CN111517776A - 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 PDFInfo
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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,属于锰锌软磁铁氧体材料加工制造技术领域,包括如下步骤:(1)主体体系原料称取、(2)掺杂体系原料称取、(3)一次预烧处理、(4)共混研磨处理、(5)浆料制备、(6)坯块制备、(7)二次预烧处理、(8)球磨处理、(9)烧结成型。本发明方法整体工艺简单,各步骤搭配合理,成本较低,便于推广应用,制得的锰锌软磁铁氧体具有较好的宽温性、较低的功率损耗以及优异的饱和磁通密度。
Description
技术领域
本发明属于锰锌软磁铁氧体材料加工制造技术领域,具体涉及一种锰锌软磁铁氧体材料的制备方法。
背景技术
软磁材料在工业中的应用是伴随着电力电工及电讯技术的兴起而出现的,最早应用始于十九世纪末。软磁材料可应用于家电领域、信息化领域、汽车领域和其他配套领域。随着现代电子技术的快速发展,软磁材料中的高磁导率锰锌铁氧体得到飞速发展,应用范围由原来的脉冲变压器逐步扩大到电磁滤波器、扼流圈、感应器等领域,应用领域越来越广,其市场需求量逐年上升,产品种类也日益增多,成为磁性材料行业发展的一大亮点。
随着铁氧体材料应用范围的扩大及电子设备的发展,对铁氧体材料的性能要求也越来越高,如频率稳定性、温度稳定性、时间稳定性等,以满足电子行业发展的需求及应用环境变化对产品适应性能的挑战。
发明内容
本发明的目的是提供一种锰锌软磁铁氧体材料的制备方法,制得的锰锌软磁铁氧体具有低损耗、使用稳定性高的特性。
本发明的上述技术目的是通过以下技术方案实现的:
一种锰锌软磁铁氧体材料的制备方法,包括如下步骤:
(1)主体体系原料称取:
以摩尔百分比计称取52~56%的精铁矿粉、33~37%的Mn3O4、余量的ZnO;
(2)掺杂体系原料称取:
以质量百分比计称取17~20%的CaCO3、6~9%的ZrO2、2~4%的MoO3、7~10%的Bi2O3、30~35%的CaO、2~5%的SnO、5~8%的的TiO2、1~2%的La2O3、0.5~1.5%的Y2O3、余量的石墨烯;
(3)一次预烧处理:
将步骤(1)称取的所有主体体系原料共同混合后,再对其进行一次预烧处理,完成后得一次预烧料备用;
(4)共混研磨处理:
将步骤(2)称取的所有掺杂体系原料与步骤(3)所得的一次预烧料进行共混研磨,持续研磨处理2~3h后得研磨料备用;
(5)浆料制备:
将步骤(4)所得的研磨料与分散剂溶液、去离子水共混,然后进行高速搅拌处理,25~30min后制得浆料备用;
(6)坯块制备:
对步骤(5)所得的浆料进行压滤制成坯块,然后再将其置于恒温干燥箱内干燥2~3h后取出备用;
(7)二次预烧处理:
对步骤(6)所得的坯块进行二次预烧处理,完成后得二次预烧料备用;
(8)球磨处理:
对步骤(7)所得的二次预烧料进行球磨处理,50~70min后取出得球磨料备用;
(9)烧结成型:
对步骤(8)所得的球磨料进行干压成型,然后对其进行高温烧结处理,最后取出自然冷却至室温后即可。
进一步的,步骤(3)中所述的一次预烧处理时控制温度为1050~1100℃、时长为2~4h。
进一步的,步骤(4)中所述的掺杂体系原料与一次预烧料对应的质量比为1:35~40;所述的研磨处理时控制研磨的转速为340~380转/分钟。
进一步的,步骤(5)中所述的分散剂溶液为质量分数为14~18%的PVA溶液;所述的研磨料、分散剂溶液、去离子水对应的重量比为90~100:2~5:40~45;所述高速搅拌处理时控制搅拌的转速为1500~1800转/分钟。
进一步的,步骤(6)中所述的恒温干燥箱内的干燥温度为90~95℃。
进一步的,步骤(7)中所述的二次预烧处理时具体工艺为:控制环境氧气含量为0.12~0.16%,先于980~1020℃的温度下加热保温处理35~45min,然后再于1200~1260℃的温度下加热保温处理1.5~2.5h,最后停止加热随炉冷却至室温即可。
