CN112142456A - 一种铁氧体吸波材料及其制备方法 - Google Patents
一种铁氧体吸波材料及其制备方法 Download PDFInfo
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- 239000011358 absorbing material Substances 0.000 title claims abstract description 38
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 10
- 239000010959 steel Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 8
- 229910052788 barium Inorganic materials 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 229910052712 strontium Inorganic materials 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000008188 pellet Substances 0.000 abstract 1
- 230000005670 electromagnetic radiation Effects 0.000 description 7
- 239000011701 zinc Substances 0.000 description 6
- 239000010936 titanium Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- FEBJSGQWYJIENF-UHFFFAOYSA-N nickel niobium Chemical compound [Ni].[Nb] FEBJSGQWYJIENF-UHFFFAOYSA-N 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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Abstract
一种铁氧体吸波材料及其制备方法，该铁氧体吸波材料的化学式为AxByFezO；制备方法包括以下步骤：（1）选用A的碳酸盐，B的氧化物和Fe2O3作为原料，根据化学式AxByFezO进行计算，并称量各原料组分；（2）将所述各原料加入球磨机内，并添加钢球和水，进行球磨；（3）将球磨后料浆过筛以分离钢球，然后将料浆脱水；（4）将脱水后的料浆造粒成料球，然后将料球置于窑炉中空气气氛下烧结，烧结完成后，自然冷却；（5）将烧结后的料球粉碎至成粉末，即成。本发明通过配方中各元素的调配，实现材料的吸波性能；制备方法，工艺简单，生产效率高，生产成本低。
Description
技术领域
本发明涉及一种吸波材料，尤其是涉及一种铁氧体吸波材料及其制备方法。
背景技术
随着通信技术的进步，4G全面应用，5G技术逐步推开，频率从越来越高1.8GHz到5GHz，传输速度越来越快，给人们生活带来很大便利的同时，电磁辐射的影响也越来越大，对自然环境和人类生存将造成一定危害。吸波材料可以消除电磁辐射的污染，在环保中有着重要的作用。另外吸波材料可以防止计算机主机和其附属设备在工作时产生的电磁辐射被接收并还原出原信息造成泄密，可以最大限度地减少或者消除雷达等对目标的探测特征，因此，它是电磁辐射防护、电磁干扰防护、电磁信息泄露防护、军事隐身等民用与国防军工技术领域中重要的材料之一。
铁氧体具有介电特性和磁特性，可以通过介电损耗和磁损耗使入射微波耗损，降低反射率，是一种较好的GHz范围的吸波材料。当前铁氧体吸波材料大多采用自蔓延燃烧法、溶胶凝胶法、水热法、化学共沉淀法来制备，如CN 104628372 B公开了一种铌镍共掺杂钡铁氧体吸波粉体材料及其制备方法，采用自蔓延燃烧法制备铁氧体前驱体粉末；CN103435798 B公开了一种稀土共掺杂钡铁氧体/聚苯胺复合材料，采用溶胶凝胶法制备稀土掺杂钡铁氧体。这些制备方法生产规模较小，效率较低。
