CN109574646B - 一种适用于6.78MHz的铁氧体片及其制备方法 - Google Patents

一种适用于6.78MHz的铁氧体片及其制备方法 Download PDF

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CN109574646B
CN109574646B CN201811539444.7A CN201811539444A CN109574646B CN 109574646 B CN109574646 B CN 109574646B CN 201811539444 A CN201811539444 A CN 201811539444A CN 109574646 B CN109574646 B CN 109574646B
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顾正青
韩朝庆
计建荣
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Suzhou Shinuo New Material Technology Co ltd
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Abstract

本发明公开了一种适用于6.78MHz的铁氧体片及其制备方法。其主要步骤为：1）预烧，将氧化铁、氧化镍、氧化铜、氧化锌球磨混合、烘干、预烧得到预烧粉；2）制浆，将预烧粉、有机溶剂、掺杂剂、粘结剂，增塑剂加入球磨机并搅拌均匀，经过筛网过滤，除泡，制备得均匀弥散的浆料；3）流延；4）烧结。本发明的优点是利用成本低的混合稀土氧化物矿掺杂工艺，在不使用贵金属钴的前提下，可以使镍铜锌铁氧体在6.78MHz获得高的磁导率，有利于无线充电效率和距离的提升。

Description

一种适用于6.78MHz的铁氧体片及其制备方法
技术领域
本发明涉及一种适用于6.78MHz的铁氧体片及其制备方法，属于电子元器件新材料新工艺领域。
背景技术
随着消费电子产业的快速发展，电子产品更新换代逐渐加快，功能越来越强大，同时耗电量也越来越大。在机载储能电池的容量无法明显提升的情况下，传统的有线充电方式的弊端逐渐显露出来，例如容易损坏，携带不便，有触电危险等。另外，每一个电子产品都具有不同规格的有线充电器，对用户造成了相当大的不便，并且还会造成资源浪费和环境污染。
无线充电相比传统充电方式具有更省电，更智能且电满自动断电的功能，并能识别不同设备对能量的要求。因此，无线充电具有广阔的发展前景。无线充电时，需要在发射端线圈和接收端线圈上加入铁氧体材料作为隔磁片，可以提高线圈之间的耦合系数，进而提高传输效率，并且可以屏蔽线圈干扰，屏蔽充电磁场对终端设备的干扰，提高无线充电设备的整体性能。
目前主流的无线充电用铁氧体隔磁片主要是适用于无线充电联盟的Qi标准，强调铁氧体材料在100-200KHz之间的性能。现有技术公布了一种适用于Qi标准的低频铁氧体隔磁片。但是在此频率下进行无线充电，充电底座和接收端设备之间的距离必须要小于1cm，否则充电效率会大大降低。一个有效的解决办法就是提高无线充电的频率，充电频率越高，充电底座和接收端设备之间可允许的距离就能更远，从而使得无线充电更加方便便捷，这也是无线充电发展的趋势。
发明内容
本发明的目的是针对上述无线充电高频化的技术趋势，提供一种适用于6.78MHz的铁氧体片及其制备方法。本发明提供的铁氧体片在频率为 6.78MHz时，其磁导率实部大于250，磁导率虚部小于20。
为了达到上述目的，本发明是这样实现的。
一种适用于6.78MHz的铁氧体片，它的化学成分有由主成分和掺杂剂组成，主成分为按照摩尔百分数为48.5-49.5%氧化铁、4-6%氧化铜、15-20%氧化锌，余量为氧化镍，掺杂剂为氧化钛和混合稀土氧化物矿，质量百分数分别为主成分的0.01-1%和0.01-5%。
所述铁氧体片的制备方法如下。
预烧：将氧化铁、氧化镍、氧化铜、氧化锌按照配比放入球磨机，加入去离子水球磨0.5-3小时后烘干，进行煅烧，煅烧温度为600-980度，煅烧时间为0.5-5小时得到预烧粉。
制浆：将预烧粉加入有机溶剂、掺杂剂、增塑剂、粘结剂，在球磨机中球磨5~30h，筛网过滤，真空脱泡，得到弥散浆料。
流延：将弥散浆料注入流延机中，刮刀的高度为0.05-2mm，控制流延机速度为0.1-2cm/s，流延时采用PET膜作为衬底，得到流延片。
烧结：将流延片从衬底剥离后，置于氧化铝或者氧化锆板上进行空气烧结；在300-400度之间保温0.1-2h进行脱胶处理，然后在900-1100度之间保温0.5-5h，完成烧结过程。
作为本技术方案的优选方案，所述的有机溶剂为乙醇、甲乙酮、丁酮、丙酮、二甲苯的一种或者几种，质量分数为浆料的20~60%。
作为本技术方案的优选方案，所述的掺杂剂为氧化钛和混合稀土氧化物矿，质量分别为所加入的预烧粉的0.01-1%和0.01-5%，混合稀土氧化物矿为含有La、Ce、Pr、Nd、Sm氧化物的矿物混合物，各组分之间比例不固定，杂质含量小于2%。
