CN109678481B - 一种复合铁氧体片的制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
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- 238000005245 sintering Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 22
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- 229910000431 copper oxide Inorganic materials 0.000 claims description 11
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 11
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 11
- 239000011787 zinc oxide Substances 0.000 claims description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
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- 239000011733 molybdenum Substances 0.000 claims description 10
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- 238000009825 accumulation Methods 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 8
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- 238000001354 calcination Methods 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 7
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
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- 239000010937 tungsten Substances 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
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- 239000010941 cobalt Substances 0.000 claims description 2
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- YHAIUSTWZPMYGG-UHFFFAOYSA-L disodium;2,2-dioctyl-3-sulfobutanedioate Chemical compound [Na+].[Na+].CCCCCCCCC(C([O-])=O)(C(C([O-])=O)S(O)(=O)=O)CCCCCCCC YHAIUSTWZPMYGG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 4
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Abstract
本发明公开了一种复合铁氧体片的制备方法。其主要步骤为：1）预烧粉制备；2）制浆；3）喷雾造粒；4）多层粉末喷涂；5）放电等离子体烧结。本发明的优点是可以制备出具有多层结构的复合铁氧体片，在很宽的频率范围内可以获得高磁导率，避免传统采用流延方法生产的铁氧体片外观缺陷多，使用频率单一，生产周期长等缺点。
Description
技术领域
本发明涉及铁氧体片的制备方法，特别是涉及一种多层结构的复合铁氧体片的制备方法，属于电子元器件新材料新工艺领域。
背景技术
随着电子信息产业的快速发展，电子产品的功能越来越丰富、强大，这也伴随着耗电量的迅速加快，一块手机电池往往很难满足用户一天的使用。目前主流的有线充电方式存在容易损环、携带不便、接口不兼容、资源浪费等问题。人们对手机等用电设备的安全性、便携性、即时性要求越来越高，在电池续航没有取得革命性突破的情况下，无线充电方式获得越来越多的人的关注。随着苹果公司在新一代的iphone中集成了Qi标准的无线充电模块，无线充电市场有望迎来大爆发。铁氧体片在无线充电中，位于发射线圈和接收线圈端，作为隔磁片，可以提高线圈之间的耦合系数，进而提高充电效率，还能屏蔽线圈发射出来的电磁场对电池、电路等其器件的电磁干扰，对于提高无线充电设备的安全性必不可少。
