CN111362684A - 一种移动谷点提高MnZn功率铁氧体材料Bs的方法 - Google Patents
一种移动谷点提高MnZn功率铁氧体材料Bs的方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 100
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 38
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003292 glue Substances 0.000 claims abstract description 22
- 239000000654 additive Substances 0.000 claims abstract description 17
- 230000000996 additive effect Effects 0.000 claims abstract description 17
- 238000005469 granulation Methods 0.000 claims abstract description 17
- 230000003179 granulation Effects 0.000 claims abstract description 17
- 239000004576 sand Substances 0.000 claims abstract description 17
- 239000007921 spray Substances 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 10
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000009472 formulation Methods 0.000 description 4
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 3
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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Abstract
本发明公开了一种移动谷点提高MnZn功率铁氧体材料Bs的方法,涉及MnZn功率铁氧体材料制备领域,包括以下步骤:1)将Fe2O3、MnO和ZnO混合,进行一次砂磨;2)加入胶水,并进行喷雾造粒,随后进行预烧,得到预烧料;3)在预烧料中加入添加剂,进行二次砂磨;4)在二次砂磨料中加入胶水,喷雾造粒,压制成标环后烧结,本发明通过控制Fe2O3含量与Co2O3含量来控制和移动谷点,降低损耗的同时,提高材料的Bs,解决了现有技术中无法同时兼顾移动谷点,降低损耗和提高材料的Bs的问题,且本发明方法较为简便,适合工业化。
Description
技术领域
本发明涉及MnZn功率铁氧体材料制备领域,尤其涉及一种移动谷点提高MnZn功率铁氧体材料Bs的方法。
背景技术
现有的MnZn功率铁氧体材料移动谷点,通常认为主配方中Fe2O3含量高的损耗谷点往低温移动,Fe2O3含量低的损耗谷点往高温移动,或者通过控制Fe2O3和ZnO含量移动谷点,减少ZnO含量提高MnZn功率铁氧体材料的Bs。现有的技术,依靠Fe2O3含量高低移动谷点,会使高温损耗增加或Bs降低,Fe2O3含量高,谷点往低温移动,高温特别是100℃之后的损耗会增加,降低Fe2O3含量,会使材料的Bs降低。通过控制Fe2O3和ZnO含量移动谷点,减少ZnO含量提高MnZn功率铁氧体材料的Bs的技术,会使材料的损耗增加。因此现有的技术条件下,提高Bs、降低损耗和移动谷点之间有一定的矛盾,无法兼顾,因为其本质还是通过Fe2O3和ZnO含量控制谷点的移动。
例如,一种在中国专利文献上公开的“一种控制宽温低温度系数锰锌铁氧体粉料谷点的方法”,其公告号CN107935579A,其公开了一种在产品研发及产品批量生产中精确控制宽温低温度系数锰锌铁氧体粉料谷点的方法。所述锰锌铁氧体粉料包括主成分和添加剂;所述主成分由Fe2O3、ZnO和Mn3O4组成;所述ZnO占主成分的重量百分比为4~9wt%;所述Fe2O3占主成分的重量百分比根据公式Fe2O3(wt%)=72.88A*ZnO(wt%)计算;其中控制谷点为80℃时,A值为0.2278;其中控制谷点为90℃时,A值为0.2313;其中控制谷点为100℃时,A值为0.2358。然而,该发明通过主配方中的Fe2O3和ZnO含量来控制谷点,未涉及如何降低损耗,提高Bs等问题,且通过该方法控制谷点也会使材料的损耗增加。
发明内容
本发明是为了克服目前通过主配方中控制Fe2O3和ZnO含量移动谷点,减少ZnO含量提高MnZn功率铁氧体材料的Bs的技术,会使材料的损耗增加等问题,提出了一种移动谷点提高MnZn功率铁氧体材料Bs的方法。
为了实现上述目的,本发明采用以下技术方案:
一种移动谷点提高MnZn功率铁氧体材料Bs的方法,包括以下步骤:
1)将Fe2O3、MnO和ZnO混合,进行一次砂磨;
2)加入胶水,并进行喷雾造粒,随后进行预烧,得到预烧料;
3)在预烧料中加入添加剂,进行二次砂磨;
4)在二次砂磨料中加入胶水,喷雾造粒,压制成标环后烧结。
