CN104446408B - 一种吸波材料及其制备方法 - Google Patents

一种吸波材料及其制备方法 Download PDF

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CN104446408B
CN104446408B CN201310441214.8A CN201310441214A CN104446408B CN 104446408 B CN104446408 B CN 104446408B CN 201310441214 A CN201310441214 A CN 201310441214A CN 104446408 B CN104446408 B CN 104446408B
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content
absorbing material
preparation
ceo
powder
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CN104446408A (zh
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刘厚胤
孔宪君
陈大军
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BYD Co Ltd
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BYD Co Ltd
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Priority to CN201310441214.8A priority Critical patent/CN104446408B/zh
Priority to EP14850054.9A priority patent/EP3027578B1/en
Priority to JP2016516860A priority patent/JP6267788B2/ja
Priority to KR1020167009803A priority patent/KR101813821B1/ko
Priority to PCT/CN2014/085053 priority patent/WO2015043347A1/en
Publication of CN104446408A publication Critical patent/CN104446408A/zh
Priority to US15/064,504 priority patent/US10308555B2/en
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Abstract

本发明提供了一种吸波材料，该吸波材料包括主成分、辅助成分及烧结助剂；所述主成分为Fe2O3、MnO、ZnO和MgO，所述辅助成分为CeO2和P2O5；所述CeO2和P2O5摩尔比为1‑2：1。本发明的吸波材料不仅具有很高的初始磁导率，而且具有很高的电阻率。

