘曲等不良外观，良品率为90%。切成圆环测试磁导率，在100KHz的初始磁导率实部μ’为740~850。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效方法或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (5)

1.一种无线充电用软磁铁氧体片材的制备方法，包含混料、球磨、预烧、配置浆料、流延成型、切片和烧结，其特征在于：在烧结前将含有铝盐或锆盐的醇水混合液喷涂于待烧结生料片的表面；所述的醇水混合液为乙二醇、乙醇、丙三醇中的至少一种与水的混合液，醇与水的比例为1:3~3:1；
所述铁氧体为镍-锌铁氧体、镍-铜-锌铁氧体、锰-锌铁氧体或锰-铜-锌铁氧体中的任意一种；
所述待烧结生料片厚度为60~400μm。
2.根据权利要求1所述的一种无线充电用软磁铁氧体片材的制备方法，其特征在于：
所述镍-铜-锌铁氧体中组份含量为：CuO：0～10wt%，Fe2O3：67～72wt%，ZnO：18~23wt%，NiO：5～10wt%；
烧结温度为900~1000℃，烧结时间为1~4小时。
3.根据权利要求1所述的一种无线充电用软磁铁氧体片材的制备方法，其特征在于：
所述锰-铜-锌铁氧体中组份含量为：CuO：0～12wt%，Fe2O3：65～75wt%，ZnO：5~10wt%，Mn3O4：15～25%；
烧结温度为1200~1380℃，烧结时间为2~10小时。
4.根据权利要求1所述的一种无线充电用软磁铁氧体片材的制备方法，其特征在于：所述的铝盐为氯化铝，硝酸铝，硫酸铝中的任意一种，醇水混合液中铝盐的浓度为0.10～0.46mol/L。
5.根据权利要求1所述的一种无线充电用软磁铁氧体片材的制备方法，其特征在于：所述的锆盐为二氯氧化锆或硝酸氧锆中的任意一种，醇水混合液中锆盐的浓度为0.15～0.50mol/L。
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