CN108793992A - 一种多相复合尖晶石柔性材料制造方法 - Google Patents
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Abstract
科技产品对人类社会行为和生活方式的改变无处不在，智能手机、汽车电子等领域的无线充电技术让人们的舒适感和便捷性得到前所未有的提高。本发明的多相复合尖晶石柔性材料制造方法，通过单相颗粒制作、第二相复合、成型烧结等工序，最终得到一种柔性材料，具有高的复数磁导率实部，低的复数磁导率虚部，高的饱和磁通密度。材料柔韧性好，可弯折，适用于制作柔性磁片、柔性变压器等产品。
Description
技术领域
本发明属于柔性材料技术领域，具体涉及到可用于制作柔性变压器、柔性磁片的软磁材料，适合于工作在10kHz至50MHz范围的，具有宽工作频率范围、高磁导率、低损耗的多相复合尖晶石柔性材料及其制备方法。
背景技术
当前社会生活节奏不断加快，消费类电子、汽车电子技术不断发展进步，人们对电子产品、汽车产品体验的要求越来越高。新的设计层出不穷，基础材料需要变革和创新才能满足产品和设备的要求。
无线充电技术起源于1890年，物理学家兼电气工程师尼古拉•特斯拉就已经做了无线输电试验，实现了交流发电。2007年，麻省理工学院等研究团队发表了磁共振传输能量的研究成果。2014年，无线充电联盟宣布，A4WP技术标准支持等充电功率增加到50W。
目前无线充电的基本模式有电磁感应式、磁场共振和无线电波式几种原理。其中以电磁感应式应用最为广泛。在发射端和接收端，模组都是磁片加线圈组合的方式。电子设备不断向着轻、薄、小和高效率的方向发展，LED显示屏、手机，都开始出现可折叠、可弯折的产品，磁性材料成为其中最薄弱环节。
2010年以后，柔性PCB板问世，柔性电源的制作成为可能。作为电源PCB上体积最大的磁性材料变压器磁芯、电感器磁芯，改变不可弯折变形的状态变得更有意义。
发明内容
针对无线充电技术和柔性电源对软磁材料的新要求，本发明的目的是提供一种可供无线充电设备、柔性电源等应用领域使用的多相复合尖晶石柔性材料。
所述的多相复合尖晶石柔性材料，其成分以氧化物计算分别为Fe2O3：40mol%~65mol%，NiO：1mol%~10.0mol%，ZnO：2mol%~15mol%，MnO：2mol%~40mol%，CuO：1mol%~10mol%。最终材料可以含有其中的几种或者全部。
本发明的多相复合尖晶石柔性材料，具有高的复数磁导率实部和低的复数磁导率虚部，高的饱和磁通密度，宽的使用频率范围，从10kHz到50MHz。
本发明的多相复合尖晶石柔性材料，主体具有多相结构，几种单相尖晶石结构并存，产品具有单相尖晶石结构无法兼顾的优异性能。这种材料，即可以是由2种单相尖晶石结构的复合，也可以是1种单相尖晶石结构和1种多相尖晶石结构的复合，或者2中多相尖晶石结构的复合。
本发明的多相复合尖晶石柔性材料，制作工艺包括单相颗粒制作、第二相复合、成型烧结等几个步骤。
具体实施方式
下面以2相都为单相尖晶石材料的多相复合尖晶石柔性材料为例，对本发明的制造方法进行详细说明。
第一步，单相颗粒制作。
按一定比例称取Fe2O3、MnO，加入球磨机，配合一定数量的水，通过球磨机充分混合后，烘干，进入振磨机振磨20min。振磨后的粉料装入承烧体进行烧结。烧结曲线采用分段设计，烧结温度1100°C~1200°C，烧结后材料形成需要的单相尖晶石结构。烧结粉体取得后，再进行微粉碎，形成小于5微米或者纳米级的颗粒，颗粒的大小可以根据特性需求确定，每个颗粒具有单相尖晶石结构。
第二步，第二相复合。
按要求比例把Ni(NO3)2、Fe(NO3)3溶液混合，并进行化学处理，使其能够在颗粒表面均匀排列。
使用处理后的混合溶液对单相颗粒进行包覆。再把包覆后的单相颗粒放入准备好的有机铵盐溶液，用NaOH滴定到要求的PH值，加热进行反应，在单相颗粒表面生第二相结构。反应完成后，用离心机分离出沉淀物，再次清洗，去除杂质和有机物等，得到第二相复合完成的颗粒。
第三步，成型烧结。
把第二相复合完成后的颗粒放入制浆容器内，按一定配比加入水，以及酒精、甲苯等有机溶剂，再和增塑剂混合，并加入一定量的消泡剂以利于后续工序生产。把制作好的浆料使用流延成型工艺制作成要求的生带，切割成需要大小，放入炉内进行烧结。烧结温度900°C～1300°C之间，配合合适的升温速度、降温速度和气氛条件。
烧结后的产品进行覆膜等后加工工艺，就得到了多相复合尖晶石柔性材料产品。按照该方法制造的柔性材料，具有高磁导率、低损耗的特点，而且具有宽的应用频率范围。产品具有柔韧性，可弯折，厚度小，可嵌入设备内部而不占用空间，满足当前产品轻量化、薄型化、小型化的发展趋势。
实施例
按照42mol%：22mol%：8mol%的比例称取Fe2O3、MnO、ZnO原料。称量好的原料加入球磨机进行混合，料：球：水为1:5:1。混合好的粉料烘干后，通过振磨机振磨20min。振磨后的粉料装入烧钵，使用钟罩炉烧结，烧结时长25hr，保温温度1150°C，保温气氛氧含量体积比为2.5vol%。烧结后的粉体使用球磨机粉碎，粉碎粒径1.5微米。粉碎粉末烘干供后续过程使用。
按照8mol%:1.5mol%的比例混合Fe(NO3)3、 Ni(NO3)2溶液。混合好的溶液与烘干后的粉碎粉末进行混合包覆。再将包覆颗粒放入有机铵盐溶液，用NaOH滴定到PH=10.5，放入反应釜加热至150°C反应8hr，反应过程中连续搅拌。反应完成后，用离心机分离沉淀物，清洗去除杂质和有机物，得到复合颗粒。
取10kg复合颗粒放入制浆容器内，加入一定量的增塑剂、酒精、水、分散剂和消泡剂，进行混合制浆。浆料完成后，使用流延成型机进行成型，流延速度800转/分，得到生带。生带切割后放入烧结炉烧结，烧结温度1200°C，保温时间2.5hr。
烧结后的产品再次进行后加工切割、覆膜等等，得到要求的柔性材料磁片。磁片具有良好的柔韧性，可弯折。磁片做成T18*6*0.1磁环测试性能，复数磁导率实部1507，复数磁导率虚部6.2。25°C饱和磁通密度506mT，截止频率3.5MHz。
Claims (4)
1.一种多相复合尖晶石柔性材料，其特征在于，主体具有多相尖晶石结构，柔韧性好，可弯折，弯折后特性不变。
2.如权利要求1所述的多相复合尖晶石柔性材料，制作工艺包括单相颗粒制作、第二相复合、成型烧结等步骤。
3. 如权利要求1所述的多相复合尖晶石柔性材料，作为主成分含有Fe2O3：40mol% ~65mol%，NiO：1mol%~10.0mol%，ZnO：2mol%~15mol%，MnO：2mol%~40mol%，CuO：1mol%~10mol%。
4.如权利要求1所述的多相复合尖晶石柔性材料，具有大于1000的复数磁导率实部，小于10的复数磁导率虚部，25°C饱和磁通密度大于500mT。
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