目前已经开发出了工作频率在100-300KHz的感应式无线充电和工作频率在数MHz的共振式无线充电，正在研发工作在GHz的微波无线充电，传统的铁氧体片采用流延烧结的方法制备，是一种均质的材料，成分固定，只在某一频段中具有较好的性能，很难同时满足多种无线充电频率的要求。同时传统流延烧结法制备铁氧体片存在翘曲、卷边等外观缺陷，产品良率低，工艺复杂，生产周期长。
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，提供一种复合铁氧体片的制备方法。本发明提供的复合铁氧体片在数百KHz到GHz的频率范围内都能获得较高的磁导率，频率为 100KHz时，其磁导率实部大于500，频率为6.78MHz时，其磁导率实部大于200，频率为2.4GHz时，磁导率实部大于50。
为了达到上述目的，本发明是这样实现的。
按照原料摩尔配比为：氧化铁46.5%~50%、氧化镍8%~15%、氧化铜6%~12%、氧化锌15%~26%、氧化钴0~5%放入球磨机，加入去离子水球磨2-6小时后烘干，进行煅烧，煅烧温度为780-920℃，煅烧时间为2-4小时得到不同成分组成的预烧粉。
将预烧粉、水、表面活性剂，加入球磨机球磨至粒度为0.5~3μm，再加入粘结剂球磨制备得到均匀弥散不沉降的浆料。其中溶剂水的质量为预烧粉质量的30%~50%。表面活性剂为聚丙烯酸钠、十二烷基苯磺酸钠、二辛基琥珀酸磺酸钠或油酸钠中的一种，质量为所加入的预烧粉的0.3-2.5%。粘结剂为乙烯乙酸酯、丙烯酸、环氧水性树脂或淀粉中的一种，质量为所加入的预烧粉的0.1-5%。
采用喷雾造粒的方法，对浆料进行干燥，造粒，喷雾造粒的粒度d50为5~10 μm。
在石墨模具中首先放置第一块耐高温金属板，然后均匀喷涂具有不同成分的多层预烧粉造粒料，然后放置第二块耐高温金属板。所述的耐高温金属板/多层预烧粉堆积层/耐高温金属板结构可以多次重复出现，即形成耐高温金属板/多层预烧粉堆积层/耐高温金属板/多层预烧粉堆积层/耐高温金属板/···/耐高温金属板的重复结构。
多层预烧粉堆积层中单层预烧粉厚度不超过100μm，耐高温金属板为钼板、钨板、或者以铁、镍、钴为主要成分的高温合金，厚度40-200μm，表面粗糙度小于2μm。
对上述复合体进行放电等离子体烧结，烧结温度为750-880℃，施加压力为20-100MPa。
本发明与现有技术相比，本发明提供的复合铁氧体片在数百KHz到GHz的频率范围内都能获得较高的磁导率，频率为100KHz时，其磁导率实部大于500，频率为6.78MHz时，其磁导率实部大于200，频率为2.4GHz时，磁导率实部大于50。
相比于传统的流延烧结制备铁氧体片的方法，本发明生产工序少，烧结时间大大缩短，制备的铁氧体片不会存在翘曲、波浪边等外观缺陷，并且能够制备较厚的铁氧体片。
附图说明
图1为复合铁氧体片的成型烧结过程示意图。
附图说明：1-石墨模具；2-耐高温金属板；3-多层预烧粉堆积层；31-单层第一组份铁氧体预烧粉造粒料；32-单层第二组份铁氧体预烧粉造粒料；33-单层第三组份铁氧体预烧粉造粒料；4-施加压力的方向。
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。
按照原料摩尔配比，配制如下两种组分：组分1为氧化铁48.5%、氧化镍15%、氧化铜11%、氧化锌25.5%，组分2为氧化铁48.5%、氧化镍11%、氧化铜11%、氧化锌26%、氧化钴3.5%，分别放入球磨机，加入去离子水球磨4小时后烘干，进行煅烧，煅烧温度为780度，煅烧时间为4小时得到两组预烧粉。
将预烧粉、水、表面活性剂，加入球磨机球磨，粒度为0.5μm，再加入粘结剂，球磨制备得均匀弥散不沉降的浆料。其中溶剂水的质量为预烧粉质量的的30%。表面活性剂为聚丙烯酸钠，质量为所加入的预烧粉的0.3%。粘结剂为乙烯乙酸酯，质量为所加入的预烧粉的0.4%。
采用喷雾造粒的方法，对浆料进行干燥，造粒，喷雾造粒的粒度d50为5μm。
在石墨模具中首先放置第一块钨板，然后均匀喷涂具有不同成分的两种预烧粉造粒料，然后放置第二块钨板。每层预烧粉厚度为100μm，钨板厚度200微米，表面粗糙度为1μm。
对上述复合体进行放电等离子体烧结，烧结温度为750℃，施加压力为40MPa。
制备出的铁氧体盘表面平整无翘曲，组织致密，晶粒尺寸为5μm，孔隙率低，密度为4.95g/cm3。将样品进行磁性能测试，频率为 100KHz时，其磁导率实部550，频率为6.78MHz时，其磁导率实部210，频率为2.4GHz时，磁导率实部为58。
实施例2。
按照原料摩尔配比，配制如下三种组分：组分1为氧化铁48.5%、氧化镍15%、氧化铜11%、氧化锌25.5%，组分2为氧化铁48.5%、氧化镍11%、氧化铜11%、氧化锌26%、氧化钴3.5%，组分3为氧化铁50%、氧化镍15%、氧化铜9%、氧化锌21%、氧化钴5%，分别放入球磨机，加入去离子水球磨4小时后烘干，进行煅烧，煅烧温度为820度，煅烧时间为4小时得到三组预烧粉。
将预烧粉、水、表面活性剂，加入球磨机球磨，粒度为1.5μm，再加入粘结剂，球磨制备得均匀弥散不沉降的浆料。其中溶剂水的质量为预烧粉质量的40%。表面活性剂为十二烷基苯磺酸钠，质量为所加入的预烧粉的0.8%。粘结剂为丙烯酸，质量为所加入的预烧粉的1.0%。
