CN107151137A - 一种锰锌软磁铁氧体材料及其制备方法 - Google Patents
一种锰锌软磁铁氧体材料及其制备方法 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 35
- 239000004615 ingredient Substances 0.000 claims abstract description 34
- 230000000996 additive effect Effects 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 15
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 15
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 35
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 22
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 22
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 21
- -1 Compound rare-earth Chemical class 0.000 claims description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 5
- 235000013539 calcium stearate Nutrition 0.000 claims description 5
- 239000008116 calcium stearate Substances 0.000 claims description 5
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 5
- 229940075613 gadolinium oxide Drugs 0.000 claims description 5
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 5
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 4
- 235000019359 magnesium stearate Nutrition 0.000 claims description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- 230000005291 magnetic effect Effects 0.000 abstract description 5
- 230000006698 induction Effects 0.000 abstract description 4
- 230000035699 permeability Effects 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 description 6
- 239000011163 secondary particle Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
本发明提出了一种锰锌软磁铁氧体材料及其制备方法,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 31.4‑33.5%、ZnO6.85‑8.3%、CoCl20.25‑0.28%、SiO20.16‑0.24%、V2O50.08‑0.12%,余量为Fe2O3,通过混合、研磨、干燥、烧结等步骤制成的,通过对传统锰锌软磁铁氧体进行元素掺杂,有效提高了铁氧体内部晶粒的细化成长,制得的锰锌软磁铁氧体材料具有优良的磁性能,电阻率、初始磁导率、饱和磁感应强度、居里温度更高,且功率损耗、矫顽力显著降低。
Description
技术领域
本发明涉及铁氧体磁性材料技术领域,具体涉及一种锰锌软磁铁氧体材料及其制备方法。
背景技术