作为本技术方案的优选方案，所述的弥散浆料中的粘结剂为环氧树脂、酚醛树脂、聚乙烯醇或聚乙烯醇缩丁醛中的一种，质量为所加入的预烧粉的0.1-5%。
作为本技术方案的优选方案，所述的弥散浆料中的增塑剂为甘油、邻苯二甲酸二辛酯或邻苯二甲酸二丁酯一种，质量为所加入的预烧粉的0.1-6%。
本发明与现有技术相比，本技术方案具有如下优点。
（1）利用成本很低的混合稀土氧化物矿掺杂工艺，在不使用贵金属钴的前提下，能够提高铁氧体片的使用频率，并且其中的Nd、Sm氧化物由于其原子半径大，不会进入铁氧体晶格，在高温下可以细化晶粒，有利于降低铁氧体的高频损耗。
（2）稀土氧化物具有超疏水性，可以防止粉料的团聚，避免使用分散剂。
（3）制备得到的铁氧体片在频率为 6.78MHz时，其磁导率实部大于250，磁导率虚部小于20，使得无线充电的距离和效率都大大提高。
（4）混合稀土属于国家稀土行业过剩材料，其中的La、Ce、Pr、Nd、Sm氧化物分离十分困难，成本很高，在确保杂质含量小于2%的前提下，直接用混合稀土氧化物矿来掺杂铁氧体，有助于促进国家的稀土平衡利用。
具体实施方式
下面结合具体实例对本发明做进一步说明，但本发明并不仅仅局限于以下实施例。
实施例1。
将氧化铁、氧化铜、氧化锌、氧化镍按照摩尔百分数：48.5%氧化铁、6%氧化铜、15%氧化锌、30.5%氧化镍来配料。将配好的料放入球磨机，加入去离子水球磨3小时后烘干，进行煅烧，煅烧温度为880度，煅烧时间为1.5小时得到预烧粉。
将预烧粉加入有机溶剂、掺杂剂、增塑剂、粘结剂，在球磨机中球磨10h，筛网过滤，真空脱泡，得到弥散浆料。有机溶剂为乙醇，质量分数为浆料的50%。掺杂剂为氧化钛和混合稀土氧化物矿，质量分别为所加入的预烧粉的0.05%和0.05%。混合稀土氧化物矿为含有La、Ce、Pr、Nd、Sm氧化物矿，各组分之间比例不固定，杂质含量小于2%。粘结剂为环氧树脂，质量为所加入的预烧粉的4%。增塑剂为邻苯二甲酸二丁酯，质量为所加入的预烧粉的1%。
将弥散浆料注入流延机中，刮刀的高度为0.15mm，控制流延机速度为1cm/s，流延时采用PET膜作为衬底，得到流延片。
将流延片从衬底剥离后，置于氧化铝进行空气烧结。在300度保温0.5h进行脱胶处理，然后在1080度之间保温3h，完成烧结过程。
制备出的样品组织致密，孔隙率低，表面平整，密度为4.95g/cm3。将样品进行磁性能测试，在频率为 6.78MHz时，其磁导率实部为260，磁导率虚部为5。
实施例2。
将氧化铁、氧化铜、氧化锌、氧化镍按照摩尔百分数：49.5%氧化铁、4%氧化铜、20%氧化锌、26.5%氧化镍来配料。将配好的料放入球磨机，加入去离子水球磨2小时后烘干，进行煅烧，煅烧温度为890度，煅烧时间为1.5小时得到预烧粉。
将预烧粉加入有机溶剂、掺杂剂、增塑剂、粘结剂，在球磨机中球磨8h，筛网过滤，真空脱泡，得到弥散浆料。有机溶剂为乙醇，质量分数为浆料的55%。掺杂剂为氧化钛和混合稀土氧化物矿，质量分别为所加入的预烧粉的0.5%和1%。混合稀土氧化物矿为含有La、Ce、Pr、Nd、Sm氧化物矿，各组分之间比例不固定，杂质含量小于2%。粘结剂为聚乙烯醇缩丁醛，质量为所加入的预烧粉的3%。增塑剂为邻苯二甲酸二辛酯，质量为所加入的预烧粉的1.8%。
将弥散浆料注入流延机中，刮刀的高度为0.2mm，控制流延机速度为1cm/s，流延时采用PET膜作为衬底，得到流延片。
将流延片从衬底剥离后，置于氧化铝进行空气烧结。在350度保温1h进行脱胶处理，然后在1060度之间保温4h，完成烧结过程。
制备出的样品组织致密，孔隙率低，表面平整，密度为4.90g/cm3。将样品进行磁性能测试，在频率为 6.78MHz时，其磁导率实部为255，磁导率虚部为8。
实施例3。
将氧化铁、氧化铜、氧化锌、氧化镍按照摩尔百分数：49%氧化铁、5%氧化铜、18%氧化锌、28%氧化镍来配料。将配好的料放入球磨机，加入去离子水球磨2.5小时后烘干，进行煅烧，煅烧温度为850度，煅烧时间为3小时得到预烧粉。
将预烧粉加入有机溶剂、掺杂剂、增塑剂、粘结剂，在球磨机中球磨5h，筛网过滤，真空脱泡，得到弥散浆料。有机溶剂为乙醇，质量分数为浆料的60%。掺杂剂为氧化钛和混合稀土氧化物矿，质量分别为所加入的预烧粉的0.35%和0.5%。混合稀土氧化物矿为含有La、Ce、Pr、Nd、Sm氧化物矿，各组分之间比例不固定，杂质含量小于2%。粘结剂为聚乙烯醇缩丁醛，质量为所加入的预烧粉的2.3%。增塑剂为邻苯二甲酸二丁酯，质量为所加入的预烧粉的1.2%。
将弥散浆料注入流延机中，刮刀的高度为0.14mm，控制流延机速度为1.2cm/s，流延时采用PET膜作为衬底，得到流延片。
将流延片从衬底剥离后，置于氧化铝进行空气烧结。在380度保温1.5h进行脱胶处理，然后在1040度之间保温3h，完成烧结过程。
制备出的样品组织致密，孔隙率低，表面平整，密度为4.92g/cm3。将样品进行磁性能测试，在频率为 6.78MHz时，其磁导率实部为250，磁导率虚部为9。