进一步的,步骤(8)中所述的球磨处理时控制球磨的转速为700~780转/分钟。
进一步的,步骤(9)中所述的高温烧结处理时具体工艺为:控制环境氧气含量为0.18~0.23%,先于1250~1350℃的温度下加热保温处理35~45min,然后停止加热随炉冷却至室温即可。
本发明相比现有技术具有以下优点:
本发明提供了一种锰锌软磁铁氧体材料的制备方法,优化改善了传统工艺方法,有效的提升了材料的品质;在制备过程中以主体体系原料和掺杂体系原料进行复配制备,尤其是在掺杂体系原料中添加了La2O3、Y2O3及石墨烯成分,其中添加的镧离子能够在锰锌铁氧体晶界间偏析,与硅等形成了阻挡层,从而能够提高晶界的电阻率,并且钇离子能够与二氧化钛共同在晶界处形成复合钛型高阻层,同时石墨烯颗粒能够固定于晶界间,稳固在二价铁离子处,形成一个静电阻,提升了整体的反应活性,改善了铁氧体的宽温性能;最终上述成分配合掺杂体系原料成分及主体体系原料成分,有效的提升了铁氧体材料的饱和磁通密度、优化了功率损耗特性、增强了使用的稳定性及寿命。本发明方法整体工艺简单,各步骤搭配合理,成本较低,便于推广应用,制得的锰锌软磁铁氧体具有较好的宽温性、较低的功率损耗以及优异的饱和磁通密度,极具市场竞争力。
具体实施方式
下面对本发明的较佳实施例进行详细阐述,以使本发明的优点和特性能够易于被本领域技术人员理解,从而对本发明的保护范围做出更为清楚明确的界定。
实施例1
一种锰锌软磁铁氧体材料的制备方法,包括如下步骤:
(1)主体体系原料称取:
以摩尔百分比计称取52%的精铁矿粉、33%的Mn3O4、余量的ZnO;
(2)掺杂体系原料称取:
以质量百分比计称取17%的CaCO3、6%的ZrO2、2%的MoO3、7%的Bi2O3、30%的CaO、2%的SnO、5%的的TiO2、1%的La2O3、0.5%的Y2O3、余量的石墨烯;
(3)一次预烧处理:
将步骤(1)称取的所有主体体系原料共同混合后,再对其进行一次预烧处理,完成后得一次预烧料备用;预烧处理时控制温度为1050℃、时长为2h;
(4)共混研磨处理:
将步骤(2)称取的所有掺杂体系原料与步骤(3)所得的一次预烧料进行共混研磨,持续研磨处理2h后得研磨料备用;所述的掺杂体系原料与一次预烧料对应的质量比为1:35;所述的研磨处理时控制研磨的转速为340转/分钟;
(5)浆料制备:
将步骤(4)所得的研磨料与分散剂溶液、去离子水共混,然后进行高速搅拌处理,25min后制得浆料备用;所述的分散剂溶液为质量分数为14%的PVA溶液;所述的研磨料、分散剂溶液、去离子水对应的重量比为90:2:40;所述高速搅拌处理时控制搅拌的转速为1500转/分钟;
(6)坯块制备:
对步骤(5)所得的浆料进行压滤制成坯块,然后再将其置于恒温干燥箱内干燥2h后取出备用;所述的恒温干燥箱内的干燥温度为90℃;
(7)二次预烧处理:
对步骤(6)所得的坯块进行二次预烧处理,完成后得二次预烧料备用;所述的二次预烧处理时具体工艺为:控制环境氧气含量为0.12%,先于980℃的温度下加热保温处理35min,然后再于1200℃的温度下加热保温处理1.5h,最后停止加热随炉冷却至室温即可;
(8)球磨处理:
对步骤(7)所得的二次预烧料进行球磨处理,50min后取出得球磨料备用;所述的球磨处理时控制球磨的转速为700转/分钟;
(9)烧结成型:
对步骤(8)所得的球磨料进行干压成型,然后对其进行高温烧结处理,最后取出自然冷却至室温后即可;所述的高温烧结处理时具体工艺为:控制环境氧气含量为0.18%,先于1250℃的温度下加热保温处理35min,然后停止加热随炉冷却至室温即可。
对本发明实施例1制得的锰锌软磁铁氧体材料进行检测发现,其在25℃时的饱和磁通密度为1100~1240mT,100℃时的饱和磁通密度为1060~1220mT;于100℃、100kHz、200mT条件下的功率损耗不大于160kW/m3。可见本发明方法制得的锰锌软磁铁氧体材料具有良好的宽温性和较低的功率损耗,以及优异的饱和磁通密度特性。
实施例2
一种锰锌软磁铁氧体材料的制备方法,包括如下步骤:
(1)主体体系原料称取:
