CN106699160A - 一种锰锌软磁铁氧体材料的制备方法 - Google Patents

一种锰锌软磁铁氧体材料的制备方法 Download PDF

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CN106699160A
CN106699160A CN201611211644.0A CN201611211644A CN106699160A CN 106699160 A CN106699160 A CN 106699160A CN 201611211644 A CN201611211644 A CN 201611211644A CN 106699160 A CN106699160 A CN 106699160A
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soft magnetic
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宋昊
李雪晴
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TRUSYN CHEM-TECH Co Ltd
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Abstract

本发明公开了一种锰锌软磁铁氧体材料的制备方法，属于软磁铁氧体的技术领域。本发明本发明将氧化铁、碳酸锰、盐酸等放入球磨机球磨，收集球磨混合物在干燥箱中干燥，随后放入粉碎机中粉碎，得过筛颗粒，并与三乙醇胺、钛酸正丁酯等搅拌均匀，接着将混合物进行煅烧，再将煅烧物与碳酸锶、五氧化二铌、氧化钙和硼化锆做球磨处理，随后放入电炉中熔融、碾磨，将碾磨混合物与聚乙烯醇溶液混合均匀，再进行喷雾干燥，将干燥物放入模具中并置于压机下压制成型，放入煅烧炉煅烧，收集煅烧物，即可得锰锌软磁铁氧体材料。本发明制备的锰锌软磁铁氧体具有较高的纯度，且性能稳定。

