CN109320228B - 一种磁共振式无线充电用镍锌铁氧体材料及其制备方法 - Google Patents
一种磁共振式无线充电用镍锌铁氧体材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004537 pulping Methods 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 6
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 6
- 239000011118 polyvinyl acetate Substances 0.000 claims description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 239000004014 plasticizer Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000001238 wet grinding Methods 0.000 claims description 3
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims 2
- 239000011787 zinc oxide Substances 0.000 claims 2
- 239000005751 Copper oxide Substances 0.000 claims 1
- 229910000431 copper oxide Inorganic materials 0.000 claims 1
- 229910000480 nickel oxide Inorganic materials 0.000 claims 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 11
- 230000004907 flux Effects 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000004615 ingredient Substances 0.000 abstract description 3
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- 230000000052 comparative effect Effects 0.000 description 10
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- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005674 electromagnetic induction Effects 0.000 description 2
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- 238000000748 compression moulding Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
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- 230000002500 effect on skin Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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Abstract
本发明公开了一种磁共振式无线充电用镍锌铁氧体材料及其制备方法，所述镍锌铁氧体由主成分和副成分组成，Fe2O3：49.0~49.9mol%、NiO：15.5~25.6mol%、ZnO：28.1~30.2mol%、CuO：2.5~5.5mol%、Co3O4：1.25~2.55mol%；副成分为：SiO2：0.04~0.10wt%、CaCO3：0.03~0.15wt%、Bi2O3：0.04~0.21wt%、MnO：0.01~0.03wt%、纳米钛白粉：0.02~0.25wt%。采用氧化物法工艺制备，步骤依次为混合、预烧、粉碎、制浆、增塑、膜片成型、烧结。烧结后制品的晶粒平均尺寸为1～5μm，晶界多，制品在6~10MHz可以保持较高的磁导率、较低的磁损耗及高饱和磁通密度的特点，适应磁共振式无线充电用铁氧体屏蔽材料高磁导率低损耗及高饱和磁通密度的性能要求。
Description
技术领域
本发明属于软磁铁氧体技术领域，具体涉及一种磁共振式无线充电用镍锌铁氧体材料及其制备方法。
背景技术
随着智能电子产品的迅猛发展，无线充电技术目前的发展态势相当迅速。根据设计原理和机理的不同，无线充电的实现方式根据不同的应用频段可分为三类，低频是电磁感应耦合式，中高频是电磁共振式，更高频是电磁辐射式。目前，市场上应用的非接触式无线充电设备主要是电磁感应式（Qi标准）和电磁共振式（A4WP标准）无线充电器，而且已经实现了商业化。Qi标准虽然能量传输效率较高，但充电的距离比较短，最大仅有几个厘米，而且不支持多个设备同时充电。相比于Qi，A4WP标准采用了更大的输出线圈，能同时为多台设备充电，充电范围更广，同时由于设定了精确的共振频率，即使微弱的感应磁场也能为设备充电，A4WP标准的充电范围会比Qi大得多，因此其实用性更强。
A4WP标准采用的共振频率一般较高，高频交变电磁场遇到金属，则会产生较大的电子涡流，电子涡流会对金属产生趋肤效应，在金属上产生热能，从而导致传输效率降低、电能浪费；如果充电电池内部的金属受到该磁场的影响，产生的涡流损耗会引起电池发烫，存在极大地安全隐患；此外交变磁场会对周边器件产生干扰而影响整个充电器正常工作。因此在技术层面必须采用屏蔽材料来阻挡磁力线外泄，从而实现无线充电装置安全、高效的运行。实际设计中在发射线圈端、接收线圈端加入铁氧体屏蔽材料后，可以达到提高效率、降低干扰、从而提高无线充电设备整体性能的目的。镍锌铁氧体材料电阻率高、应用频率高，在高频下有较高的磁导率及较低的损耗，非常适合应用到磁共振式无线充电设备中。同时A4WP标准需要实现一对多充电功能以及快速充电，往往功率较大，这也要求铁氧体材料必须具备较高的饱和磁通密度。
在国内已有一些相关镍锌铁氧体材料的制造方法的专利，具体如下：
（1）公开号为CN 104030674B，公开日为2016.03.30，发明名称为“一种NiCuZn铁氧体材料及其制备方法”的中国专利公开了一种针对于无线充电中铁氧体材料作为屏蔽材料应用背景的NiCuZn 铁氧体材料及其制备方法。采用传统的氧化物烧结制备工艺，制备出的NiCuZn 铁氧体材料在100kHz~200kHz 频率区间，起始磁导率μi为950~1000，100kHz、100mT、25℃下功率损耗Pcv 为460~500mW/cc，饱和磁感应强度Bs≥360mT，矫顽力Hc<32A/m。实现了无线充电中铁氧体材料作为屏蔽材料要求的：较低的功率损耗Pcv和Hc，更高的μi和较高的Bs；
（2）公开号为CN 104030674B，公开日为2014.10.22，发明名称为“一种无线信号感应用镍锌铁氧体材料、薄片磁心及其制备方法” 的中国专利公开了一种一种无线信号感应用镍锌铁氧体材料、薄片磁心及其制备方法。该镍锌铁氧体采用氧化物法制备，薄片磁心为网状薄片，长度45~250mm，宽度45~250mm，厚度0.05~0.3mm，由小薄片连结而成，小薄片间的间隙＜ 50μm，直接采用模压成型后烧结而成，或者压制成磁棒烧结后切成小薄片并经SMT贴装而成。该材料在13.56MHz 具有μ'=125±20% 且μ"≤4的电磁性能，满足无线信号感应对铁氧体材料高频低损耗的要求。
发明内容
本发明目的是针对上述技术问题，提供一种磁共振式无线充电用镍锌铁氧体材料及其制备方法，在主成分中添加Co3O4，并控制主成分、副成分的组成含量，使镍锌铁氧体材料同时具备高频低损耗、高饱和磁通密度的性能。
为了达到上述目的，本发明采取以下的技术方案：一种磁共振式无线充电用镍锌铁氧体材料及其制备方法，其特征包括主成分和副成分，所述主成分为五元系，以各自标准物计的含量如下：
Fe2O3：49.0~49.9mol%
NiO：15.5~25.6mol%