以摩尔百分比计称取54%的精铁矿粉、36%的Mn3O4、余量的ZnO;
(2)掺杂体系原料称取:
以质量百分比计称取19%的CaCO3、8%的ZrO2、3%的MoO3、9%的Bi2O3、32%的CaO、4%的SnO、7%的的TiO2、1.5%的La2O3、1%的Y2O3、余量的石墨烯;
(3)一次预烧处理:
将步骤(1)称取的所有主体体系原料共同混合后,再对其进行一次预烧处理,完成后得一次预烧料备用;预烧处理时控制温度为1080℃、时长为3h;
(4)共混研磨处理:
将步骤(2)称取的所有掺杂体系原料与步骤(3)所得的一次预烧料进行共混研磨,持续研磨处理2.5h后得研磨料备用;所述的掺杂体系原料与一次预烧料对应的质量比为1:38;所述的研磨处理时控制研磨的转速为360转/分钟;
(5)浆料制备:
将步骤(4)所得的研磨料与分散剂溶液、去离子水共混,然后进行高速搅拌处理,27min后制得浆料备用;所述的分散剂溶液为质量分数为16%的PVA溶液;所述的研磨料、分散剂溶液、去离子水对应的重量比为95:4:42;所述高速搅拌处理时控制搅拌的转速为1700转/分钟;
(6)坯块制备:
对步骤(5)所得的浆料进行压滤制成坯块,然后再将其置于恒温干燥箱内干燥2.6h后取出备用;所述的恒温干燥箱内的干燥温度为92℃;
(7)二次预烧处理:
对步骤(6)所得的坯块进行二次预烧处理,完成后得二次预烧料备用;所述的二次预烧处理时具体工艺为:控制环境氧气含量为0.14%,先于1000℃的温度下加热保温处理40min,然后再于1230℃的温度下加热保温处理2h,最后停止加热随炉冷却至室温即可;
(8)球磨处理:
对步骤(7)所得的二次预烧料进行球磨处理,60min后取出得球磨料备用;所述的球磨处理时控制球磨的转速为740转/分钟;
(9)烧结成型:
对步骤(8)所得的球磨料进行干压成型,然后对其进行高温烧结处理,最后取出自然冷却至室温后即可;所述的高温烧结处理时具体工艺为:控制环境氧气含量为0.20%,先于1300℃的温度下加热保温处理40min,然后停止加热随炉冷却至室温即可。
对本发明实施例2制得的锰锌软磁铁氧体材料进行检测发现,其在25℃时的饱和磁通密度为1130~1280mT,100℃时的饱和磁通密度为1100~1270mT;于100℃、300kHz、200mT条件下的功率损耗不大于150kW/m3。可见本发明方法制得的锰锌软磁铁氧体材料具有良好的宽温性和较低的功率损耗,以及优异的饱和磁通密度特性。
实施例3
一种锰锌软磁铁氧体材料的制备方法,包括如下步骤:
(1)主体体系原料称取:
以摩尔百分比计称取56%的精铁矿粉、37%的Mn3O4、余量的ZnO;
(2)掺杂体系原料称取:
以质量百分比计称取20%的CaCO3、9%的ZrO2、4%的MoO3、10%的Bi2O3、35%的CaO、5%的SnO、8%的的TiO2、2%的La2O3、1.5%的Y2O3、余量的石墨烯;
(3)一次预烧处理:
将步骤(1)称取的所有主体体系原料共同混合后,再对其进行一次预烧处理,完成后得一次预烧料备用;预烧处理时控制温度为1100℃、时长为4h;
(4)共混研磨处理:
将步骤(2)称取的所有掺杂体系原料与步骤(3)所得的一次预烧料进行共混研磨,持续研磨处理3h后得研磨料备用;所述的掺杂体系原料与一次预烧料对应的质量比为1:40;所述的研磨处理时控制研磨的转速为380转/分钟;
(5)浆料制备:
将步骤(4)所得的研磨料与分散剂溶液、去离子水共混,然后进行高速搅拌处理,30min后制得浆料备用;所述的分散剂溶液为质量分数为18%的PVA溶液;所述的研磨料、分散剂溶液、去离子水对应的重量比为100:5:45;所述高速搅拌处理时控制搅拌的转速为1800转/分钟;
(6)坯块制备:
对步骤(5)所得的浆料进行压滤制成坯块,然后再将其置于恒温干燥箱内干燥3h后取出备用;所述的恒温干燥箱内的干燥温度为95℃;
(7)二次预烧处理:
对步骤(6)所得的坯块进行二次预烧处理,完成后得二次预烧料备用;所述的二次预烧处理时具体工艺为:控制环境氧气含量为0.16%,先于1020℃的温度下加热保温处理45min,然后再于1260℃的温度下加热保温处理2.5h,最后停止加热随炉冷却至室温即可;