高电阻率铁氧体磁粉、磁芯是实现程控通讯、数字技术、网络通讯彩电等电子设备中用作电感器、滤波器、脉冲变压器等产品使其小型化、轻量化必不可少的电子材料,不断提高磁性材料中的电阻率,一直是从事该专业的工程技术人员和生产厂商的追求,但材料的性能指标,如损耗、频率特性、居里温度等都不尽人意。当前软磁铁氧体材料的研究重点主要集中在两个方面:一方面研究配方以及添加剂对材料性能的影响,另一方面研究生产工艺的优化及新设备的开发对提高材料性能的作用。大量的研究表明、配方、添加剂、粉体的制备方法、烧结工艺中的各种因素等都会对铁氧体的性能产生很大的影响。其中合理的配方、添加剂对软磁铁氧体的性能有着重要的影响,也是制备高性能铁氧体材料的有效方法之一,配方与添加剂的研究已经逐步成为铁氧体制备中的关键技术。
发明内容
针对上述存在的问题,本发明提出了一种锰锌软磁铁氧体材料及其制备方法,通过对传统锰锌软磁铁氧体进行元素掺杂,有效提高了铁氧体内部晶粒的细化成长,制得的锰锌软磁铁氧体材料具有优良的磁性能,电阻率、初始磁导率、饱和磁感应强度、居里温度更高,且功率损耗、矫顽力显著降低。
为了实现上述的目的,本发明采用以下的技术方案:
一种锰锌软磁铁氧体材料,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 31.4-33.5%、ZnO 6.85-8.3%、CoCl2 0.25-0.28%、SiO2 0.16-0.24%、V2O50.08-0.12%,余量为Fe2O3。
优选的,所述添加剂包括Al2O3、Nb2O5、CaO、TiO2、Bi2O3。
优选的,所述添加剂中各组分占主料质量百分含量为Al2O3 0.012-0.028%、Nb2O50.036-0.045%、CaO 0.04-0.06%、TiO2 0.005-0.03%、Bi2O3 0.005-0.02%。
优选的,所述添加剂中还包括复合稀土,所述复合稀土占主料质量百分含量为0.008-0.015%。
优选的,所述复合稀土为摩尔比1:1的氧化镧或氧化铈和氧化钆的混合物。
优选的,锰锌软磁铁氧体材料,制备步骤如下:
1)按配比称取MnO、ZnO、CoCl2、SiO2、V2O5、Fe2O3干混15-20min,然后加水、调节pH,并向其中添加主料质量0.5-2.5%的硬脂酸盐,高速搅拌8-10min,再转移至球磨机内球磨至粒径为8-15μm,得预混料;
2)将预混料干燥后在850-900℃、供氧条件下预烧结1-1.5h,取出后送入球磨机内进行二次球磨至粒径小于5μm;
3)向添加剂中添加占其质量2-3%的硅烷偶联剂和占其质量1-4%的聚乙烯醇,送入研磨机中研磨至粒径小于5μm,取出真空干燥得辅料;
4)将预混料和辅料共混,在高速搅拌机中搅拌混合4-6min,然后再送入球磨机内球磨至粒径小于1μm,得基料;
5)将基料喷雾干燥后压制成型,在1278-1285℃条件下烧结,得锰锌软磁铁氧体材料。
优选的,步骤1)pH值为11.4-11.8。
优选的,步骤1)中硬脂酸盐为硬脂酸钙、硬脂酸镁、硬脂酸锌中的一种或多种。
优选的,步骤1)中高速搅拌速度为2800-3000rpm,步骤4)中高速搅拌速度为3600-4000rpm。
由于采用上述的技术方案,本发明的有益效果是:本发明锰锌软磁铁氧体通过混合、研磨、干燥、烧结等步骤制成的,通过对传统锰锌软磁铁氧体进行元素掺杂,有效提高了铁氧体内部晶粒的细化成长,制得的锰锌软磁铁氧体材料具有优良的磁性能,电阻率、初始磁导率、饱和磁感应强度、居里温度更高,且功率损耗、矫顽力显著降低。初始磁导率为8260,饱和磁感应强度为531mT(常温),居里温度为256℃,功率损耗为326kw/m3(100℃)(以上数据均为本发明实施例经检测后的平均值)。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述。基于本发明的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:
一种锰锌软磁铁氧体材料,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 32.5%、ZnO 6.85%、CoCl2 0.26%、SiO2 0.18%、V2O5 0.09%,余量为Fe2O3,所述添加剂包括Al2O3、Nb2O5、CaO、TiO2、Bi2O3,添加剂中各组分占主料质量百分含量为Al2O30.016%、Nb2O5 0.042%、CaO 0.05%、TiO2 0.005%、Bi2O3 0.01%。
添加剂中还包括复合稀土,所述复合稀土占主料质量百分含量为0.012%,复合稀土为摩尔比1:1的氧化铈和氧化钆的混合物。
锰锌软磁铁氧体材料,制备步骤如下:
1)按配比称取MnO、ZnO、CoCl2、SiO2、V2O5、Fe2O3干混15-20min,然后加水、调节pH为11.6,并向其中添加主料质量1%的硬脂酸钙,以2800rpm高速搅拌8-10min,再转移至球磨机内球磨至粒径为8-15μm,得预混料;
