CN101269953A - 一组高饱和磁化强度软磁铁氧体及其制备方法 - Google Patents
一组高饱和磁化强度软磁铁氧体及其制备方法 Download PDFInfo
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Abstract
本发明是一组高饱和磁化强度软磁铁氧体及其制备方法。本发明的目的是针对现有软磁铁氧体材料及制备方法所存在的产品颗粒大、烧结温度高的不足之处,提供一种产品的颗粒小、烧结温度低的一组高饱和磁化强度软磁铁氧体及其制备方法。本发明的制备方法是:采用硝酸盐或氯化物或硫酸盐为原料,采用水杨酸、柠檬酸、苹果酸、酒石酸中的一种为鳌合剂,按配比称取原料和鳌合剂,经混合、研磨均匀后,加适量的乙醇溶剂调制成流变体,将流变体注入反应釜中进行反应,反应结束后,经冷却、抽滤、分别用去离子水和无水乙醇洗涤固相物,经干燥后得到的有机酸盐前驱物经预烧、焙烧后,冷却后得到一组高饱和磁化强度软磁铁氧体材料(钴锌铁氧体纳米粉体)。
Description
技术领域
本发明属于磁性材料技术领域,特别是一组高饱和磁化强度软磁铁氧体及其制备方法。
背景技术
铁氧体是一种具有铁磁性的金属复合氧化物,就其电磁特性来说,铁氧体的电阻率比金属、合金磁性材料大得多,而且还有较高的介电性能,其磁性能还表现在高频时具有较高的磁导率。因而,铁氧体已成为高频弱电领域用途广泛的非金属磁性材料。由于铁氧体单位体积中储存的磁能较低,饱合磁化强度也较低(通常只有纯铁的1/3~1/5),因而限制了它在要求较高磁能密度的低频强电和大功率领域的应用。
软磁铁氧体是一种用途广、产量大、成本低的基础材料,是电子、机电工业和信息产业重要的支柱产品之一,它的推广应用直接影响到电子信息、家电行业、计算机与通讯、环保及节能技术的发展。它主要用作各种电感元件,如滤波器磁芯、变压器磁芯、无线电磁芯、电磁铁、加速器高频加速腔、磁场探头、磁性基片、高频淬火聚能、电磁吸盘、磁带录音和录像磁头以及磁敏元件等,也是磁记录元件的关键材料。随着电子技术日益广泛的应用,特别是数字电路和开关电源的普及,电磁干扰(EMI)问题日益重要,以软磁铁氧体为基础的EMI磁性元件发展迅速,产品种类繁多,如电磁干扰抑制器、电波吸收材料、倍频器、调制器等,已成为现代军事电子设备、工业和民用电子仪器不可缺少的组成部分。
软磁铁氧体的磁性参数与其组成元素、结构、形状有关外,还与制备条件及方法有关。目前,软磁铁氧体材料的制备一般是采用共沉淀法、氧化物直接烧结法、直接球磨法和烧结法等,现有的软磁铁氧体材料及制备方法存在着产品的颗粒大(微米级),很难得到纳米级的产品,烧结温度高、烧结时间长,能耗大的不足之处。
发明内容
本发明的目的是针对现有的软磁铁氧体材料及制备方法所存在的产品的颗粒大、烧结温度高、烧结时间长、能耗大的不足之处,提供一种产品的颗粒小、烧结温度低、烧结时间短、能耗小的一组高饱和磁化强度软磁铁氧体及其制备方法。
本发明是通过以下的技术方案完成的:一组高饱和磁化强度软磁铁氧体及其制备方法,采用硝酸盐或氯化物或硫酸盐为原料,原料中的Co(钴)、Zn(锌)、Fe(铁)的物质的量比为Co∶Zn∶Fe=0.9~0.1∶0.1~0.9∶2.1~1.9;采用水杨酸、柠檬酸、苹果酸、酒石酸中的一种为鳌合剂,鳌合剂的物质的量是原料中过渡金属离子总的物质的量的1~3倍;按配比称取原料和鳌合剂,经混合、研磨均匀后,加适量的乙醇溶剂调制成似固非固、似液非液的流变体,乙醇溶剂由去离子水和无水乙醇配制而成,其中去离子水与无水乙醇之间的配比为1∶0.8~1.2(体积比);将流变体注入反应釜中,温度控制在60~80℃,反应16~24小时;反应结束后,冷却至10~30℃,抽滤,分别用去离子水和无水乙醇洗涤固相物2~3次,再于80~120℃干燥4~12小时,即得有机酸盐前驱物;将干燥过的有机酸盐前驱物在马弗炉中400~500℃预烧0.5~2小时,然后700~1200℃焙烧1~3小时,冷却后得到钴锌铁氧体纳米粉体,该钴锌铁氧体纳米粉体即是一组高饱和磁化强度软磁铁氧体材料。
在上述一组高饱和磁化强度软磁铁氧体材料的制备过程中,反应釜由不锈钢材料制成,在反应釜的内壁上衬聚四氟乙烯材料。