作为优选,步骤1)中各组分配比:Fe2O3为52.9-53.3mol%,MnO为38.3-39.08mol%,ZnO为7.62-8.8mol%。
作为优选,步骤3)中添加剂包括以下组分且占预烧料的质量百分比为:0.03-0.08wt%CaCO3,0.015-0.04wt%ZrO2,0.43-0.52wt%Co2O3,0.05-0.2wt%SnO2。
本发明通过调整Fe2O3含量与Co2O3含量配比,使谷点往高温方向移动,提高Bs的同时,降低高温损耗。
本发明的原理在于,材料的谷点是受磁晶各向异性常数K1与温度的关系的影响,在K1为0处,就是材料的谷点处。在本发明的主配方中,即Fe2O3、MnO和ZnO的配比要控制在一定的范围,这是由于当主配方中Fe2O3含量超过53.3mol%,会使材料的涡流损耗增加,低于52.9mol%,则不能与Co2O3协同有效降低材料的磁晶各向异性常数K1。其次,相对于主配方的总重量而言,本发明Co2O3含量必须在0.43%-0.52%;这是由于Co2O3含量低于0.43%时,增加Fe2O3含量,会使谷点往低温方向移动,高于0.52%时,会使材料的损耗变差,主要是因为过量的Co2O3,会使材料的磁晶各向异性常数K2变大,导致损耗增加。因此,在原配方的基础上,包括添加剂,通过提高原配方的Fe2O3含量,将Co2O3含量控制在相对于主配方的总重量的0.43%--0.52%,可以使谷点往高温方向移动,来降低高温损耗,提高材料的Bs。而这与现有技术中通常认为的提高Fe2O3含量谷点往低温移动,降低Fe2O3含量谷点往高温移动是相违背的。
而现有技术K1为0是通过控制Fe2O3含量的高低或控制Fe2O3与ZnO的配比来控制K1与温度的关系,即通过调整Fe2O3含量的高低或控制Fe2O3和ZnO的配比来移动谷点,其并不能同时兼顾移动谷点,降低损耗和提高材料的Bs;虽然,现有的技术在移动谷点方面,也会考虑到用Co2O3来调整,但现有技术认为,加入Co2O3谷点就肯定往低温方向移动,因此现有技术中Co2O3通常是认为对谷点往低温方向移动有帮助,有利于降低室温损耗,所以Co2O3的添加量也不会多,一般控制在预烧料总重量的0.35wt%以下,其并没有考虑到Co2O3的量在一定范围内时,谷点会出现相反的移动,即Fe2O3含量的增加,导致谷点往高温移动。
作为优选,所述一次砂磨和二次砂磨的料球水比例为1:5-7:0.4-0.6,砂磨时间为0.5-1.5h。
在该条件配比下,砂磨更加均匀。
作为优选,步骤2)中加入预烧料总质量10%、质量分数为7.5%的胶水。
作为优选,步骤2)中所述预烧为在回转窑中900-1000℃下预烧。
作为优选,步骤3)中加入二次砂磨料总质量10%、质量分数为7.5%的胶水。
作为优选,步骤4)中所述压制的压力为6-8Mpa。
因此,本发明具有如下有益效果:本发明通过控制Fe2O3含量与Co2O3含量来控制和移动谷点,降低损耗的同时,提高材料的Bs,解决了现有技术中无法同时兼顾移动谷点,降低损耗和提高材料的Bs的问题,且本发明方法较为简便,适合工业化。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
实施例1:一种移动谷点提高MnZn功率铁氧体材料Bs的方法,包括以下步骤:
1)将52.9mol%的Fe2O3、38.3mol%的MnO和8.8mol%的ZnO混合,在料球水比例为1:5:0.4下一次砂磨1.5h;
2)加入预烧料总质量10%、质量分数为7.5%的胶水,并进行喷雾造粒,随后在回转窑中900℃下预烧,得到预烧料;
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为:CaCO3为0.03%、ZrO2为0.04%,Co2O3为0.44%,SnO2为0.05%,随后在料球水比例为1:5:0.4下二次砂磨1.5h;
4)在二次砂磨料中加入二次砂磨料总质量10%、质量分数为7.5%的胶水,喷雾造粒,在6Mpa压制成标环后烧结。
实施例2:一种移动谷点提高MnZn功率铁氧体材料Bs的方法,包括以下步骤:
1)将53.3mol%的Fe2O3、39.08mol%的MnO和7.62mol%的ZnO混合,在料球水比例为1:7:0.6下一次砂磨0.5h;
2)加入预烧料总质量10%、质量分数为7.5%的胶水,并进行喷雾造粒,随后在回转窑中1000℃下预烧,得到预烧料;
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为:CaCO3为0.03%、ZrO2为0.04%,Co2O3为0.48%,SnO2为0.05%,随后在料球水比例为1:7:0.6下二次砂磨0.5h;
4)在二次砂磨料中加入二次砂磨料总质量10%、质量分数为7.5%的胶水,喷雾造粒,在8Mpa压制成标环后烧结。
实施例3:一种移动谷点提高MnZn功率铁氧体材料Bs的方法,包括以下步骤:
1)将53.1mol%的Fe2O3、38.5mol%的MnO和8.4mol%的ZnO混合,在料球水比例为1:6:0.5下一次砂磨1h;
2)加入预烧料总质量10%、质量分数为7.5%的胶水,并进行喷雾造粒,随后在回转窑中950℃下预烧,得到预烧料;
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为:CaCO3为0.03%、ZrO2为0.04%,Co2O3为0.52%,SnO2为0.05%,随后在料球水比例为1:6:0.5下二次砂磨1h;
