CN113845359A - 一种低损耗LiZnTiMn旋磁铁氧体材料及制备方法 - Google Patents
一种低损耗LiZnTiMn旋磁铁氧体材料及制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 79
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 57
- 239000002131 composite material Substances 0.000 claims abstract description 22
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 19
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 29
- 238000001816 cooling Methods 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000009766 low-temperature sintering Methods 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 230000005350 ferromagnetic resonance Effects 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 description 12
- 230000005291 magnetic effect Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000006698 induction Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 238000005469 granulation Methods 0.000 description 2
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- 230000005415 magnetization Effects 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
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- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
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Abstract
本发明提供了一种低损耗LiZnTiMn旋磁铁氧体材料及其制备方法,属于磁性材料技术领域。所述旋磁铁氧体材料包括主料和复合助烧剂,其中主料的重量百分比为99.0%~99.5%,复合助烧剂的重量百分比为0.5%~1.0%;所述主料为Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4,所述复合助烧剂由Bi2O3与Nb2O5组成,其中Bi2O3和Nb2O5的质量比为5:(1~5)。本发明通过优化烧结工艺和添加复合助烧剂实现了LiZnTiMn的低温烧结,得到了具有低损耗的LiZnTiMn铁氧体材料,同时也降低材料的矫顽力,优化了材料性能。
Description
技术领域
本发明属于磁性材料技术领域,具体涉及一种低温烧结具有低损耗的LiZnTiMn旋磁铁氧体材料及其制备方法。
背景技术
随着雷达技术的发展及应用领域的需求,相控阵雷达用移相器等微波/毫米波器件正朝着大功率、高精度、高频化方向发展。而具有高饱和磁化强度的Li系铁氧体材料能够很好地应用于Ka波段及其以上频段的铁氧体微波器件。LiZnTiMn旋磁铁氧体是Li系铁氧体材料的一种,其具有低矫顽力、高饱和磁化强度、高剩磁比等优点,在微波器件的制备中得到了广泛的应用。