(8)球磨处理:
对步骤(7)所得的二次预烧料进行球磨处理,70min后取出得球磨料备用;所述的球磨处理时控制球磨的转速为780转/分钟;
(9)烧结成型:
对步骤(8)所得的球磨料进行干压成型,然后对其进行高温烧结处理,最后取出自然冷却至室温后即可;所述的高温烧结处理时具体工艺为:控制环境氧气含量为0.23%,先于1350℃的温度下加热保温处理45min,然后停止加热随炉冷却至室温即可。
对本发明实施例3制得的锰锌软磁铁氧体材料进行检测发现,其在25℃时的饱和磁通密度为1120~1260mT,100℃时的饱和磁通密度为1090~1250mT;于100℃、500kHz、200mT条件下的功率损耗不大于160kW/m3。可见本发明方法制得的锰锌软磁铁氧体材料具有良好的宽温性和较低的功率损耗,以及优异的饱和磁通密度特性。
Claims (8)
1.一种锰锌软磁铁氧体材料的制备方法,其特征在于,包括如下步骤:
(1)主体体系原料称取:
以摩尔百分比计称取52~56%的精铁矿粉、33~37%的Mn3O4、余量的ZnO;
(2)掺杂体系原料称取:
以质量百分比计称取17~20%的CaCO3、6~9%的ZrO2、2~4%的MoO3、7~10%的Bi2O3、30~35%的CaO、2~5%的SnO、5~8%的的TiO2、1~2%的La2O3、0.5~1.5%的Y2O3、余量的石墨烯;
(3)一次预烧处理:
将步骤(1)称取的所有主体体系原料共同混合后,再对其进行一次预烧处理,完成后得一次预烧料备用;
(4)共混研磨处理:
将步骤(2)称取的所有掺杂体系原料与步骤(3)所得的一次预烧料进行共混研磨,持续研磨处理2~3h后得研磨料备用;
(5)浆料制备:
将步骤(4)所得的研磨料与分散剂溶液、去离子水共混,然后进行高速搅拌处理,25~30min后制得浆料备用;
(6)坯块制备:
对步骤(5)所得的浆料进行压滤制成坯块,然后再将其置于恒温干燥箱内干燥2~3h后取出备用;
(7)二次预烧处理:
对步骤(6)所得的坯块进行二次预烧处理,完成后得二次预烧料备用;
(8)球磨处理:
对步骤(7)所得的二次预烧料进行球磨处理,50~70min后取出得球磨料备用;
(9)烧结成型:
对步骤(8)所得的球磨料进行干压成型,然后对其进行高温烧结处理,最后取出自然冷却至室温后即可。
2.根据权利要求1所述的一种锰锌软磁铁氧体材料的制备方法,其特征在于,步骤(3)中所述的一次预烧处理时控制温度为1050~1100℃、时长为2~4h。
3.根据权利要求1所述的一种锰锌软磁铁氧体材料的制备方法,其特征在于,步骤(4)中所述的掺杂体系原料与一次预烧料对应的质量比为1:35~40;所述的研磨处理时控制研磨的转速为340~380转/分钟。
4.根据权利要求1所述的一种锰锌软磁铁氧体材料的制备方法,其特征在于,步骤(5)中所述的分散剂溶液为质量分数为14~18%的PVA溶液;所述的研磨料、分散剂溶液、去离子水对应的重量比为90~100:2~5:40~45;所述高速搅拌处理时控制搅拌的转速为1500~1800转/分钟。
5.根据权利要求1所述的一种锰锌软磁铁氧体材料的制备方法,其特征在于,步骤(6)中所述的恒温干燥箱内的干燥温度为90~95℃。
6.根据权利要求1所述的一种锰锌软磁铁氧体材料的制备方法,其特征在于,步骤(7)中所述的二次预烧处理时具体工艺为:控制环境氧气含量为0.12~0.16%,先于980~1020℃的温度下加热保温处理35~45min,然后再于1200~1260℃的温度下加热保温处理1.5~2.5h,最后停止加热随炉冷却至室温即可。
7.根据权利要求1所述的一种锰锌软磁铁氧体材料的制备方法,其特征在于,步骤(8)中所述的球磨处理时控制球磨的转速为700~780转/分钟。
8.根据权利要求1所述的一种锰锌软磁铁氧体材料的制备方法,其特征在于,步骤(9)中所述的高温烧结处理时具体工艺为:控制环境氧气含量为0.18~0.23%,先于1250~1350℃的温度下加热保温处理35~45min,然后停止加热随炉冷却至室温即可。
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