CN114604858B - 一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法 - Google Patents

一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法 Download PDF

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CN114604858B
CN114604858B CN202210328319.1A CN202210328319A CN114604858B CN 114604858 B CN114604858 B CN 114604858B CN 202210328319 A CN202210328319 A CN 202210328319A CN 114604858 B CN114604858 B CN 114604858B
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魏汉军
赵峰
王清远
周春林
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Abstract

本发明涉及微波吸收材料技术领域，尤其涉及一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法。本发明将Sc(NO3)3·6H2O与Fe(NO3)3·9H2O加入到去离子水中，搅拌溶解得到溶液A；将水性聚乙烯醇PVA溶解于Sc(NO3)3水溶液中得到溶液B；将溶液A和溶液B混合均匀并搅拌12～14h得到均质溶胶C；将均质溶胶C匀速升温至温度为200～300℃并保温6～8h，在匀速升温至温度为900～1000℃煅烧6～8h得到ScFeO3粉末；将氧化石墨烯GO加入至去离子水中，超声分散10～12h得到GO悬浮液；将ScFeO3粉末加入到GO悬浮液中混匀得到前驱体溶液；将前驱体溶液冷冻干燥，然后置于氩气氛围、温度为1000～1200℃下保温2～3h得到三维还原氧化石墨烯rGO/ScFeO3复合吸波材料。本发明ScFeO3颗粒嵌入rGO中可显著降低电导率，增加孔隙率，改善阻抗匹配特性和电导率损失。