在本发明中,通过流变相反应产生的高压和空化作用使反应体系中固体微粒和液体物质成为混合均匀的流变体,固体微粒的表面可得到有效利用,能与流体接触紧密、均匀.由于体系的热交换良好,不会出现局部过热。本发明的软磁铁氧体制备方法,具有合成温度较低、醇水混合溶剂减弱了前驱物的软团聚作用,且前驱物在热分解过程中产生的气体可以阻止或延缓产物粒子的硬团聚;在前驱物热分解过程中,产生的过渡金属氧化物按尖晶石结构作有规则的排列在A位和B位,B位磁性离子的自旋平行增强了离子间的超交换作用,从而增大了样品的饱和磁化强度。
综上,本发明与现有的软磁铁氧体材料相比,具有产品的颗粒细、分布均匀的特点;本发明与现有的软磁铁氧体材料的制备方法相比,具有烧结温度低、烧结时间短、能耗小的特点。
具体实施方式
下面通过实施例对本发明的其制备方法作进一步说明,但本发明并不限于以下实施例。
实施例1
称取7 mmol Co(NO3)2·6H2O、3 mmol Zn(NO3)2·6H2O、20 mmol Fe(NO3)2·9H2O和40 mmol柠檬酸(C6H8O7·H2O),混合后研磨均匀,加入适量的混合溶剂变体(去离子水和无水乙醇按体积比1∶1混合)调制成流变体;将流变体转入内衬聚四氟乙烯的不锈钢反应釜中,在60~80℃反应16~24小时,随后冷却至25℃,抽滤,分别用去离子水和无水乙醇洗涤固相物2~3次,再于80~120℃干燥4~12小时,即得有机酸盐前驱物;将干燥过的有机酸盐前驱物在马弗炉中400~500℃预烧0.5~2小时,然后700~1200℃焙烧1~3小时,冷却后得到尖晶石型的钴锌铁氧体纳米粉体。经测定其化学组成与Co0.7Zn0.3Fe2O4相符合。
实施例2
称取9 mmol Co(NO3)2·6H2O、1 mmol Zn(NO3)2·6H2O、20 mmol Fe(NO3)2·9H2O和40 mmol柠檬酸(C6H8O7·H2O),混合后研磨均匀,加入适量的混合溶剂变体(去离子水和无水乙醇按体积比1∶1混合)调制成流变体;余下的步骤与实例1相同。经测定其化学组成与Co0.9Zn0.1Fe2O4相符合。
实施例3
称取5 mmol Co(NO3)2·6H2O、5 mmol Zn(NO3)2·6H2O、20 mmol Fe(NO3)2·9H2O和40 mmol柠檬酸(C6H8O7·H2O),混合后研磨均匀,加入适量的混合溶剂变体(去离子水和无水乙醇按体积比1∶1混合)调制成流变体;余下的步骤与实例1相同。经测定其化学组成与Co0.5Zn0.5Fe2O4相符合。
实施例4
称取3 mmol Co(NO3)2·6H2O、7 mmol Zn(NO3)2·6H2O、20 mmol Fe(NO3)2·9H2O和40 mmol柠檬酸(C6H8O7·H2O),混合后研磨均匀,加入适量的混合溶剂变体(去离子水和无水乙醇按体积比1∶1混合)调制成流变体;余下的步骤与实例1相同。经测定其化学组成与Co0.3Zn0.7Fe2O4相符合。
实施例5
称取1 mmol Co(NO3)2·6H2O、9 mmol Zn(NO3)2·6H2O、20 mmol Fe(NO3)2·9H2O和40 mmol柠檬酸(C6H8O7·H2O),混合后研磨均匀,加入适量的混合溶剂变体(去离子水和无水乙醇按体积比1∶1混合)调制成流变体;余下的步骤与实例1相同。经测定其化学组成与Co0.1Zn0.9Fe2O4相符合。
五个实例样品的饱和磁化强度和晶粒尺寸如下表所示:
样 品 | 饱和磁化强度(emu/g) | 晶粒尺寸(nm) |
Co0.9Zn0.1Fe2O4 | 78.42 | 25~45 |
Co0.7Zn0.3Fe2O4 | 96.14 | 25~45 |
Co0.5Zn0.5Fe2O4 | 67.26 | 25~45 |
Co0.3Zn0.7Fe2O4 | 51.94 | 25~45 |
Co0.1Zn0.9Fe2O4 | 45.27 | 25~45 |
Claims (4)
