CN116239376B - 一种高熵尖晶石吸波陶瓷材料及其制备方法 - Google Patents
一种高熵尖晶石吸波陶瓷材料及其制备方法 Download PDFInfo
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- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 67
- 239000011029 spinel Substances 0.000 title claims abstract description 67
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 19
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 17
- 239000010949 copper Substances 0.000 claims description 16
- 239000011777 magnesium Substances 0.000 claims description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 239000011701 zinc Substances 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 15
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000011787 zinc oxide Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 7
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 7
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 7
- 239000005751 Copper oxide Substances 0.000 claims description 6
- 229910000431 copper oxide Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 230000005855 radiation Effects 0.000 claims description 4
- 238000001238 wet grinding Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 4
- 239000011358 absorbing material Substances 0.000 abstract description 3
- 238000005341 cation exchange Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 16
- 238000000227 grinding Methods 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000012700 ceramic precursor Substances 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
本发明提供了一种高熵尖晶石吸波陶瓷材料及其制备方法,涉及吸波材料技术领域。本发明提供的高熵尖晶石吸波陶瓷材料,化学式为(MgxCoyNizCumZnn)Fe2O4,x为0.2~0.25,y为0.11~0.2,z为0.13~0.23,m为0.2~0.25,n为0.2~0.25。本发明通过高熵效应和尖晶石型材料固有的阳离子交换作用,极大的提升了材料的电磁波损耗能力,并通过对金属元素含量的控制,在保持单相材料的前提下提高了材料的阻抗匹配。本发明提供的高熵尖晶石吸波陶瓷材料具有宽吸收频段和高吸收能力。
Description
技术领域
本发明涉及吸波材料技术领域,具体涉及一种高熵尖晶石吸波陶瓷材料及其制备方法。
背景技术
随着信息技术的迅速发展,尤其是5G技术的广泛应用,电磁污染变得越来越严重,对人的健康产生了巨大影响,可能引发心脑血管疾病,细胞癌变和多种永久性病变。
陶瓷基电磁波吸收材料具有强度大、耐腐蚀和耐高温等多种优点,但却在微波吸收方面由于阻抗匹配问题导致吸收带宽窄,最大反射损耗低等问题。
发明内容
本发明的目的在于提供一种高熵尖晶石吸波陶瓷材料及其制备方法,本发明提供的高熵尖晶石吸波陶瓷材料具有宽吸收频段和高吸收能力。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种高熵尖晶石吸波陶瓷材料,化学式为(MgxCoyNizCumZnn)Fe2O4,x为0.2~0.25,y为0.11~0.2,z为0.13~0.23,m为0.2~0.25,n为0.2~0.25。