通讯电磁辐射的频率一般在1.8GHz到5GHz，计算机电磁辐射一般在MHz到GHz（文献：计算机主机的电磁辐射的测试与分析，《科技与创新》2014年第1期），厘米波雷达探测频率一般为3GHz~30GHz。频段范围较宽，但常用的一般在2GHz~18GHz范围内。对钡铁氧体而言，其本身的自然共振频率高于40 GHz。CN 104628372 B公开的吸波材料，通过钛掺杂可将频率控制在26 .5~40 GHz范围调节，制备方法中公开需要在70℃~90 ℃干燥3~5天，能耗高，时间长，效率低，成本高。CN103922716A公开的技术方案，通过锌掺杂，降低吸波频率，可将吸波特性峰控制在12.8GHz、16.9GHz和17.5GHz，但吸波层较厚，17.5GHz匹配的厚度达到5.2mm，实用性较差，工艺过程中需在80℃左右干燥18h~22h，干燥时间长，能耗仍然较高，生产效率仍然较低，成本仍然较高。
发明内容
本发明所要解决的技术问题是，克服现有技术存在的上述不足，提供一种吸波频段可在1GHz~20GHz较大范围内变化的铁氧体吸波材料。
本发明进一步要解决的技术问题，提供一种工艺简单的所述铁氧体吸波材料的制备方法。
本发明解决其技术问题采用的技术方案是，一种铁氧体吸波材料，所述吸波材料的化学式为AxByFezO，其中x＝1~3，y=1~2，z=10~16；所述A为Ba、Sr元素中的一种或两种，B为Co、Zn、Ti、La、Mn、Cu等元素中的一种或几种。
进一步，所述铁氧体吸波材料的化学式为AxByFezO中，A为Ba和Sr，Ba:Sr=3~1；B为Co、Ti、La、Mn和Cu等，其中 Co:（Ti+La+Mn+Cu）=10~0.5:1；x=1，y=1~2，z=10~12。
进一步，所述铁氧体吸波材料的化学式为AxByFezO中，A为Ba，B为Co、Zn、Ti、La和Cu等，x=1，y=1~2，z=14~16。Co:（Zn +Ti+La+Mn+Cu）=8~1:1。
本发明进一步解决其技术问题采用的技术方案是，一种所述铁氧体吸波材料的制备方法，包括以下步骤：
（1）选用A的碳酸盐，B的氧化物和Fe2O3作为原料，根据化学式AxByFezO进行计算，并称量各原料组分；
（2）将所述各原料加入球磨机内，并添加钢球和水，进行球磨；
（3）将球磨后料浆过筛以分离钢球，然后将料浆脱水；（4）将脱水后的料浆造粒成料球，然后将料球置于窑炉中空气气氛下烧结，烧结完成后，自然冷却；
（5）将烧结后的料球振磨粉碎至成粉末，即得到本发明铁氧体吸波材料。
进一步，步骤(2)中，料:球:水的质量比为1:10~15:2~3；球磨时间为2h~10h。
进一步，步骤(2)中，球磨罐转速为20转/min~90转/min，球磨时间为3h~6h。
进一步，步骤(3)中，脱水后料浆含水量为10%~40%。
进一步，步骤(3)中，脱水后料浆含水量为20%~30%；脱水方式为离心脱水。
进一步，步骤(4)中，所述料球的直径为φ5mm~φ20mm，烧结的温度为1200~1400℃烧结的时间为1h~5h；所述窑炉为轨道窑；所述烧结的方式为连续烧结。
进一步，步骤(5)中，所述粉末的粒径≤10μm；粉碎的方式为振磨粉碎。
所述各原料可以选用工业纯产品，以降低生产成本。
本发明通过配方中各元素的调配技术，实现材料的吸波性能，并可针对不同使用领域，通过调整合金元素的比例，即可使铁氧体吸波材料的吸波频段在1GHz~20GHz较大范围内变化。本发明制备方法，选用粉末冶金方法，工艺简单，生产效率高，不仅解决了大批量生产的问题，而且能耗低，生产成本低。
具体实施方式
下面结合实施例对本发明的具体实施方式作说明。
本发明实施例所使用的原料，均为工业纯成品；均通过常规商业途径获得。
实施例1-3
以下所述实施例1-3铁氧体吸波材料，化学式为（BaSr）x[Cow（ZnTiLaMnCu）]yFezO，其中实施例1的x＝1、y=2、z=13、w=8，实施例2的x＝2、y=2、z=15、w=3，实施例3的x＝3、y=1、z=16、w=1；按实施例1~3配料，其中Ba以BaCO3、Sr以SrCO3，Co以Co2O3、Zn以ZnO、Ti以TiO2、La以La2O3、Mn以Mn3O4、Cu以CuO、Fe以Fe2O3形式加入。
本发明实施例1~3铁氧体永磁材料的制备方法，包括以下步骤：
（1）分别称量好工业纯的碳酸盐和氧化物原材料，称量误差保持在0.1%以内；
（2）将上述各原材料加入球磨机内，并添加10倍质量的钢球和3倍质量的水，球磨10h；