Description

一种锰锌软磁铁氧体材料的制备方法
技术领域
本发明公开了一种锰锌软磁铁氧体材料的制备方法，属于软磁铁氧体的技术领域。
背景技术
软磁铁氧体材料是一种在较弱的磁场作用下，很容易被磁化和退磁的铁氧体材料。作为发展早、种类多、用途广泛的材料，软磁铁氧体已经成为经济发展中较为重要的产品之一。近年来，随着计算机网络技术、通信技术和电力技术等电子信息技术的发展，传统领域对性能优良的软磁铁氧体材料的需求不断增加，应用也不断延伸至其它的领域，也已成为各种通信设备、计算机、家用电器、汽车电子、电源装置、仪器仪表、航天工业等不可缺少的一种基础材料。
目前，应用较为广泛的软磁铁氧体材料可以分为锰锌系铁氧体、镍锌系铁氧体和甚高频铁氧体等三大类，其中锰锌系铁氧体根据应用条件和性能指标的不同，可以被分为两大类：其中一种为高磁导率铁氧体，通常应用于通信与控制设备、民用电器和电子产品等的低频和宽频变压器以及电感元件中；另一种为高频率低损耗铁氧体，其最开始被应用于电视机、收音机、开关电源等设备的回扫和功率变压器中，并逐步发展到应用于电脑设备的适配变压器以及各类设备的高频变压器中。
现如今制备锰锌软磁铁氧体的方法主要有氧化物法和鲁氏纳法。其中氧化物法也称陶瓷工艺，它是以金属的氧化物Fe2O3、Mn3O4、ZnO等为原料，经混合、粗磨、预烧、细磨和造粒、成型烧结等工艺来生产软磁铁氧体材料的。由于该种工艺采用的是固体原料，三种原料的物性相差较大，因而很难混合均匀，导致生产的软磁铁氧体材料性能不稳定，成本高，而且生产过程中还有一定的粉尘污染。鲁氏纳法是以钢铁厂的盐酸废酸洗液FeCl2、MnCl2和ZnCl2为原料，通过喷头雾化后进入高温反应器，使溶液中的水份挥发掉，FeCl2、MnCl2和ZnCl2在高温下直接氧化成MnO·ZnO·Fe2O3，而挥发的Cl2采用水吸收法可以回收成盐酸重新利用，但是该方法的生产设备结构复杂，投资巨大，配套设备多，污染严重。
发明内容
本发明所要解决的技术问题：针对目前锰锌软磁铁氧体在制备过程中原料的物性相差较大，难混合均匀，导致软磁铁氧体材料性能不稳定，同时制备过程中原料易挥发，对环境造成污染的问题，本发明通过盐酸对原料进行溶解，通过硅烷偶联剂将游离的金属离子结合，促使物料充分混合，再使用钛酸正丁酯、三氧化二铬作为辅助剂，在煅烧过程中促进晶粒的生长，提高活性，随后添加氧化钙、碳酸锶等物质，降低烧结温度，促进材料中晶粒的长大，使晶力分布均匀，促使材料致密化，抑制了物料挥发，提高晶粒内部电阻率，从而制备的锰锌软磁铁氧体材料。本发明将氧化铁、碳酸锰、盐酸等放入球磨机球磨，收集球磨混合物在干燥箱中干燥，随后放入粉碎机中粉碎，得过筛颗粒，并与三乙醇胺、钛酸正丁酯等搅拌均匀，接着将混合物进行煅烧，再将煅烧物与碳酸锶、五氧化二铌、氧化钙和硼化锆做球磨处理，随后放入电炉中熔融、碾磨，将碾磨混合物与聚乙烯醇溶液混合均匀，再进行喷雾干燥，将干燥物放入模具中并置于压机下压制成型，放入煅烧炉煅烧，收集煅烧物，即可得锰锌软磁铁氧体材料。本发明制备的锰锌软磁铁氧体具有较高的纯度，且性能稳定。
为解决上述技术问题，本发明采用如下所述的技术方案是：
（1）按重量份数计，取50～60份氧化铁、20～24份碳酸锰、19～24份质量分数为3％的盐酸、10～13份氧化锌及3～7份γ-氨丙基三乙氧基硅烷，放入球磨机中，按球料比10:1，以200r/min球磨4～6h，收集球磨混合物，并放入100℃干燥箱中干燥10～12h，收集干燥物；
（2）将上述干燥物放入粉碎机中进行粉碎，过80目筛，收集过筛颗粒，将过筛颗粒、过筛颗粒质量7～9％的三乙醇胺、过筛颗粒质量3～5％的钛酸正丁酯及过筛颗粒质量1～2％的三氧化二铬，放入搅拌机中搅拌均匀，随后将搅拌混合物放入煅烧炉中，设定温度为800～900℃，煅烧1～2h，随炉冷却至室温，收集煅烧物；
（3）按重量份数计，取60～65份上述煅烧物、3～4份碳酸锶、2～4份五氧化二铌、1～3份氧化钙及0.9～1.2份硼化锆放入球磨机中，以300r/min球磨30～40min，将球磨混合物放入电炉中，使用氩气进行保护，设定温度为1100～1200℃，保温30～40min；
（4）在上述保温结束后，收集电炉中的混合物放入碾磨机中以400r/min碾磨20～25min，收集碾磨混合物，将碾磨混合物与其质量1～2倍的质量分数为5％聚乙烯醇溶液混合均匀，再进行喷雾干燥，收集干燥物，将干燥物放入模具中，并将模具置于压机中，在40～45℃，0.9～1.2GPa下压制成型，收集模具中的坯体，放入煅烧炉中，使用氦气保护，设定温度为980～1200℃，煅烧2～3h，随后以8℃/min降温至室温，收集煅烧物，即可得锰锌软磁铁氧体材料。
经检测本发明所制得的锰锌软磁铁氧体材料得：饱和兹感应强度为520～600mT，电阻率为103～109Ω·m，居里温度为580～820℃，磁导率为115～130mH/m，耗损率为100～150kw/m3。
本发明与其他方法相比，有益技术效果是：
（1）本发明所得的锰锌软磁铁氧体材料具有较高的初始磁导率，同时具有良好的温度特性、频率特性、低的损耗、高的阻抗和良好的叠加性能；
（2）本发明所得的锰锌软磁铁氧体材料的具有较高的电阻率，高的机加工性能，易于模压成型，化学稳定性好，同时制备工艺简单，成本低，操作方便。
具体实施方式