作为制作铁氧体移相器的优良旋磁材料之一,当LiZnTiMn铁氧体应用于LTCF(低温共烧铁氧体)技术与银电极实现低温共烧(~960℃)时晶粒尺寸较小,气孔率较高,导致微波损耗特性(铁磁共振线宽和介电损耗)会急剧增大,从而导致铁氧体移相器的损耗变大,恶化相控阵雷达系统的性能。铁磁共振线宽常用于表征磁损耗的大小,铁磁共振线宽越大,铁磁性物质的磁损耗越大。因此,研究如何降低铁磁共振线宽以实现低损耗的LiZnTiMn铁氧体材料十分重要。
发明内容
本发明的目的在于,针对背景技术存在的缺陷,提出了一种低损耗LiZnTiMn旋磁铁氧体材料及制备方法。本发明通过优化烧结工艺和添加复合助烧剂实现了LiZnTiMn的低温烧结,得到了具有低损耗的LiZnTiMn铁氧体材料,同时也降低材料的矫顽力,优化了材料性能。
为实现上述目的,本发明采用的技术方案如下:
一种低损耗LiZnTiMn旋磁铁氧体材料,其特征在于,所述旋磁铁氧体材料包括主料和复合助烧剂,其中主料的重量百分比为99.0%~99.5%,复合助烧剂的重量百分比为0.5%~1.0%;所述主料为Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4,所述复合助烧剂由Bi2O3与Nb2O5组成,其中Bi2O3和Nb2O5的质量比为5:(1~5)。
本发明还提供了一种低损耗LiZnTiMn旋磁铁氧体材料的制备方法,其特征在于,包括以下步骤:
步骤1、以Fe2O3、ZnO、TiO2、Li2CO3、Mn3O4为原料,按照Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4分子式的比例称取原料,混料,得到主粉体;
步骤2、按照质量比主粉体:水:铁球=1:1.5:3的比例进行一次球磨,球磨时间为4~8h,球磨完成后,取出、在80~100℃下烘干,烘干后得到的粉料放入烧结炉内,以2℃/min的升温速率由室温升温至800~820℃并保温2~3h,然后随炉自然降温至室温,得到LiZnTiMn主料;
步骤3、将Bi2O3与Nb2O5组成的复合助烧剂加入步骤2得到的主料中,其中主料的重量百分比为99.0%~99.5%,复合助烧剂的重量百分比为0.5%~1.0%,复合助烧剂中Bi2O3和Nb2O5的质量比为5:(1~5);得到的粉料进行二次球磨,球磨时,粉料、水和铁球的重量比为1:1:3,球磨时间为6~8h,球磨转速为220r/min,球磨完成后,取出并在80~100℃下烘干;
步骤4、在步骤3得到的二次球磨料中加入聚乙烯醇(PVA)造粒成型并压制成坯件,再将坯件放入烧结炉中,先以2℃/min的升温速率升至450℃,保温2~3h,再以2℃/min的升温速率升至900~920℃下烧结2~4h,烧结完成后,以1℃/min的降温速率降温至600℃后随炉自然降温至室温,即得到所述低损耗LiZnTiMn旋磁铁氧体材料。
进一步地,步骤4中,所述压制成坯件时,压力为10Mpa,压力保持时间为10~20s。
本发明的有益效果为:
1、本发明提供了一种低温烧结LiZnTiMn旋磁铁氧体材料及其制备方法,LiZnTiMn铁氧体材料中加入了Bi2O3与Nb2O5复合助烧剂,通过Bi2O3助烧剂和Nb2O5助烧剂的协同作用实现了低温烧结工艺。其中,Bi2O3助烧剂能显著促进LiZnTiMn铁氧体晶粒的成核与晶粒生长,Nb2O5能提高晶粒生长的均匀性,两者的协同作用能促进LiZnTiMn铁氧体晶粒在低温下更有效地成核和均匀生长,最终实现了LiZnTiMn铁氧体在900~920℃的烧结和制备。
2、本发明中Bi2O3与Nb2O5复合助烧剂的加入使得在低温下(900~920℃)制备得到的LiZnTiMn旋磁铁氧体材料的铁磁共振线宽大大减小,降低了材料的损耗。其中,适量的Nb2O5可以抑制过大晶粒的生长,但也会导致整体晶粒尺寸偏小,影响材料的磁性能。Bi2O3可以显著的促进晶粒的生长,但在晶粒生长过程中可能会产生一些过大晶粒从而影响晶粒的均匀性,造成铁磁共振线宽和矫顽力的增大。多晶铁氧体材料的铁磁共振线宽ΔH多晶可以通过公式表示:ΔH多晶=ΔH单晶+ΔH表面+ΔH各向异性+ΔH气孔。ΔH单晶是内在线宽,相比ΔH各向异性和ΔH气孔,ΔH单晶基本可以被忽视,ΔH表面一般也受控,而ΔH各向异性和ΔH气孔与材料的微观结构关系很大,从而直接影响线宽。Bi2O3和Nb2O5的精巧的协同作用使得该LiZnTiMn铁氧体晶粒在低温下能有效且均匀地生长,从而有效的减小了铁磁共振线宽,降低了该LiZnTiMn铁氧体材料的损耗。
附图说明