（3）将球磨后料浆过筛以分离钢球，然后将料浆离心脱水至含水量40%；
（4）将脱水后的料浆造粒成φ10mm的料球，然后将料球置于窑炉中空气气氛下1200~1400℃烧结5h，自然冷却；
（5）将烧结后的料球振磨粉碎至≤10μm的粉末，即得到本发明的铁氧体吸波材料。
将上述吸波材料与石蜡按85:15比例混合，压制成标准环，测试其介电常数和磁导率，计算2mm厚度的吸波峰值出现在10~15GHz，达到-22dB~-41dB（参见表1）。
表1：实施例1-3铁氧体永磁材料的吸波峰值
实施例4-6
以下所述实施例4-6铁氧体吸波材料，化学式为（BaSr）x[Cow（TiLaMnCu）]yFezO，其中，实施例4的x＝1、y=1、z=10、w=10，实施例5的x＝1、y=2、z=12、w=4，实施例6的x＝1、y=2、z=10、w=0.5；按实施例4-6配料，其中Ba以BaCO3、Sr以SrCO3，Co以Co2O3、Zn以ZnO、Ti以TiO2、La以La2O3、Mn以Mn3O4、Cu以CuO、Fe以Fe2O3形式加入。
本发明实施例4-6铁氧体永磁材料的制备方法，包括以下步骤：
（2）分别称量好工业纯的碳酸盐和氧化物原材料，称量误差保持在0.1%以内；
（2）将上述各原材料加入球磨机内，并添加15倍质量的钢球和2倍质量的水，球磨2h；
（3）将球磨后料浆过筛以分离钢球，然后将料浆离心脱水至含水量10%；
（4）将脱水后的料浆造粒成φ5mm的料球，然后将料球置于窑炉中空气气氛下1200℃烧结2h，自然冷却；
（5）将烧结后的料球振磨粉碎至≤10μm的粉末，即得到本发明的铁氧体吸波材料。
将上述吸波材料与石蜡按85:15比例混合，压制成标准环，测试其介电常数和磁导率，计算2mm厚度的吸波峰值出现在4~8GHz，达到-20dB~-34dB。
表2：实施例1-3铁氧体永磁材料的吸波峰值
Claims (10)
1.一种铁氧体吸波材料，其特征在于：化学式为AxByFezO，其中x＝1~3，y=1~2，z=10~16；A为Ba、Sr元素中的一种或两种，B为Co、Zn、Ti、La、Mn、Cu元素中的一种或几种。
2.根据权利要求1所述的铁氧体吸波材料，其特征在于：A为Ba和Sr，Ba:Sr=3~1；B为Co、Ti、La、Mn和Cu，其中，Co:（Ti+La+Mn+Cu）=10~0.5:1；x=1，y=1~2，z=10~12。
3.根据权利要求1所述的铁氧体吸波材料，其特征在于：A为Ba，B为Co、Zn、Ti、La和Cu，其中Co:（Zn+Ti+La+Mn+Cu）=8~1:1；x=1，y=1~2，z=14~16。
4.一种如权利要求1-3之一所述铁氧体吸波材料的制备方法，其特征在于，包括以下步骤：
（1）选用A的碳酸盐，B的氧化物和Fe2O3作为原料，根据化学式AxByFezO进行计算，并称量各原料组分；（2）将所述各原料加入球磨机内，并添加钢球和水，进行球磨；
（3）将球磨后料浆过筛以分离钢球，然后将料浆脱水；（4）将脱水后的料浆造粒成料球，然后将料球置于窑炉中空气气氛下烧结，烧结完成后，自然冷却；
（5）将烧结后的料球粉碎至成粉末，即得到本发明铁氧体吸波材料。
5.根据权利要求4所述的铁氧体吸波材料的制备方法，其特征在于：步骤(2)中，料:球:水的质量比为1:10~15:2~3；球磨时间为2h~10h。
6.根据权利要求4或5所述的铁氧体吸波材料的制备方法，其特征在于：步骤(2)中，球磨罐转速为20转/min~90转/min，球磨时间为3h~6h。
7.根据权利要求4或5所述的铁氧体吸波材料的制备方法，其特征在于：步骤(3)中，脱水后料浆含水量为10%~40%。
8.根据权利要求7所述的铁氧体吸波材料的制备方法，其特征在于：步骤(3)中，脱水后料浆含水量为20%~30%；脱水方式为离心脱水。
9.根据权利要求4-8之一所述的铁氧体吸波材料的制备方法，其特征在于：步骤(4)中，所述料球的直径为φ5mm~φ20mm，烧结的温度为1200~1400℃烧结的时间为1h~5h；所述窑炉为轨道窑；所述烧结的方式为连续烧结。
10.根据权利要求4-9之一所述的铁氧体吸波材料的制备方法，其特征在于：步骤(5)中，所述粉末的粒径≤10μm；粉碎的方式为振磨粉碎。
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