按重量份数计，取50～60份氧化铁、20～24份碳酸锰、19～24份质量分数为3％的盐酸、10～13份氧化锌及3～7份γ-氨丙基三乙氧基硅烷，放入球磨机中，按球料比10:1，以200r/min球磨4～6h，收集球磨混合物，并放入100℃干燥箱中干燥10～12h，收集干燥物；将上述干燥物放入粉碎机中进行粉碎，过80目筛，收集过筛颗粒，将过筛颗粒、过筛颗粒质量7～9％的三乙醇胺、过筛颗粒质量3～5％的钛酸正丁酯及过筛颗粒质量1～2％的三氧化二铬，放入搅拌机中搅拌均匀，随后将搅拌混合物放入煅烧炉中，设定温度为800～900℃，煅烧1～2h，随炉冷却至室温，收集煅烧物；按重量份数计，取60～65份上述煅烧物、3～4份碳酸锶、2～4份五氧化二铌、1～3份氧化钙及0.9～1.2份硼化锆放入球磨机中，以300r/min球磨30～40min，将球磨混合物放入电炉中，使用氩气进行保护，设定温度为1100～1200℃，保温30～40min；在上述保温结束后，收集电炉中的混合物放入碾磨机中以400r/min碾磨20～25min，收集碾磨混合物，将碾磨混合物与其质量1～2倍的质量分数为5％聚乙烯醇溶液混合均匀，再进行喷雾干燥，收集干燥物，将干燥物放入模具中，并将模具置于压机中，在40～45℃，0.9～1.2GPa下压制成型，收集模具中的坯体，放入煅烧炉中，使用氦气保护，设定温度为980～1200℃，煅烧2～3h，随后以8℃/min降温至室温，收集煅烧物，即可得锰锌软磁铁氧体材料。
实例1
按重量份数计，取50份氧化铁、20份碳酸锰、19份质量分数为3％的盐酸、10份氧化锌及3份γ-氨丙基三乙氧基硅烷，放入球磨机中，按球料比10:1，以200r/min球磨4h，收集球磨混合物，并放入100℃干燥箱中干燥10h，收集干燥物；将上述干燥物放入粉碎机中进行粉碎，过80目筛，收集过筛颗粒，将过筛颗粒、过筛颗粒质量7％的三乙醇胺、过筛颗粒质量3％的钛酸正丁酯及过筛颗粒质量1％的三氧化二铬，放入搅拌机中搅拌均匀，随后将搅拌混合物放入煅烧炉中，设定温度为800℃，煅烧1h，随炉冷却至室温，收集煅烧物；按重量份数计，取60份上述煅烧物、3份碳酸锶、2份五氧化二铌、1份氧化钙及0.9份硼化锆放入球磨机中，以300r/min球磨30min，将球磨混合物放入电炉中，使用氩气进行保护，设定温度为1100℃，保温30min；在上述保温结束后，收集电炉中的混合物放入碾磨机中以400r/min碾磨20min，收集碾磨混合物，将碾磨混合物与其质量1倍的质量分数为5％聚乙烯醇溶液混合均匀，再进行喷雾干燥，收集干燥物，将干燥物放入模具中，并将模具置于压机中，在40℃，0.9GPa下压制成型，收集模具中的坯体，放入煅烧炉中，使用氦气保护，设定温度为980℃，煅烧2h，随后以8℃/min降温至室温，收集煅烧物，即可得锰锌软磁铁氧体材料。
经检测本发明所制得的锰锌软磁铁氧体材料得：饱和兹感应强度为520mT，电阻率为103Ω·m，居里温度为580℃，磁导率为115mH/m，耗损率为100kw/m3。
实例2
按重量份数计，取60份氧化铁、24份碳酸锰、24份质量分数为3％的盐酸、13份氧化锌及7份γ-氨丙基三乙氧基硅烷，放入球磨机中，按球料比10:1，以200r/min球磨6h，收集球磨混合物，并放入100℃干燥箱中干燥12h，收集干燥物；将上述干燥物放入粉碎机中进行粉碎，过80目筛，收集过筛颗粒，将过筛颗粒、过筛颗粒质量9％的三乙醇胺、过筛颗粒质量5％的钛酸正丁酯及过筛颗粒质量2％的三氧化二铬，放入搅拌机中搅拌均匀，随后将搅拌混合物放入煅烧炉中，设定温度为900℃，煅烧2h，随炉冷却至室温，收集煅烧物；按重量份数计，取65份上述煅烧物、4份碳酸锶、4份五氧化二铌、3份氧化钙及1.2份硼化锆放入球磨机中，以300r/min球磨40min，将球磨混合物放入电炉中，使用氩气进行保护，设定温度为1200℃，保温40min；在上述保温结束后，收集电炉中的混合物放入碾磨机中以400r/min碾磨25min，收集碾磨混合物，将碾磨混合物与其质量2倍的质量分数为5％聚乙烯醇溶液混合均匀，再进行喷雾干燥，收集干燥物，将干燥物放入模具中，并将模具置于压机中，在45℃，1.2GPa下压制成型，收集模具中的坯体，放入煅烧炉中，使用氦气保护，设定温度为1200℃，煅烧3h，随后以8℃/min降温至室温，收集煅烧物，即可得锰锌软磁铁氧体材料。
经检测本发明所制得的锰锌软磁铁氧体材料得：饱和兹感应强度为600mT，电阻率为109Ω·m，居里温度为820℃，磁导率为130mH/m，耗损率为150kw/m3。
实例3
按重量份数计，取55份氧化铁、22份碳酸锰、22份质量分数为3％的盐酸、12份氧化锌及5份γ-氨丙基三乙氧基硅烷，放入球磨机中，按球料比10:1，以200r/min球磨5h，收集球磨混合物，并放入100℃干燥箱中干燥11h，收集干燥物；将上述干燥物放入粉碎机中进行粉碎，过80目筛，收集过筛颗粒，将过筛颗粒、过筛颗粒质量8％的三乙醇胺、过筛颗粒质量4％的钛酸正丁酯及过筛颗粒质量2％的三氧化二铬，放入搅拌机中搅拌均匀，随后将搅拌混合物放入煅烧炉中，设定温度为850℃，煅烧2h，随炉冷却至室温，收集煅烧物；按重量份数计，取63份上述煅烧物、3份碳酸锶、3份五氧化二铌、2份氧化钙及1.1份硼化锆放入球磨机中，以300r/min球磨35min，将球磨混合物放入电炉中，使用氩气进行保护，设定温度为1150℃，保温35min；在上述保温结束后，收集电炉中的混合物放入碾磨机中以400r/min碾磨22min，收集碾磨混合物，将碾磨混合物与其质量2倍的质量分数为5％聚乙烯醇溶液混合均匀，再进行喷雾干燥，收集干燥物，将干燥物放入模具中，并将模具置于压机中，在43℃，1.1GPa下压制成型，收集模具中的坯体，放入煅烧炉中，使用氦气保护，设定温度为1090℃，煅烧2h，随后以8℃/min降温至室温，收集煅烧物，即可得锰锌软磁铁氧体材料。
经检测本发明所制得的锰锌软磁铁氧体材料得：饱和兹感应强度为570mT，电阻率为106Ω·m，居里温度为680℃，磁导率为123mH/m，耗损率为130kw/m3。