Claims (5)

1.一种适用于6.78MHz的铁氧体片，其特征在于：它的化学成分由主成分和掺杂剂组成，主成分为按照摩尔百分数为48.5-49.5%氧化铁、4-6%氧化铜、15-20%氧化锌，余量为氧化镍，掺杂剂为氧化钛和混合稀土氧化物矿，质量百分数分别为主成分的0.01-1%和0.01-5%；
所述混合稀土氧化物矿为含有La、Ce、Pr、Nd、Sm氧化物矿，各组分之间比例不固定，杂质含量小于2%；
所述适用于6.78MHz的铁氧体片在频率 6.78MHz时，其磁导率实部大于250，磁导率虚部小于20。
2.一种如权利要求1所述的适用于6.78MHz的铁氧体片的制备方法，其特征在于包括如下步骤：
S1预烧：将氧化铁、氧化镍、氧化铜、氧化锌按照配比放入球磨机，加入去离子水球磨0.5-3小时后烘干，进行煅烧，煅烧温度为600-980度，煅烧时间为0.5-5小时得到预烧粉；
S2制浆：将预烧粉加入有机溶剂、掺杂剂、增塑剂、粘结剂，无需使用分散剂，在球磨机中球磨5~30h，筛网过滤，真空脱泡，得到弥散浆料；
S3流延：将弥散浆料注入流延机中，刮刀的高度为0.05-2mm，控制流延机速度为0.1-2cm/s，流延时采用PET膜作为衬底，得到流延片；
S4烧结：将流延片从衬底剥离后，置于氧化铝或者氧化锆板上进行空气烧结；在300-400度之间保温0.1-2h进行脱胶处理，然后在900-1100度之间保温0.5-5h，完成烧结过程。
3.根据权利要求2所述的一种适用于6.78MHz的铁氧体片的制备方法，其特征在于：所述有机溶剂为乙醇、甲乙酮、丁酮、丙酮、二甲苯中的至少一种，质量分数为浆料的20-60%。
4.根据权利要求2所述的一种适用于6.78MHz的铁氧体片的制备方法，其特征在于：所述粘结剂为环氧树脂、酚醛树脂、聚乙烯醇或聚乙烯醇缩丁醛中的一种，质量为预烧粉的0.1-5%。
5.根据权利要求2所述的一种适用于6.78MHz的铁氧体片的制备方法，其特征在于：所述增塑剂为甘油、邻苯二甲酸二辛酯或邻苯二甲酸二丁酯一种，质量为预烧粉的0.1-6%。
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