图1为本发明实施例2与对比例3得到的铁氧体材料的扫描电镜图(SEM);其中,(a)为实施例2得到的铁氧体材料的SEM图,(b)为对比例3得到的铁氧体材料的SEM图。
具体实施方式
下面结合实施例和附图对本发明做进一步地说明。
实施例1
一种低损耗LiZnTiMn旋磁铁氧体材料的制备方法,包括以下步骤:
步骤1、以Fe2O3、ZnO、TiO2、Li2CO3、Mn3O4为原料,按照Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4分子式的比例称取原料,混料,得到主粉体;
步骤2、按照质量比主粉体:水:铁球=1:1.5:3的比例进行一次球磨,球磨时间为6h,球磨完成后,取出、在100℃下烘干,烘干后得到的粉料放入烧结炉内,以2℃/min的升温速率由室温升温至800℃并保温2h,然后随炉自然降温至室温,得到LiZnTiMn主料;
步骤3、将Bi2O3与Nb2O5组成的复合助烧剂加入步骤2得到的主料中,其中主料的重量百分比为99.4%,复合助烧剂的重量百分比为0.6%,复合助烧剂中Bi2O3和Nb2O5的质量比为5:1;得到的粉料进行二次球磨,球磨时,粉料、水和铁球的重量比为1:1:3,球磨时间为6h,球磨转速为220r/min,球磨完成后,取出并在100℃下烘干;
步骤4、在步骤3得到的二次球磨料中加入聚乙烯醇(PVA)造粒成型并压制成坯件,成型压力为10Mpa,再将坯件放入烧结炉中,先以2℃/min的升温速率升至450℃,保温2h,再以2℃/min的升温速率升至900℃下烧结2h,烧结完成后,以1℃/min的降温速率降温至600℃后随炉自然降温至室温,即得到所述低损耗LiZnTiMn旋磁铁氧体材料。
实施例1制备得到的LiZnTiMn旋磁铁氧体材料的性能为:样品密度:4.65g/cm3;饱和磁感应强度:307mT;铁磁共振线宽:286Oe;矫顽力:256A/m;矩形比:0.90。
实施例2
实施例2与实施例1相比,区别在于:步骤4的过程为:在步骤3得到的二次球磨料中加入聚乙烯醇(PVA)造粒成型并压制成坯件,成型压力为10Mpa,再将坯件放入烧结炉中,先以2℃/min的升温速率升至450℃,保温2h,再以2℃/min的升温速率升至920℃下烧结2h,烧结完成后,以1℃/min的降温速率降温至600℃后随炉自然降温至室温,即得到所述低损耗LiZnTiMn旋磁铁氧体材料。
实施例2制备得到的LiZnTiMn旋磁铁氧体材料的性能为:样品密度:4.70g/cm3;饱和磁感应强度:328mT;铁磁共振线宽:161Oe;矫顽力:152A/m;矩形比:0.87。
对比例1
一种低损耗LiZnTiMn旋磁铁氧体材料的制备方法,包括以下步骤:
步骤1、以Fe2O3、ZnO、TiO2、Li2CO3、Mn3O4为原料,按照Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4分子式的比例称取原料,混料,得到主粉体;
步骤2、按照质量比主粉体:水:铁球=1:1.5:3的比例进行一次球磨,球磨时间为6h,球磨完成后,取出、在100℃下烘干,烘干后得到的粉料放入烧结炉内,以2℃/min的升温速率由室温升温至800℃并保温2h,然后随炉自然降温至室温,得到LiZnTiMn主料;
步骤3、将Bi2O3助烧剂加入步骤2得到的主料中,其中主料的重量百分比为99.5%,Bi2O3助烧剂的重量百分比为0.5%;得到的粉料进行二次球磨,球磨时,粉料、水和铁球的重量比为1:1:3,球磨时间为6h,球磨转速为220r/min,球磨完成后,取出并在100℃下烘干;
步骤4、在步骤3得到的二次球磨料中加入聚乙烯醇(PVA)造粒成型并压制成坯件,成型压力为10Mpa,再将坯件放入烧结炉中,先以2℃/min的升温速率升至450℃,保温2h,再以2℃/min的升温速率升至900℃下烧结2h,烧结完成后,以1℃/min的降温速率降温至600℃后随炉自然降温至室温,即得到所述低损耗LiZnTiMn旋磁铁氧体材料。
对比例1制备得到的LiZnTiMn旋磁铁氧体材料的性能为:样品密度:4.62g/cm3;饱和磁感应强度:299mT;铁磁共振线宽:340Oe;矫顽力:314A/m;矩形比:0.91。
对比例2