4)在二次砂磨料中加入二次砂磨料总质量10%、质量分数为7.5%的胶水,喷雾造粒,在7Mpa压制成标环后烧结。
对比例1:一种移动谷点提高MnZn功率铁氧体材料Bs的方法,包括以下步骤:
1)将52.6mol%的Fe2O3、38.6mol%的MnO和8.8mol%的ZnO混合,在料球水比例为1:5:0.4下一次砂磨1.5h;
2)加入预烧料总质量10%、质量分数为7.5%的胶水,并进行喷雾造粒,随后在回转窑中900℃下预烧,得到预烧料;
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为:CaCO3为0.03%、ZrO2为0.04%,Co2O3为0.44%,SnO2为0.05%,随后在料球水比例为1:5:0.4下二次砂磨1.5h;
4)在二次砂磨料中加入二次砂磨料总质量10%、质量分数为7.5%的胶水,喷雾造粒,在6Mpa压制成标环后烧结。
对比例2:一种移动谷点提高MnZn功率铁氧体材料Bs的方法,包括以下步骤:
1)将53.3mol%的Fe2O3、39.08mol%的MnO和7.62mol%的ZnO混合,在料球水比例为1:7:0.6下一次砂磨0.5h;
2)加入预烧料总质量10%、质量分数为7.5%的胶水,并进行喷雾造粒,随后在回转窑中1000℃下预烧,得到预烧料;
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为:CaCO3为0.03%、ZrO2为0.04%,Co2O3为0.35%,SnO2为0.05%,随后在料球水比例为1:7:0.6下二次砂磨0.5h;
4)在二次砂磨料中加入二次砂磨料总质量10%、质量分数为7.5%的胶水,喷雾造粒,在8Mpa压制成标环后烧结。
对比例3:一种移动谷点提高MnZn功率铁氧体材料Bs的方法,包括以下步骤:
1)将53.5mol%的Fe2O3、38.9mol%的MnO和7.6mol%的ZnO混合,在料球水比例为1:6:0.5下一次砂磨1h;
2)加入预烧料总质量10%、质量分数为7.5%的胶水,并进行喷雾造粒,随后在回转窑中950℃下预烧,得到预烧料;
3)在预烧料中加入包括以下组分的添加剂且占预烧料的质量百分比为:CaCO3为0.03%、ZrO2为0.04%,Co2O3为0.52%,SnO2为0.05%,随后在料球水比例为1:6:0.5下二次砂磨1h;
4)在二次砂磨料中加入二次砂磨料总质量10%、质量分数为7.5%的胶水,喷雾造粒,在7Mpa压制成标环后烧结。
对实施例和对比例制备得到的MnZn功率铁氧体材料的谷点和Bs进行测试,所得数据如下表所示。
表1:实施例及对比例测试数据表。
从上表可知,实施例1和对比例1只是Fe2O3含量不同,两者的Co2O3含量相同,实施例1中Fe2O3含量高,谷点却往高温方向移动,对比例1中Fe2O3含量低,谷点却往低温方向移动,这些都是因为加入了一定量的Co2O3所致。同时Fe2O3含量高的,Bs也高。
实施例2和对比例2只是Co2O3含量不同,比较例2中的Co2O3含量不在本发明范围内,所以Fe2O3含量多时,谷点往低温方向移动。
实施例3和对比例3对比,其中对比例3中的Fe2O3和ZnO的含量超出了本发明的范围,损耗偏高。
Claims (8)
1.一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,包括以下步骤:
1)将Fe2O3、MnO和ZnO混合,进行一次砂磨;
2)加入胶水,并进行喷雾造粒,随后进行预烧,得到预烧料;
3)在预烧料中加入添加剂,进行二次砂磨;
4)在二次砂磨料中加入胶水,喷雾造粒,压制成标环后烧结。
2.根据权利要求1所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,步骤1)中各组分配比:Fe2O3为52.9-53.3mol%,MnO为38.3-39.08mol%,ZnO为7.62-8.8mol%。
3.根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,步骤3)中添加剂包括以下组分且占预烧料的质量百分比为:0.03-0.08wt%CaCO3,0.015-0.04 wt % ZrO2,0.43-0.52 wt % Co2O3,0.05-0.2 wt % SnO2。
4.根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,所述一次砂磨和二次砂磨的料球水比例为1:5-7:0.4-0.6,砂磨时间为0.5-1.5h。
5.根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,步骤2)中加入预烧料总质量10%、质量分数为7.5%的胶水。
6.根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,步骤2)中所述预烧为在回转窑中900-1000℃下预烧。
7.根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,步骤3)中加入二次砂磨料总质量10%、质量分数为7.5%的胶水。
8.根据权利要求1或2所述的一种移动谷点提高MnZn功率铁氧体材料Bs的方法,其特征在于,步骤4)中所述压制的压力为6-8Mpa。
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