Description

一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备 方法
技术领域
本发明涉及微波吸收材料技术领域，尤其涉及一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法。
背景技术
随着电磁波污染和电磁干扰在日常生活和军事领域日益突出，迫切需要解决电磁辐射污染问题。最近，解决这一问题需要创新新型高性能微波吸收材料。由于仅存在单损耗介质(如磁损耗或介电损耗)，大多数传统微波吸收材料无法实现更好的阻抗匹配和耗散性能，这限制了其广泛的发展。
发明内容
本发明针对现有技术中微波吸收材料存在的问题，提供一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法，采用溶胶-凝胶法制备ScFeO3粉末，再采用冷冻干燥和热处理合成三维还原氧化石墨烯rGO/ScFeO3复合吸波材料，通过控制复合材料中ScFeO3粉末的含量，从而调整电磁参数和微波吸收性能。
一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法，具体步骤如下：
(1)将Sc(NO3)3·6H2O与Fe(NO3)3·9H2O加入到去离子水中，搅拌溶解得到溶液A；将水性聚乙烯醇PVA溶解于Sc(NO3)3水溶液中得到溶液B；
(2)将溶液A和溶液B混合均匀并搅拌12～14h得到均质溶胶C；
(3)将均质溶胶C匀速升温至温度为200～400℃并保温6～8h，在匀速升温至温度为900～1100℃煅烧6～8h得到ScFeO3粉末；
(4)将氧化石墨烯GO加入至去离子水中，超声分散10～12h得到GO悬浮液；将ScFeO3粉末加入到GO悬浮液中混匀得到前驱体溶液；
(5)将前驱体溶液冷冻干燥形成多孔泡沫结构，然后置于氩气氛围、温度为1000～1200℃下保温2～4h得到三维还原氧化石墨烯rGO/ScFeO3复合吸波材料。
所述均质溶胶C中Sc与Fe的摩尔比为1:1～1:1.5。
所述ScFeO3粉末占氧化石墨烯GO质量的1～3％。
本发明的有益效果是：
(1)本发明将ScFeO3颗粒嵌入rGO中显著降低了电导率，增加了孔隙率，从而改善了阻抗匹配特性和电导率损失；
(2)本发明三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的3D网络为多次反射、散射微波和快速损耗微波能量提供了更多空间；
(3)本发明三维还原氧化石墨烯rGO/ScFeO3复合吸波材料中的大量的异质界面和缺陷也增强了极化损耗；
(4)本发明三维还原氧化石墨烯rGO/ScFeO3复合吸波材料由于高磁各向异性增强了磁损耗，具有自然共振效应；
(5)本发明方法操作过程简便，易于实施，适合于规模化工业生产应用。
附图说明
图1为不同ScFeO3含量的三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的SEM图，(a)为0wt％，(b)为1wt％，(c)为2wt％，(d)为3wt％；
图2为不同ScFeO3含量的三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的拉曼光谱图；
图3为高分辨透射的三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的TEM图，(a)为rGO/ScFeO3的TEM成分，(b)为高分辨透射rGO/ScFeO3的TEM成分，(c)为高分辨透射rGO/ScFeO3的TEM成分。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明，但本发明的保护范围并不限于所述内容。
对比例：三维还原氧化石墨烯rGO吸波材料的制备方法，具体步骤如下：
(1)将氧化石墨烯GO加入至去离子水中，超声分散10h得到GO悬浮液；
(5)将GO悬浮液冷冻干燥形成多孔泡沫结构，然后置于氩气氛围、温度为1000℃下保温2h得到三维还原氧化石墨烯rGO吸波材料，即ScFeO3含量为0wt％。
实施例1：一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法，具体步骤如下：
(1)将Sc(NO3)3·6H2O与Fe(NO3)3·9H2O加入到去离子水中，搅拌溶解得到溶液A；将水性聚乙烯醇PVA溶解于Sc(NO3)3水溶液中得到溶液B；
(2)将溶液A和溶液B混合均匀并搅拌12h得到均质溶胶C；其中均质溶胶C中Sc与Fe的摩尔比为1:1；
(3)将均质溶胶C匀速升温至温度为200℃并保温6h，在匀速升温至温度为900℃煅烧6h得到ScFeO3粉末；
(4)将氧化石墨烯GO加入至去离子水中，超声分散10h得到GO悬浮液；将ScFeO3粉末加入到GO悬浮液中混匀得到前驱体溶液；ScFeO3粉末占氧化石墨烯GO质量的1％；