采用喷雾造粒的方法，对浆料进行干燥，造粒，喷雾造粒的粒度d50为7μm。
在石墨模具中首先放置第一块钼板，然后均匀喷涂具有不同成分的三种预烧粉造粒料，然后放置第二块钼板。每层预烧粉厚度为80μm，钼板厚度150微米，表面粗糙度为1.5μm。
对上述复合体进行放电等离子体烧结，烧结温度为780℃，施加压力为80MPa。
制备出的铁氧体盘表面平整无翘曲，组织致密，晶粒尺寸为4μm，孔隙率低，密度为4.92g/cm3。将样品进行磁性能测试，频率为 100KHz时，其磁导率实部580，频率为6.78MHz时，其磁导率实部240，频率为2.4GHz时，磁导率实部为75。
实施例3。
按照原料摩尔配比，配制如下三种组分：组分1为氧化铁49.5%、氧化镍14%、氧化铜12%、氧化锌24.5%，组分2为氧化铁49.5%、氧化镍10%、氧化铜12%、氧化锌24%、氧化钴4.5%，组分3为氧化铁50%、氧化镍15%、氧化铜10%、氧化锌20%、氧化钴5%，分别放入球磨机，加入去离子水球磨5小时后烘干，进行煅烧，煅烧温度为810度，煅烧时间为3小时得到预烧粉。
将预烧粉、水、表面活性剂，加入球磨机球磨，粒度为3μm，再加入粘结剂球磨制备得均匀弥散不沉降的浆料。其中溶剂水的质量为预烧粉质量的50%。表面活性剂为二辛基琥珀酸磺酸钠，质量为所加入的预烧粉的2.5%。粘结剂为淀粉，质量为所加入的预烧粉的3.1%。
采用喷雾造粒的方法，对浆料进行干燥，造粒，喷雾造粒的粒度d50为10μm。
在石墨模具中首先放置第一块钼板，然后均匀喷涂具有不同成分的三种预烧粉造粒料，然后放置第二块钼板。第一层预烧粉厚度为80μm，第二层预烧粉厚度为100μm，第三层预烧粉厚度为90μm，钼板厚度120μm，表面粗糙度为0.8μm。
对上述复合体进行放电等离子体烧结，烧结温度为800℃，施加压力为60MPa。
制备出的铁氧体盘表面平整无翘曲，组织致密，晶粒尺寸为4.5μm，孔隙率低，密度为4.96g/cm3。将样品进行磁性能测试，频率为 100KHz时，其磁导率实部620，频率为6.78MHz时，其磁导率实部280，频率为2.4GHz时，磁导率实部为82。
以上所述仅为本申请较优的实施例，并非因此限定本申请的保护范围，凡事利用本申请说明书及附图内容所做的等效结构，或直接或间接地运用在其他相关的技术领域，均同理包括在本申请的保护范围内。
Claims (7)
1.一种复合铁氧体片的制备方法，其特征在于制备步骤为：
1）预烧粉制备：将氧化铁、氧化镍、氧化铜、氧化锌、氧化钴按比例球磨混合、烘干、预烧，得到不同成分的预烧粉；
2）制浆：将预烧粉、水、表面活性剂，加入球磨机球磨至粒度为0.5~3μm，再加入粘结剂制备得均匀弥散不沉降的浆料；
3）喷雾造粒：采用喷雾造粒的方法使浆料干燥，获得粒度分布均匀的预烧粉造粒料；
4）多层粉末喷涂与叠片：在石墨模具中放置耐高温金属板，依次将不同成分的预烧粉造粒料在石墨模具中喷涂，得到多层预烧粉末堆积层，然后放置耐高温金属片，形成耐高温金属板/多层预烧粉堆积层/耐高温金属板结构；重复前述喷涂多层粉末堆积层步骤，在最表面放置高温金属片；
5）放电等离子体烧结；
所述原料摩尔配比为：氧化铁46.5%~50%、氧化镍8%~15%、氧化铜6%~12%、氧化锌15%~26%、氧化钴0~5%；
所述复合铁氧体片在频率为 100KHz时，磁导率实部大于500；频率为6.78MHz时，磁导率实部大于200；频率为2.4GHz时，磁导率实部大于50。
2.根据权利要求1所述的一种复合铁氧体片的制备方法，其特征在于：所述球磨混合、烘干、煅烧工艺具体为将原料按照配比放入球磨机，加入去离子水球磨2~6小时后烘干，进行煅烧，煅烧温度为780~920℃，煅烧时间为2~4小时得到预烧粉。
3.根据权利要求1所述的一种复合铁氧体片的制备方法，其特征在于：所述浆料中水的质量为预烧粉质量的30%~50%；所述的表面活性剂为聚丙烯酸钠、十二烷基苯磺酸钠、二辛基琥珀酸磺酸钠或油酸钠中的一种，质量为所加入的预烧粉的0.3~2.5%；所述的粘结剂为乙烯乙酸酯、丙烯酸、环氧水性树脂或淀粉中的一种，质量为所加入的预烧粉的0.1~5%。
4.根据权利要求1所述的一种复合铁氧体片的制备方法，其特征在于：所述的喷雾造粒的粒度d50为5~10 μm。
5.根据权利要求1所述的一种复合铁氧体片的制备方法，其特征在于：所述的耐高温金属板/多层预烧粉堆积层/耐高温金属板结构可以多次重复出现。
6.根据权利要求1所述的一种复合铁氧体片的制备方法，其特征在于：所述的多层预烧粉堆积层中单层预烧粉厚度不超过100μm；耐高温金属板为钼板、钨板、或者以铁、镍、钴为主要成分的高温合金，厚度40~200μm，表面粗糙度小于2μm。
7.根据权利要求1所述的一种复合铁氧体片的制备方法，其特征在于：所述的放电等离子体烧结温度为750~880℃，施加压力为20~100MPa。
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