2)将预混料干燥后在880℃、供氧条件下预烧结1.2h,取出后送入球磨机内进行二次球磨至粒径小于5μm;
3)向添加剂中添加占其质量2.5%的硅烷偶联剂和占其质量1.5%的聚乙烯醇,送入研磨机中研磨至粒径小于5μm,取出真空干燥得辅料;
4)将预混料和辅料共混,在高速搅拌机中以3600rpm搅拌混合4-6min,然后再送入球磨机内球磨至粒径小于1μm,得基料;
5)将基料喷雾干燥后压制成型,在1280℃条件下烧结,得锰锌软磁铁氧体材料。
实施例2:
一种锰锌软磁铁氧体材料,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 33.2%、ZnO 7.23%、CoCl2 0.27%、SiO2 0.2%、V2O5 0.1%,余量为Fe2O3,所述添加剂包括Al2O3、Nb2O5、CaO、TiO2、Bi2O3,添加剂中各组分占主料质量百分含量为Al2O30.025%、Nb2O5 0.045%、CaO 0.06%、TiO2 0.01%、Bi2O3 0.015%。
添加剂中还包括复合稀土,所述复合稀土占主料质量百分含量为0.015%,复合稀土为摩尔比1:1的氧化铈和氧化钆的混合物。
锰锌软磁铁氧体材料,制备步骤如下:
1)按配比称取MnO、ZnO、CoCl2、SiO2、V2O5、Fe2O3干混15-20min,然后加水、调节pH为11.8,并向其中添加主料质量0.5%的硬脂酸锌,以3000rpm高速搅拌8-10min,再转移至球磨机内球磨至粒径为8-15μm,得预混料;
2)将预混料干燥后在850℃、供氧条件下预烧结1.5h,取出后送入球磨机内进行二次球磨至粒径小于5μm;
3)向添加剂中添加占其质量2.6%的硅烷偶联剂和占其质量2%的聚乙烯醇,送入研磨机中研磨至粒径小于5μm,取出真空干燥得辅料;
4)将预混料和辅料共混,在高速搅拌机中以3800rpm搅拌混合4-6min,然后再送入球磨机内球磨至粒径小于1μm,得基料;
5)将基料喷雾干燥后压制成型,在1285℃条件下烧结,得锰锌软磁铁氧体材料。
实施例3:
一种锰锌软磁铁氧体材料,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 33.5%、ZnO 8.3%、CoCl2 0.26%、SiO2 0.24%、V2O5 0.12%,余量为Fe2O3,所述添加剂包括Al2O3、Nb2O5、CaO、TiO2、Bi2O3,添加剂中各组分占主料质量百分含量为Al2O30.02%、Nb2O5 0.04%、CaO 0.04%、TiO2 0.03%、Bi2O3 0.005%。
添加剂中还包括复合稀土,所述复合稀土占主料质量百分含量为0.008%,复合稀土为摩尔比1:1的氧化镧和氧化钆的混合物。
锰锌软磁铁氧体材料,制备步骤如下:
1)按配比称取MnO、ZnO、CoCl2、SiO2、V2O5、Fe2O3干混15-20min,然后加水、调节pH为11.5,并向其中添加主料质量2%的硬脂酸钙、硬脂酸锌组合物,以2800rpm高速搅拌8-10min,再转移至球磨机内球磨至粒径为8-15μm,得预混料;
2)将预混料干燥后在860℃、供氧条件下预烧结1.2h,取出后送入球磨机内进行二次球磨至粒径小于5μm;
3)向添加剂中添加占其质量2%的硅烷偶联剂和占其质量4%的聚乙烯醇,送入研磨机中研磨至粒径小于5μm,取出真空干燥得辅料;
4)将预混料和辅料共混,在高速搅拌机中以3800rpm搅拌混合4-6min,然后再送入球磨机内球磨至粒径小于1μm,得基料;
5)将基料喷雾干燥后压制成型,在1278℃条件下烧结,得锰锌软磁铁氧体材料。
实施例4:
一种锰锌软磁铁氧体材料,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 31.4%、ZnO 8.16%、CoCl2 0.25%、SiO2 0.22%、V2O5 0.08%,余量为Fe2O3,所述添加剂包括Al2O3、Nb2O5、CaO、TiO2、Bi2O3,添加剂中各组分占主料质量百分含量为Al2O30.012%、Nb2O5 0.036%、CaO 0.05%、TiO2 0.005%、Bi2O3 0.02%。
锰锌软磁铁氧体材料,制备步骤如下:
1)按配比称取MnO、ZnO、CoCl2、SiO2、V2O5、Fe2O3干混15-20min,然后加水、调节pH为11.4,并向其中添加主料质量2.5%的硬脂酸镁,以2900rpm高速搅拌8-10min,再转移至球磨机内球磨至粒径为8-15μm,得预混料;