ZnO：28.1~30.2mol%
CuO：2.5~5.5mol%
Co3O4：1.25~2.55mol%；
所述副成分包括二氧化硅、碳酸钙、氧化铋、氧化锰、纳米钛白粉，相对所述主成分总量，所述副成分以各自标准物计的含量如下：
SiO2：0.04~0.10wt%
CaCO3：0.03~0.15wt%
Bi2O3：0.04~0.21wt%
MnO：0.01~0.03wt%
纳米钛白粉：0.02~0.25wt%。
作为一种优选，相对所述主成分总量，所述副成分优选SiO2：0.075wt%，CaCO3：0.065wt%，Bi2O3：0.06wt%，MnO：0.024wt%，纳米钛白粉：0.096wt%。
一种上述的磁共振式无线充电用镍锌铁氧体材料的制造方法，包括如下步骤：
（1）混合：按主成分配比配料后置于混合设备中进行混合，混合时间为30~45min；
（2）预烧：将混合好的材料在钟罩窑中进行预烧，预烧温度控制在880±20℃，保温1.5~2h后随炉冷却；
（3）粉碎：将上步得到的主成分预烧料中加入副成分后采用立式砂磨机进行湿法粉碎，粉碎时间为70~90min，粉碎后料浆中位粒径控制在0.6~0.8μm，并烘干；
（4）制浆：在上步制备的粉料中加入相当于粉料重量的1.6~3.0%的PVA，7.5~9.5%的有机溶剂，0.2~0.5%的分散剂，在混合设备中混合15~20h，制成料浆；
（5）增塑：在上步的料浆中加入2.2~4.1%的增塑剂，进行增塑处理，使料浆粘度达到60~85Pa.s；
（6）膜片成型：将上步的料浆在成型设备中进行膜片成型，膜片坯件厚度为0.06~0.20mm；
（7）烧结：将上步的膜片坯件在电阻炉中进行烧结，烧结温度控制在950℃~1050℃，保温120~150分钟，烧结气氛为空气，烧结结束后随炉冷却至室温。
通过以上工序制得所述镍锌铁氧体磁片样品，进行贴膜柔性处理后激光切割成Φ18mm×Φ6mm×0.1mm磁环样品。
本发明通过对Fe2O3、ZnO含量的调整来优化材料的饱和磁通密度、起始磁导率以及居里温度；通过NiO、Co3O4含量的调整来调整材料的使用频率，降低损耗；通过CuO含量的调整来调整材料的烧结温度。在副成分中加入SiO2、CaCO3增加晶界的厚度，降低高频段损耗；加入Bi2O3加速固相反应，促进晶粒生长；加入MnO、钛白粉改善材料的频率特性与磁导率温度特性；再通过烧结工艺进一步调整材料晶体结构和晶界分布，从而得到高频低损耗高饱和磁通密度镍锌铁氧体材料。在采用A4WP技术标准的发射线圈端、接收线圈端加入该镍锌铁氧体材料后，可以达到提高效率、降低干扰、从而提高无线充电设备整体性能的目的。
材料的性能指标如下：
（1）复数磁导率实部 μ′：200(1±20%),( f=6MHz,100mV,25℃)
240(1±20%),( f=10MHz,100mV,25℃)
复数磁导率虚部 μ″：≤3, ( f=6MHz,100mV,25℃)
≤10, ( f=10MHz,100mV,25℃)
（2）饱和磁通密度 Bs：≥420mT,( f=1kHz,Hm=4000A/m,25℃)
（3）居里温度 Tc：≥200 ℃, (f=10kHz,B＜0.25mT)。
附图说明
图1 为实施例1铁氧体材料磁谱曲线图；
图2断面SEM照片：(a) 对比例1；(b) 实施例1。
具体实施方式
以下按照具体实施例说明本发明，但本发明不限定于这些实施例。
本发明的镍锌铁氧体采用传统氧化物法制造，具体步骤依次如下：
（1）混合：按表1(实施例和对比例)主成分配比配料后置于混合设备中进行混合，混合时间为45min；
（2）预烧：将混合好的材料在钟罩窑中进行预烧，预烧温度控制在880℃，保温2h后随炉冷却；
（3）粉碎：将上步得到的主成分预烧料中加入副成分后采用立式砂磨机进行湿法粉碎，粉碎时间为90min，粉碎后料浆中位粒径控制在0.6~0.8μm，并烘干；
（4）制浆：在上步制备的粉料中加入相当于粉料重量的2.0%的PVA，7.5%的有机溶剂，0.2~0.5%的分散剂，在混合设备中混合20h，制成料浆；
（5）增塑：在上步的料浆中加入2.2~4.1%的增塑剂，进行增塑处理，使料浆粘度达到60~85Pa.s；
（6）膜片成型：将上步的料浆在成型设备中进行膜片成型，膜片坯件厚度为0.125mm；