1、一组高饱和磁化强度软磁铁氧体及其制备方法,其特征在于一组高饱和磁化强度软磁铁氧体采用硝酸盐或氯化物或硫酸盐为原料,采用水杨酸、柠檬酸、苹果酸、酒石酸中的一种为鳌合剂,其中,原料中的Co(钴)、Zn(锌)、Fe(铁)的物质的量比为Co∶Zn∶Fe=0.9~0.1∶0.1~0.9∶2.1~1.9,鳌合剂的物质的量是原料中过渡金属离子总的物质的量的1~3倍。
2、根据权利要求1所述的一组高饱和磁化强度软磁铁氧体及其制备方法,其特征在于一组高饱和磁化强度软磁铁氧体的制备方法是:按配比称取原料和鳌合剂,经混合、研磨均匀后,加适量的乙醇溶剂调制成流变体,将流变体注入反应釜中,温度控制在60~80℃,反应16~24小时;反应结束后,冷却至10~30℃,抽滤,分别用去离子水和无水乙醇洗涤固相物2~3次,再于80~120℃干燥4~12小时,即得有机酸盐前驱物;将干燥过的有机酸盐前驱物在马弗炉中400~500℃预烧0.5~2小时,然后700~1200℃焙烧1~3小时,冷却后得到钴锌铁氧体纳米粉体,该钴锌铁氧体纳米粉体即是一组高饱和磁化强度软磁铁氧体材料。
3、根据权利要求2所述的一组高饱和磁化强度软磁铁氧体及其制备方法,其特征在于在一组高饱和磁化强度软磁铁氧体的制备方法中,乙醇溶剂由去离子水和无水乙醇配制而成,其中去离子水与无水乙醇之间的配比为1∶0.8~1.2(体积比)。
4、根据权利要求2所述的一组高饱和磁化强度软磁铁氧体及其制备方法,其特征在于在一组高饱和磁化强度软磁铁氧体材料的制备方法中,反应釜由不锈钢材料制成,在反应釜的内壁上衬聚四氟乙烯材料。
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Cited By (4)
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CN101372417B (zh) * | 2008-09-25 | 2011-08-10 | 中国科学院青海盐湖研究所 | 高比饱和磁化强度和高矫顽力锶铁氧体磁粉及其制备方法 |
US8123973B2 (en) * | 2008-12-10 | 2012-02-28 | Cheng Uei Precision Industry Co. | Method of manufacturing magnetic material |
CN104882240A (zh) * | 2015-05-14 | 2015-09-02 | 江苏有能新能源有限公司 | 一种光伏逆变器用磁性材料及其制备方法 |
CN104891981A (zh) * | 2015-05-14 | 2015-09-09 | 江苏有能新能源有限公司 | 一种岸基变频电源专用磁性材料及其制备方法 |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101372417B (zh) * | 2008-09-25 | 2011-08-10 | 中国科学院青海盐湖研究所 | 高比饱和磁化强度和高矫顽力锶铁氧体磁粉及其制备方法 |
US8123973B2 (en) * | 2008-12-10 | 2012-02-28 | Cheng Uei Precision Industry Co. | Method of manufacturing magnetic material |
CN104882240A (zh) * | 2015-05-14 | 2015-09-02 | 江苏有能新能源有限公司 | 一种光伏逆变器用磁性材料及其制备方法 |
CN104891981A (zh) * | 2015-05-14 | 2015-09-09 | 江苏有能新能源有限公司 | 一种岸基变频电源专用磁性材料及其制备方法 |
CN104882240B (zh) * | 2015-05-14 | 2017-11-14 | 江苏有能新能源有限公司 | 一种光伏逆变器用磁性材料及其制备方法 |
CN104891981B (zh) * | 2015-05-14 | 2017-11-14 | 江苏有能新能源有限公司 | 一种岸基变频电源专用磁性材料及其制备方法 |
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