优选地,包括(Mg0.2Co0.2Ni0.2Cu0.2Zn0.2)Fe2O4、(Mg0.25Co0.12Ni0.13Cu0.25Zn0.25)Fe2O4或(Mg0.22Co0.11Ni0.23Cu0.22Zn0.22)Fe2O4。
优选地,所述高熵尖晶石吸波陶瓷材料为单一尖晶石结构,空间群为Fd-3m。
本发明提供了上述技术方案所述高熵尖晶石吸波陶瓷材料的制备方法,包括以下步骤:
将氧化镁、一氧化钴、氧化镍、氧化铜、氧化锌和三氧化二铁混合,进行烧结,得到高熵尖晶石吸波陶瓷材料。
优选地,所述氧化镁、一氧化钴、氧化镍、氧化铜、氧化锌和三氧化二铁的摩尔比为0.2±0.05:0.2±0.15:0.2±0.15:0.2±0.05:0.2±0.05:1。
优选地,所述混合为研磨。
优选地,所述研磨为湿磨。
优选地,所述烧结的温度为900~1100℃,保温时间为4~6h。
优选地,所述烧结采用的加热方式为辐射加热。
优选地,所述烧结的气氛为空气气氛。
本发明提供了一种高熵尖晶石吸波陶瓷材料,化学式为(MgxCoyNizCumZnn)Fe2O4,x为0.2~0.25,y为0.11~0.2,z为0.13~0.23,m为0.2~0.25,n为0.2~0.25。本发明通过高熵效应和尖晶石型材料固有的阳离子交换作用,极大的提升了材料的电磁波损耗能力,并通过对金属元素含量的控制,在保持单相材料的前提下提高了材料的阻抗匹配。本发明提供的高熵尖晶石吸波陶瓷材料具有宽吸收频段和高吸收能力。
本发明还提供了上述技术方案所述高熵尖晶石吸波陶瓷材料的制备方法,本发明采用固相反应法制备高熵陶瓷粉体,所需实验设备简单,操作容易,便于规模生产。本发明的原料价格低,生产成本低,制备工艺简单,便于产业化大规模生产。
附图说明
图1为实施例1~3所制备的高熵尖晶石吸波陶瓷材料的XRD图谱;
图2为实施例3制备的高熵尖晶石吸波陶瓷材料的形貌扫描电镜照片;
图3为实施例3制备的高熵尖晶石吸波陶瓷材料的复介电常数图;
图4为实施例3制备的高熵尖晶石吸波陶瓷材料的复磁导率图;
图5为实施例3制备的高熵尖晶石吸波陶瓷材料的磁滞回线图;
图6为实施例1制备的高熵尖晶石吸波陶瓷材料的反射损耗图;
图7为实施例2制备的高熵尖晶石吸波陶瓷材料的反射损耗图;
图8为实施例3制备的高熵尖晶石吸波陶瓷材料的反射损耗图。
具体实施方式
本发明提供了一种高熵尖晶石吸波陶瓷材料,化学式为(MgxCoyNizCumZnn)Fe2O4,x为0.2~0.25,y为0.11~0.2,z为0.13~0.23,m为0.2~0.25,n为0.2~0.25。在本发明中,所述x优选为0.22,y优选为0.12,z优选为0.2,m为0.22,n为0.22。
在本发明中,所述高熵尖晶石吸波陶瓷材料优选包括Mg0.2Co0.2Ni0.2Cu0.2Zn0.2)Fe2O4、(Mg0.25Co0.12Ni0.13Cu0.25Zn0.25)Fe2O4或(Mg0.22Co0.11Ni0.23Cu0.22Zn0.22)Fe2O4。
在本发明中,所述高熵尖晶石吸波陶瓷材料优选为单一尖晶石结构,空间群优选为Fd-3m。在本发明中,所述高熵尖晶石吸波陶瓷材料属于尖晶石型铁氧体。
本发明提供了上述技术方案所述高熵尖晶石吸波陶瓷材料的制备方法,包括以下步骤:
将氧化镁、一氧化钴、氧化镍、氧化铜、氧化锌和三氧化二铁混合,进行烧结,得到高熵尖晶石吸波陶瓷材料。
在本发明中,所述氧化镁、一氧化钴、氧化镍、氧化铜、氧化锌和三氧化二铁的摩尔比优选为0.2±0.05:0.2±0.15:0.2±0.15:0.2±0.05:0.2±0.05:1,更优选为0.22:0.11:0.23:0.22:0.22:1。在本发明中,所述氧化镁、一氧化钴、氧化镍、氧化铜、氧化锌和三氧化二铁以粉末的形式进行混合;所述氧化镁粉末、一氧化钴粉末、氧化镍粉末、氧化铜粉末、氧化锌粉末和三氧化二铁粉末的粒径独立优选为100~200μm。
在本发明中,所述混合优选为研磨。在本发明中,所述研磨优选为湿磨。在本发明中,所述研磨的时间优选为0.5h。本发明通过研磨使原料混合更加均匀,保证了烧结后各种元素分布的均匀性。在本发明中,所述湿磨时采用的助磨剂优选为酒精。本发明在所述研磨过程中加入的酒精助磨剂在研磨过程中完全挥发,得到混合均匀的氧化物前驱体。本发明对所述酒精的添加量没有特殊要求,只要满足浸润全部氧化物,研磨过程能够完全挥发即可。
在本发明中,所述烧结的温度优选为900~1100℃,保温时间优选为4~6h。在本发明中,由室温升温至所述烧结的温度的升温速率优选为3~10℃/min。
在本发明中,所述烧结采用的加热方式优选为辐射加热,更优选为热辐射加热。
在本发明中,所述烧结的气氛优选为空气气氛。在本发明中,所述烧结优选在马弗炉的坩埚中进行。在本发明中,所述坩埚优选为氧化铝坩埚。
在本发明中,所述高熵尖晶石吸波陶瓷材料优选为粉体;微观形貌优选为1~5μm的微球。
本发明在单相材料中通过元素配比调控了材料的阻抗匹配,得到了吸收带宽宽,损耗能力强的高熵尖晶石吸波陶瓷材料。