2)将预混料干燥后在900℃、供氧条件下预烧结1h,取出后送入球磨机内进行二次球磨至粒径小于5μm;
3)向添加剂中添加占其质量2.8%的硅烷偶联剂和占其质量3%的聚乙烯醇,送入研磨机中研磨至粒径小于5μm,取出真空干燥得辅料;
4)将预混料和辅料共混,在高速搅拌机中以3600rpm搅拌混合4-6min,然后再送入球磨机内球磨至粒径小于1μm,得基料;
5)将基料喷雾干燥后压制成型,在1284℃条件下烧结,得锰锌软磁铁氧体材料。
实施例5:
一种锰锌软磁铁氧体材料,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 32%、ZnO 7.58%、CoCl2 0.28%、SiO2 0.16%、V2O5 0.11%,余量为Fe2O3,所述添加剂包括Al2O3、Nb2O5、CaO、TiO2、Bi2O3,添加剂中各组分占主料质量百分含量为Al2O30.028%、Nb2O5 0.038%、CaO 0.06%、TiO2 0.02%、Bi2O3 0.018%。
锰锌软磁铁氧体材料,制备步骤如下:
1)按配比称取MnO、ZnO、CoCl2、SiO2、V2O5、Fe2O3干混15-20min,然后加水、调节pH为11.6,并向其中添加主料质量1.5%的硬脂酸钙、硬脂酸镁的组合物,以3000rpm高速搅拌8-10min,再转移至球磨机内球磨至粒径为8-15μm,得预混料;
2)将预混料干燥后在875℃、供氧条件下预烧结1.4h,取出后送入球磨机内进行二次球磨至粒径小于5μm;
3)向添加剂中添加占其质量3%的硅烷偶联剂和占其质量1%的聚乙烯醇,送入研磨机中研磨至粒径小于5μm,取出真空干燥得辅料;
4)将预混料和辅料共混,在高速搅拌机中以4000rpm搅拌混合4-6min,然后再送入球磨机内球磨至粒径小于1μm,得基料;
5)将基料喷雾干燥后压制成型,在1280℃条件下烧结,得锰锌软磁铁氧体材料。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (9)
1.一种锰锌软磁铁氧体材料,其特征在于,包括主料和添加剂,所述主料包括以下摩尔百分比组分:MnO 31.4-33.5%、ZnO 6.85-8.3%、CoCl2 0.25-0.28%、SiO2 0.16-0.24%、V2O5 0.08-0.12%,余量为Fe2O3。
2.根据权利要求1所述的锰锌软磁铁氧体材料,其特征在于:所述添加剂包括Al2O3、Nb2O5、CaO、TiO2、Bi2O3。
3.根据权利要求2所述的锰锌软磁铁氧体材料,其特征在于:所述添加剂中各组分占主料质量百分含量为Al2O3 0.012-0.028%、Nb2O5 0.036-0.045%、CaO 0.04-0.06%、TiO20.005-0.03%、Bi2O3 0.005-0.02%。
4.根据权利要求2或3所述的锰锌软磁铁氧体材料,其特征在于:所述添加剂中还包括复合稀土,所述复合稀土占主料质量百分含量为0.008-0.015%。
5.根据权利要求4所述的锰锌软磁铁氧体材料,其特征在于:所述复合稀土为摩尔比1:1的氧化镧或氧化铈和氧化钆的混合物。
6.根据权利要求1-5任一项所述的锰锌软磁铁氧体材料,其特征在于,制备步骤如下:
1)按配比称取MnO、ZnO、CoCl2、SiO2、V2O5、Fe2O3干混15-20min,然后加水、调节pH,并向其中添加主料质量0.5-2.5%的硬脂酸盐,高速搅拌8-10min,再转移至球磨机内球磨至粒径为8-15μm,得预混料;
2)将预混料干燥后在850-900℃、供氧条件下预烧结1-1.5h,取出后送入球磨机内进行二次球磨至粒径小于5μm;
3)向添加剂中添加占其质量2-3%的硅烷偶联剂和占其质量1-4%的聚乙烯醇,送入研磨机中研磨至粒径小于5μm,取出真空干燥得辅料;
4)将预混料和辅料共混,在高速搅拌机中搅拌混合4-6min,然后再送入球磨机内球磨至粒径小于1μm,得基料;
5)将基料喷雾干燥后压制成型,在1278-1285℃条件下烧结,得锰锌软磁铁氧体材料。
7.根据权利要求6所述的锰锌软磁铁氧体材料的制备步骤,其特征在于:步骤1)pH值为11.4-11.8。
8.根据权利要求6所述的锰锌软磁铁氧体材料的制备步骤,其特征在于:步骤1)中硬脂酸盐为硬脂酸钙、硬脂酸镁、硬脂酸锌中的一种或多种。
9.根据权利要求6所述的锰锌软磁铁氧体材料的制备步骤,其特征在于:步骤1)中高速搅拌速度为2800-3000rpm,步骤4)中高速搅拌速度为3600-4000rpm。
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