（7）烧结：将上步的膜片坯件在电阻炉中进行烧结，烧结温度控制在990~1025℃，保温140分钟，烧结气氛为空气，烧结结束后随炉冷却至室温。
通过以上工序制得所述镍锌铁氧体磁片样品，进行贴膜柔性处理后激光切割成Φ18mm×Φ6mm×0.1mm磁环样品。
将烧结后的磁环分别进行测试和评价。用E4991B测试仪测量样品在6MHz、10MHz下的复数磁导率实部和虚部；用HP4284A配合MC-711小型超低温试验箱和PHH-101高温试验箱测试样品的居里温度Tc；用SY-8218型B-H分析仪测试样品的饱和磁通密度Bs；
表1 实施例和对比例的成份配比
表2 实施例和对比例的磁性能
注意: 超过规格上限的附加“﹢”，超过规格下限的附加“－”。
表2列出了实施例和对比例的性能及评价，从表2中可以看出，本发明的实施例和对比例相比较，本发明有效地降低了材料的磁损耗的同时，能保持较高的磁导率，较高的饱和磁感应强度，并具有较高的居里温度。对比实施例和对比例的微观结构(图2)，对比例材料结晶粗大，晶界薄，主要晶粒尺寸为6～10μm，气孔率较高；实施例的结晶较小，晶界明显，主要晶粒尺寸为1～5μm。晶粒细化、晶界增多，电阻率升高应该是实施例的材料的μ′′相对于对比例降低的重要原因。本发明的材料应该能够满足磁共振式无线充电用镍锌铁氧体材料的性能要求。
本发明所描述的具体实施例仅仅是对本发明作举例说明，相关技术领域的专家或技术人员可以对所描述的具体实施例做不同程度的修改，补充或者用类似的方式替代，但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (4)
1.一种磁共振式无线充电用镍锌铁氧体材料，其特征在于，其包括主成分和副成分组成，所述主成分为五元系，分别为：氧化铁、氧化镍、氧化锌、四氧化三钴、氧化铜，所述主成分以各自标准物计的含量如下：
Fe2O3：49.0~49.9mol%、NiO：15.5~25.6mol%、ZnO：28.1~30.2mol%、CuO：2.5 ~ 5.5mol%、Co3O4：1.25~2.55mol%；
所述副成分包括二氧化硅、碳酸钙、氧化铋、氧化锰、纳米钛白粉，相对所述主成分总量，所述副成分以各自标准物计的含量如下：
SiO2：0.04~0.10wt%、CaCO3：0.03~0.15wt%、Bi2O3：0.04~0.21wt%、MnO：0.01~0.03wt%、纳米钛白粉：0.02~0.25wt%。
2.如权利要求1所述的磁共振式无线充电用镍锌铁氧体材料，其特征在于：相对所述主成分总量，所述副成分为SiO2：0.075wt%，CaCO3：0.065wt%，Bi2O3：0.06wt%，MnO：0.024wt%，纳米钛白粉：0.096wt%。
3.一种如权利要求1所述的磁共振式无线充电用镍锌铁氧体材料的制备方法，其特征在于，包括如下步骤：
（1）混合：按主成分配比配料后置于混合设备中进行混合，混合时间为30~45min；
（2）预烧：将混合好的材料在钟罩窑中进行预烧，预烧温度控制在880±20℃，保温1.5~2h后随炉冷却；
（3）粉碎：将上步得到的主成分预烧料中加入副成分后采用立式砂磨机进行湿法粉碎，粉碎时间为70~90min，粉碎后料浆中位粒径控制在0.6~0.8μm，并烘干；
（4）制浆：在上步制备的粉料中加入相当于粉料重量的1.6~3.0%的PVA，7.5~9.5%的有机溶剂，0.2~0.5%的分散剂，在混合设备中混合15~20h，制成料浆；
（5）增塑：在上步的料浆中加入2.2~4.1%的增塑剂，进行增塑处理，使料浆粘度达到60~85Pa.s；
（6）膜片成型：将上步的料浆在成型设备中进行膜片成型，膜片坯件厚度为0.06~0.20mm；
（7）烧结：将上步的膜片坯件在电阻炉中进行烧结，烧结温度控制在950℃~1050℃，保温120~150分钟，烧结气氛为空气，烧结结束后随炉冷却至室温。
4.根据权利要求3所述的磁共振式无线充电用镍锌铁氧体材料制备方法，其特征在于，在增塑步骤中：加入相当于料浆重量的2.2~4.1%的增塑剂，进行增塑处理，使料浆粘度达到60~85Pa.s。
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