对比例2与对比例1相比,区别在于:步骤4的过程为:在步骤3得到的二次球磨料中加入聚乙烯醇(PVA)造粒成型并压制成坯件,成型压力为10Mpa,再将坯件放入烧结炉中,先以2℃/min的升温速率升至450℃,保温2h,再以2℃/min的升温速率升至920℃下烧结2h,烧结完成后,以1℃/min的降温速率降温至600℃后随炉自然降温至室温,即得到所述低损耗LiZnTiMn旋磁铁氧体材料。
对比例2制备得到的LiZnTiMn旋磁铁氧体材料的性能为:样品密度:4.65g/cm3;饱和磁感应强度:327mT;铁磁共振线宽:263Oe;矫顽力:218A/m;矩形比:0.88。
对比例3
一种低损耗LiZnTiMn旋磁铁氧体材料的制备方法,包括以下步骤:
步骤1、以Fe2O3、ZnO、TiO2、Li2CO3、Mn3O4为原料,按照Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4分子式的比例称取原料,混料,得到主粉体;
步骤2、按照质量比主粉体:水:铁球=1:1.5:3的比例进行一次球磨,球磨时间为6h,球磨完成后,取出、在100℃下烘干,烘干后得到的粉料放入烧结炉内,以2℃/min的升温速率由室温升温至800℃并保温2h,然后随炉自然降温至室温,得到LiZnTiMn主料;
步骤3、在步骤2处理后得到的粉料中加入聚乙烯醇(PVA)造粒成型并压制成坯件,成型压力为10Mpa,再将坯件放入烧结炉中,先以2℃/min的升温速率升至450℃,保温2h,再以2℃/min的升温速率升至920℃下烧结2h,烧结完成后,以1℃/min的降温速率降温至600℃后随炉自然降温至室温,即得到LiZnTiMn旋磁铁氧体材料。
对比例3制备得到的LiZnTiMn旋磁铁氧体材料的性能为:样品密度:4.15g/cm3;饱和磁感应强度:150mT;铁磁共振线宽:749Oe;矫顽力:620A/m;矩形比:0.80。
图1为本发明实施例2与对比例3得到的铁氧体材料的扫描电镜图(SEM)。由图1可知,本发明加入Bi2O3和Nb2O5复合助烧剂后得到的LiZnTiMn旋磁铁氧体材料的晶粒明显生长,且晶粒均匀,表面致密。由实施例2和对比例3的性能对比可知,本发明LiZnTiMn旋磁铁氧体材料相比对比例得到的LiZnTiMn旋磁铁氧体材料的铁磁共振线宽大大的降低,材料的损耗降低。
Claims (3)
1.一种低损耗LiZnTiMn旋磁铁氧体材料,其特征在于,所述旋磁铁氧体材料包括主料和复合助烧剂,其中主料的重量百分比为99.0%~99.5%,复合助烧剂的重量百分比为0.5%~1.0%;所述主料为Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4,所述复合助烧剂由Bi2O3与Nb2O5组成,其中Bi2O3和Nb2O5的质量比为5:(1~5)。
2.一种低损耗LiZnTiMn旋磁铁氧体材料的制备方法,其特征在于,包括以下步骤:
步骤1、以Fe2O3、ZnO、TiO2、Li2CO3、Mn3O4为原料,按照Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4分子式的比例称取原料,混料,得到主粉体;
步骤2、将步骤1得到的主粉体进行一次球磨,球磨时间为4~8h,球磨完成后,取出、烘干,得到的粉料放入烧结炉内,由室温升温至800~820℃并保温2~3h,然后随炉自然降温至室温,得到LiZnTiMn主料;
步骤3、将Bi2O3与Nb2O5组成的复合助烧剂加入步骤2得到的主料中,其中主料的重量百分比为99.0%~99.5%,复合助烧剂的重量百分比为0.5%~1.0%,复合助烧剂中Bi2O3和Nb2O5的质量比为5:(1~5);得到的粉料进行二次球磨,球磨时间为6~8h,球磨完成后,取出、烘干;
步骤4、将步骤3得到的二次球磨料造粒成型并压制成坯件,再将坯件放入烧结炉中,先升至450℃,保温2~3h,再升至900~920℃下烧结2~4h,烧结完成后,降温至600℃后随炉自然降温至室温,即得到所述低损耗LiZnTiMn旋磁铁氧体材料。
3.根据权利要求2所述的低损耗LiZnTiMn旋磁铁氧体材料的制备方法,其特征在于,步骤4中,所述压制成坯件时,压力为10Mpa,压力保持时间为10~20s。
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