Description

一种吸波材料及其制备方法
技术领域
本发明属于磁性材料制备领域领域，尤其涉及一种天线用吸波材料及其制备方法。
背景技术
电磁感应式无线充电系统中的接收端模块中的吸波磁片，可以起到吸收进入材料内电磁波的作用，防止电磁波干扰接收端设备电磁信号，避免电磁波使接收端电池等设备产生热效应；目前使用的铁硅铝合金与树脂的复合材料要求铁硅铝合金颗粒需要有统一的固定形状，并且要求金属颗粒在树脂中的排列有一定的取向，否则初始磁导率会很低。即使是金属颗粒在树脂中的取向很好，由于含有一定量的树脂，材料的初始磁导率也不会很高，但由于含有金属，材料的电阻率却较高。材料的这些缺点会导致电磁感应式无线充电设备效率低，电池等充电设备热效应明显，充电不安全。
公开号为CN102211929A公开了一种低温烧结高磁导率NiCuZn铁氧体材料，其特征在于：该材料是一种NiCuZn铁氧体材料，包括主成分以及辅助成分，主成分以氧化物含量计算为：Fe2O3为40.5-49.6mol%：ZnO为30-47mol%；CuO为5-20mol%；余为NiO；所述辅助成分包括NaCO3、B2O3、Ta2O5，相对所述主成分总量，NaCO3、B2O3、Ta2O5的总含量为0.16wt%-1.65wt%。该材料虽然有很好的高磁导率，但是其磁损耗也较高，不能满足要求。
发明内容
本发明为解决现有的吸波材料的磁导率较大而磁损耗也较大的技术问题，提供一种磁导率较大而磁损耗较小的吸波材料及其制备方法。
本发明提供了一种吸波材料，该吸波材料包括主成分、辅助成分及烧结助剂；所述主成分为Fe2O3、MnO、ZnO和MgO，所述辅助成分为CeO2和P2O5；所述CeO2和P2O5摩尔比为1-2：1。
本发明还提供了该吸波材料的制备方法，该方法包括以下步骤：
S1将主成分及烧结助剂混合，再加入溶剂和分散剂，进行湿法研磨、烘干得到粉料；
S2 粉料预烧：将粉料进行预烧；
S3向预烧后的粉料中加入CeO2和P2O5，球磨后过筛；
S4 成型：将步骤S3得到的粉料进行成型、烧结即得到本发明所述的吸波材料。
本发明选用CeO2和P2O5并控制其摩尔比为1-2：1，CeO2和P2O5起到协同作用，使吸波材料的初始磁导率和电阻率同时增大。使用该材料的磁场损耗可降至很低，大大提高了设备的充电工作效率。
具体实施方式
为了使本发明所解决的技术问题、技术方案及有益效果更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明提供了一种吸波材料，该吸波材料包括主成分、辅助成分及烧结助剂；所述主成分为Fe2O3、MnO、ZnO和MgO，所述辅助成分为CeO2和P2O5；所述CeO2和P2O5摩尔比为1-2：1。
本发明的吸波材料中，添加了高熔点的镧系金属氧化物CeO2，CeO2起到细化晶粒，提高材料的电阻率和起始磁导率，降低涡流损耗的作用。同时还添加了非金属氧化物P2O5，P2O5可以引起晶界附近金属离子的空位增多，加速晶界移动，材料密度增大，起始磁导率增加。控制P2O5和CeO2的摩尔比为1-2：1，可以使CeO2和P2O5起到协同作用，使材料的初始磁导率和电阻率同时增大。
根据本发明所你提供的吸波材料，优选地，以吸波材料的总摩尔量为基准，所述Fe2O3的含量为40-54mol%，所述MnO的含量为12-20mol%，所述ZnO的含量为22-25mol%，所述MgO的含量为5-10mol%，CeO2的含量为0.1-3.5mol%， P2O5的含量为0.1-2.5mol%，所述烧结助剂的含量为0.2-3.5mol%。
进一步地，以吸波材料的总摩尔量为基准，所述Fe2O3的含量为45-50mol%，所述MnO的含量为13-16mol%，所述ZnO的含量为22-25mol%，所述MgO的含量为5-10mol%，CeO2的含量为1.5-3.0mol%， P2O5的含量为1-2mol%，所述烧结助剂的含量为0.2-3.5mol%。
根据本发明所提供的吸波材料，所述烧结助剂降低烧结温度，使磁片在较低温度下就形成液相烧结，提高相对密度，增大产品强度。优选地，所述烧结助剂为所述烧结助剂为Nb2O5、MoO3、Bi2O3、V2O5 和SiO2中的至少一种。
根据本发明所你提供的吸波材料，优选地，以吸波材料的总摩尔量为基准，烧结助剂中，所述Nb2O5的含量为0.1-2.5mol%，所述MoO3的含量为0.1-1.5mol%，所述Bi2O3的含量为0.2-1.5mol%，所述V2O5的含量为0.1-1.5mol%，所述SiO2的含量为0.2-2.5mol%。
本发明所提供的吸波材料中， Nb2O5可以增大晶界厚度和晶界电阻率，从而导致材料电阻率增大。控制Bi2O3的添加量，形成液相烧结，促进晶粒长大，组织更致密，降低晶粒内外气孔率，适量添加可降低矫顽力，提高起始磁导率。添加的少量SiO2粉可以对Fe起到稀释作用，从而抑制了Fe2+和Fe3+的导电性，故电阻率增大。SiO2粉还具有表面渗透性好、比表面积大、密度低、机械性能好以及热稳定性好的特点，加入可以提高铁氧体强度。加入MoO3、Bi2O3、V2O5可以降低烧结温度，使吸波材料在较低温度下就形成液相烧结，提高相对密度，增大吸波材料的强度。
本发明还提供了一种本发明所述的吸波材料的制备方法，该方法包括以下步骤：
S1将主成分及烧结助剂混合，再加入溶剂和分散剂，进行湿法研磨、烘干得到粉料；
S2 粉料预烧：将粉料进行预烧；
S3向预烧后的粉料中加入CeO2和P2O5，球磨后过筛；
S4 成型：将步骤S3得到的粉料进行成型、烧结即得到本发明所述的吸波材料。
根据本发明所提供的制备方法，优选地，步骤S1所述的湿法研磨的速度为400-450r/min，时间为8-12h。
根据本发明所提供的制备方法，优选地，所述烘干的温度为60-80℃，时间为10-20h。
根据本发明所提供的制备方法，优选地，所述预烧的过程为：升温速率3-5℃/min，升温至700-950℃，保温1-4h，然后随炉冷却。
根据本发明所提供的制备方法，优选地，步骤S3所述的研磨的速度为300-450r/min，时间为4-10h。
根据本发明所提供的制备方法，优选地，所述成型方法为流延、涂布、压制模压和注射中的至少一种。
根据本发明所提供的制备方法，优选地，所述步骤S4所述的烧结过程为：升温速率0.5-3℃/min，温度1000℃-1150℃烧结，保温时间为2-4h。
本发明所提供的吸波材料，CeO2和P2O5按照摩尔比为1-2：1的比例添加，可以起到协同作用，使材料的初始磁导率和电阻率同时增大。使用该材料后发射端的磁场损耗可降至很低，大大提高了设备的充电工作效率。
下面通过具体实施例对本发明进行进一步的详细说明。
实施例1
1、按表1所示的原料含量（全部为摩尔含量，单位mol）将主成分及烧结助剂混合，再加入溶剂和分散剂，进行湿法研磨：450r/min，8h；
2、将步骤1研磨得到的粉料盛入容器内，放入烘箱烘干：80℃，10h；
3、粉料预烧：将烘干后的粉料粉碎，置入烧结容器中进行预烧： 5℃/min，升温至950℃，保温2h，随炉冷却；
4、向预烧后的粉料中加入CeO2和P2O5混合后进行球磨过筛；球磨转速为400r/min，时间为6h；
5、成型：采用模压方式成型成圆环状，环尺寸外径为20mm，内径为5mm，高度为8mm；
6、烧结：将成型得到的产品进行烧结，即得到本发明所述的吸波材料A1；烧结条件为：升温速率为2℃/min；300℃保温30min；550℃保温30min；900℃保温60min；最高温度为1100℃，保温120min；随炉冷却。
实施例2-7
按照实施例1的方法分别制备吸波材料A2-A7，区别在于：各原料含量见表1。
对比例1-3
按照实施例1的方法分别制备吸波材料CA1-CA3，区别在于：各原料含量见表1。
对比例4
采用CN102211929A实施例1的方法制备吸波材料CA4。
表1
实施例1 实施例2 实施例3 实施例4 实施例5 实施例6 实施例7 对比例1 对比例2 对比例3
Fe2O3 1 1 1 1 1 1 1 1 1 1
MnO 0.3 0.36 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3
ZnO 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5
MgO 0.22 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
CeO2 0.04 0.06 0.04 0.05 0.05 0.077 0.002 0 0.04 0
P2O5 0.02 0.04 0.03 0.04 0.05 0.055 0.002 0 0 0.04
Nb2O5 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02
MoO3 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015
Bi2O3 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02
V2O5 0.01 0.01 0.01 0.01 0.01 0.007 0.01 0.01 0.01 0.01
SiO2 0.01 0.01 0.01 0.01 0.01 0.007 0.01 0.01 0.01 0.01
测试方法及结果
1、初始磁导率测试
采用美国Aglient公司生产HP4284A 测试仪和测量专用夹具16454A测试材料初始磁导率。把粉末样品采用模压的方法制成中空的圆柱体，入炉烧结，圆环尺寸外径为20mm，内径为5mm，高度为8mm。将该圆环体看做一个单匝线圈，通过测量该线圈的阻抗可得到圆环线圈电感的大小，继而计算出样品初始磁导率，测试频率100kHz。结果见表2。
2、电阻率测试
采用Semilab公司生产的RT-100电阻率测量仪测量材料的电阻率。把粉末样品采用模压的方法制成正六面体，入炉烧结，六面体长20～25mm，截面对角线长10～15mm。将样品放入测试设备中，按测试说明书的步骤测量材料的电阻率。结果见表2。
表2
初始磁导率μi 电阻率ρ/Ω·m
A1 7000 4.75
A2 12000 5.68
A3 7200 4.55
A4 7500 4.72
A5 10000 5.63
A6 9800 5.20
A7 7010 4.80
CA1 4200 2.51
CA2 5500 4.33
CA3 5400 4.98
CA4 4000 2.30
从表2中可以看出，本发明的吸波材料不仅具有很高的初始磁导率，而且具有很高的电阻率，而对比例的吸波材料虽然具有较高的初始磁导率，但是其电阻率低。说明本发明的吸波材料具有高的初始磁导率和高的电阻率。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (11)