Claims (1)

1.一种锰锌软磁铁氧体材料的制备方法，其特征在于具体制备步骤为：
（1）按重量份数计，取50～60份氧化铁、20～24份碳酸锰、19～24份质量分数为3％的盐酸、10～13份氧化锌及3～7份γ-氨丙基三乙氧基硅烷，放入球磨机中，按球料比10:1，以200r/min球磨4～6h，收集球磨混合物，并放入100℃干燥箱中干燥10～12h，收集干燥物；
（2）将上述干燥物放入粉碎机中进行粉碎，过80目筛，收集过筛颗粒，将过筛颗粒、过筛颗粒质量7～9％的三乙醇胺、过筛颗粒质量3～5％的钛酸正丁酯及过筛颗粒质量1～2％的三氧化二铬，放入搅拌机中搅拌均匀，随后将搅拌混合物放入煅烧炉中，设定温度为800～900℃，煅烧1～2h，随炉冷却至室温，收集煅烧物；
（3）按重量份数计，取60～65份上述煅烧物、3～4份碳酸锶、2～4份五氧化二铌、1～3份氧化钙及0.9～1.2份硼化锆放入球磨机中，以300r/min球磨30～40min，将球磨混合物放入电炉中，使用氩气进行保护，设定温度为1100～1200℃，保温30～40min；
（4）在上述保温结束后，收集电炉中的混合物放入碾磨机中以400r/min碾磨20～25min，收集碾磨混合物，将碾磨混合物与其质量1～2倍的质量分数为5％聚乙烯醇溶液混合均匀，再进行喷雾干燥，收集干燥物，将干燥物放入模具中，并将模具置于压机中，在40～45℃，0.9～1.2GPa下压制成型，收集模具中的坯体，放入煅烧炉中，使用氦气保护，设定温度为980～1200℃，煅烧2～3h，随后以8℃/min降温至室温，收集煅烧物，即可得锰锌软磁铁氧体材料。
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