下面将结合本发明中的实施例,对本发明中的技术方案进行清楚、完整地描述。显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做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
(Mg0.2Co0.2Ni0.2Cu0.2Zn0.2)Fe2O4高熵尖晶石吸波陶瓷材料的制备方法如下:
步骤1,称量0.803gMgO,1.499gCoO,1.494gNiO,1.591gCuO,1.628gZnO和15.969gFe2O3粉末,置于研钵中,再滴加酒精直至浸润所有粉体,研磨混合0.5h,得到高熵尖晶石吸波陶瓷前驱体;
步骤2,将步骤1制得的高熵尖晶石吸波陶瓷前驱体置于刚玉坩埚中,在马弗炉中以10℃/min升温至1100℃,保温6h,获得(Mg0.2Co0.2Ni0.2Cu0.2Zn0.2)Fe2O4高熵尖晶石吸波陶瓷粉体。
对实施例1所得高熵尖晶石吸波陶瓷材料进行XRD表征,结果如图1所示,说明得到的高熵陶瓷为尖晶石结构。
测试并计算实施例1所得高熵尖晶石吸波陶瓷材料的电磁波吸收性能,结果如图6所示。由图6可以看出,本实施例制备的高熵尖晶石吸波陶瓷材料在6.48GHz~12.4GHz(吸收带宽5.92GHz)吸收频段均具有较好的吸波性能,RLmin=-25.5dB。
实施例2
(Mg0.25Co0.12Ni0.13Cu0.25Zn0.25)Fe2O4高熵尖晶石吸波陶瓷材料的制备方法如下:
步骤1,称量1.008gMgO,0.899gCoO,0.971gNiO,1.989gCuO,2.035gZnO和15.969gFe2O3粉末,置于研钵中,再滴加酒精直至浸润所有粉体,研磨混合0.5h,得到高熵尖晶石吸波陶瓷前驱体;
步骤2,将步骤1制得的高熵尖晶石吸波陶瓷前驱体置于刚玉坩埚中,在马弗炉中以10℃/min升温至1100℃,保温6h,获得(Mg0.25Co0.12Ni0.13Cu0.25Zn0.25)Fe2O4高熵尖晶石吸波陶瓷粉体。
对实施例2所得高熵尖晶石吸波陶瓷材料进行XRD表征,结果如图1所示,说明得到的高熵陶瓷为尖晶石结构。
测试并计算实施例2所得高熵尖晶石吸波陶瓷材料的电磁波吸收性能,结果如图7所示。由图7可以看出,本实施例制备的高熵尖晶石吸波陶瓷材料在5.36GHz~10.32GHz(吸收带宽4.96GHz)吸收频段均具有较好的吸波性能,RLmin=-29.1dB。
实施例3
(Mg0.22Co0.11Ni0.23Cu0.22Zn0.22)Fe2O4高熵尖晶石吸波陶瓷材料的制备方法如下:
步骤1,称量0.887gMgO,0.824gCoO,1.718gNiO,1.750gCuO,1.791gZnO和15.969gFe2O3粉末,置于研钵中,再滴加酒精直至浸润所有粉体,研磨混合0.5h,得到高熵尖晶石吸波陶瓷前驱体;
步骤2,将步骤1制得的高熵尖晶石吸波陶瓷前驱体置于刚玉坩埚中,在马弗炉中以10℃/min升温至1100℃,保温6h,获得(Mg0.22Co0.11Ni0.23Cu0.22Zn0.22)Fe2O4高熵尖晶石吸波陶瓷粉体。
对实施例3所得高熵尖晶石吸波陶瓷材料进行XRD表征,结果如图1所示,说明得到的高熵陶瓷为尖晶石结构。
对实施例3所得高熵尖晶石吸波陶瓷材料进行SEM表征,结果如图2所示,说明得到的高熵陶瓷的微观形貌为1~5μm的微球。
对实施例3所得高熵尖晶石吸波陶瓷材料进行电磁参数测试,复介电常数如图3所示,复磁导率如图4所示。由图3可以看出,实施例3的介电常数实部和虚部在2~18GHz上基本不变,由图4可以看出,实施例3的磁导率实部和虚部在2~18GHz上先增后减。
对实施例3所得高熵尖晶石吸波陶瓷材料进行VSM测试,磁滞回线如图5所示,说明获得的高熵吸波陶瓷为软磁性材料。
测试并计算实施例3所得高熵尖晶石吸波陶瓷材料的电磁波吸收性能,结果如图8所示。由图8可以看出,本实施例制备的高熵尖晶石吸波陶瓷材料在4.8GHz~9.52GHz(吸收带宽4.72GHz)吸收频段均具有较好的吸波性能,RLmin=-50.4dB。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (6)
1.一种高熵尖晶石吸波陶瓷材料的制备方法,步骤为:
将氧化镁、一氧化钴、氧化镍、氧化铜、氧化锌和三氧化二铁混合,进行烧结,得到高熵尖晶石吸波陶瓷材料;所述烧结的温度为1100℃,保温时间为6h;
所述高熵尖晶石吸波陶瓷材料的化学式为(Mg0.22Co0.11Ni0.23Cu0.22Zn0.22)Fe2O4。
2.根据权利要求1所述的制备方法,其特征在于,所述高熵尖晶石吸波陶瓷材料为单一尖晶石结构,空间群为Fd-3m。
3.根据权利要求1所述的制备方法,其特征在于,所述混合为研磨。
4.根据权利要求3所述的制备方法,其特征在于,所述研磨为湿磨。
5.根据权利要求1所述的制备方法,其特征在于,所述烧结采用的加热方式为辐射加热。
6.根据权利要求1所述的制备方法,其特征在于,所述烧结的气氛为空气气氛。
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