1.一种吸波材料，其特征在于，该吸波材料包括主成分、辅助成分及烧结助剂；所述主成分为Fe2O3、MnO、ZnO和MgO，所述辅助成分为CeO2和P2O5；所述CeO2和P2O5摩尔比为1-2：1；所述烧结助剂为Nb2O5、MoO3、Bi2O3、V2O5 和SiO2中的至少一种。
2.根据权利要求1所述的吸波材料，其特征在于，以吸波材料的总摩尔量为基准，所述Fe2O3的含量为40-54mol%，所述MnO的含量为12-20mol%，所述ZnO的含量为22-25mol%，所述MgO的含量为5-10mol%，CeO2的含量为0.1-3.5mol%， P2O5的含量为0.1-2.5mol%，所述烧结助剂的含量为0.2-3.5mol%。
3.根据权利要求1所述的吸波材料，其特征在于，以吸波材料的总摩尔量为基准，所述Fe2O3的含量为45-50mol%，所述MnO的含量为13-16mol%，所述ZnO的含量为22-25mol%，所述MgO的含量为5-10mol%，CeO2的含量为1.5-3.0mol%,P2O5的含量为1-2mol%，所述烧结助剂的含量为0.2-3.5mol%。
4.根据权利要求1所述的吸波材料，其特征在于，以吸波材料的总摩尔量为基准，烧结助剂中，所述Nb2O5的含量为0.1-2.5mol %，所述MoO3的含量为0.1-1.5mol%，所述Bi2O3的含量为0.2-1.5mol%，所述V2O5的含量为0.1-1.5mol %，所述SiO2的含量为0.2-2.5mol%。
5.一种权利要求1-4任意一项所述的吸波材料的制备方法，其特征在于，该方法包括以下步骤：
S1将主成分及烧结助剂混合，再加入溶剂和分散剂，进行湿法研磨、烘干得到粉料；
S2 粉料预烧：将粉料进行预烧；
S3向预烧后的粉料中加入CeO2和P2O5，球磨后过筛；
S4 成型：将步骤S3得到的粉料进行成型、烧结即得到所述的吸波材料。
6.根据权利要求5所述的制备方法，其特征在于，步骤S1所述的湿法研磨的速度为400-450r/min，时间为8-12h。
7.根据权利要求5所述的制备方法，其特征在于，所述烘干的温度为60-80℃，时间为10-20h。
8.根据权利要求5所述的制备方法，其特征在于，所述预烧的过程为：升温速率3-5℃/min，升温至700-950℃，保温1-4h，然后随炉冷却。
9.根据权利要求5所述的制备方法，其特征在于，步骤S3所述的湿法研磨的速度为300-450r/min，时间为4-10h。
10.根据权利要求5所述的制备方法，其特征在于，所述成型方法为流延、涂布、压制模压和注射中的至少一种。
11.根据权利要求5所述的制备方法，其特征在于，所述步骤S4所述的烧结过程为：升温速率0.5-3℃/min，温度1000℃-1150℃烧结，保温时间为2-4h。
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