(5)将前驱体溶液冷冻干燥形成多孔泡沫结构，然后置于氩气氛围、温度为1000℃下保温2h得到三维还原氧化石墨烯rGO/ScFeO3复合吸波材料，即ScFeO3含量为1wt％；
本实施例rGO/ScFeO3复合材料中ScFeO3颗粒附着在rGO上，阻碍了电子的运动，ScFeO3颗粒逐渐占据rGO的层状结构，嵌入rGO中的ScFeO3颗粒显着降低了rGO/ScFeO3复合材料的电导率，同时，rGO/ScFeO3复合材料阻抗匹配特性也得到了提高；因此其微波吸收性能得到了提高，也增加了微波损耗机制。
实施例2：一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法，具体步骤如下：
(1)将Sc(NO3)3·6H2O与Fe(NO3)3·9H2O加入到去离子水中，搅拌溶解得到溶液A；将水性聚乙烯醇PVA溶解于Sc(NO3)3水溶液中得到溶液B；
(2)将溶液A和溶液B混合均匀并搅拌13h得到均质溶胶C；其中均质溶胶C中Sc与Fe的摩尔比为1:1.3；
(3)将均质溶胶C匀速升温至温度为300℃并保温7h，在匀速升温至温度为1000℃煅烧7h得到ScFeO3粉末；
(4)将氧化石墨烯GO加入至去离子水中，超声分散11h得到GO悬浮液；将ScFeO3粉末加入到GO悬浮液中混匀得到前驱体溶液；ScFeO3粉末占氧化石墨烯GO质量的2％；
(5)将前驱体溶液冷冻干燥形成多孔泡沫结构，然后置于氩气氛围、温度为1100℃下保温3h得到三维还原氧化石墨烯rGO/ScFeO3复合吸波材料，即ScFeO3含量为2wt％；
本实施例rGO/ScFeO3复合材料中ScFeO3颗粒附着在rGO上，阻碍了电子的运动，ScFeO3颗粒逐渐占据rGO的层状结构，嵌入rGO中的ScFeO3颗粒显着降低了rGO/ScFeO3复合材料的电导率，同时，rGO/ScFeO3复合材料阻抗匹配特性也得到了提高；因此其微波吸收性能得到了提高，也增加了微波损耗机制。
实施例3：一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法，具体步骤如下：
(1)将Sc(NO3)3·6H2O与Fe(NO3)3·9H2O加入到去离子水中，搅拌溶解得到溶液A；将水性聚乙烯醇PVA溶解于Sc(NO3)3水溶液中得到溶液B；
(2)将溶液A和溶液B混合均匀并搅拌14h得到均质溶胶C；其中均质溶胶C中Sc与Fe的摩尔比为1:1.5；
(3)将均质溶胶C匀速升温至温度为400℃并保温8h，在匀速升温至温度为1100℃煅烧8h得到ScFeO3粉末；
(4)将氧化石墨烯GO加入至去离子水中，超声分散12h得到GO悬浮液；将ScFeO3粉末加入到GO悬浮液中混匀得到前驱体溶液；ScFeO3粉末占氧化石墨烯GO质量的3％；
(5)将前驱体溶液冷冻干燥形成多孔泡沫结构，然后置于氩气氛围、温度为1200℃下保温4h得到三维还原氧化石墨烯rGO/ScFeO3复合吸波材料，即ScFeO3含量为3wt％。
不同含量的ScFeO3粉末的CNT/SiCNWs复合材料的截面形貌见图1，图(a)显示了纯rGO具有大比表面积的层状结构，为ScFeO3颗粒的包裹提供了空间；图(b)显示ScFeO3颗粒附着在rGO上，并且阻碍了电子运动，嵌入RGO中的ScFeO3颗粒显著降低了rGO/ScFeO3复合材料的导电性；图(c)和(d)显示更多的ScFeO3颗粒附着在rGO上，随着ScFeO3颗粒含量的增加，ScFeO3颗粒逐渐占据rGO的层状结构，并形成3D结构，进一步阻碍了电子运动，同时增加了孔隙率，这不仅增加了阻抗匹配特性，而且丰富了损耗机制；
不同含量的ScFeO3粉末的CNT/SiCNWs复合材料的拉曼光谱图见图2，当ScFeO3粉末含量为0wt％时，ID/IG(rGO)值为0.89；当ScFeO3粉末含量为1wt％时，ID/IG(SC-1)值为0.91；当ScFeO3粉末含量为2wt％时，ID/IG(SC-2)值为0.98；当ScFeO3粉末含量为3wt％时，ID/IG(SC-3)值为0.95；石墨缺陷、无定形和无序碳有助于形成G峰，而sp2游离碳有助于形成D峰；由图可知，ID/IG随ScFeO3粉末含量变化而变化；
高分辨透射的ScFeO3粉末的CNT/SiCNWs复合材料的TEM图见图3，(a)显示rGO/ScFeO3复合材料的薄层结构，并且存在一些褶皱以增加比表面积，ScFeO3颗粒的大小约为100nm；(b)高分辨透射rGO/ScFeO3的TEM成分，(c)显示晶面间距为0的rGO/ScFeO3复合材料的HRTEM，rGO和ScFeO3颗粒之间的纳米界面约为5nm；纳米界面有利于微波的反射和散射，提高了微波吸收性能。
以上对本发明的具体实施方式作了详细说明，但是本发明并不限于上述实施方式，在本领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下作出各种变化。

Claims (1)

1.一种三维还原氧化石墨烯rGO/ScFeO3复合吸波材料的制备方法，其特征在于，具体步骤如下：
（1）将Sc(NO3)3·6H2O与Fe(NO3)3·9H2O加入到去离子水中，搅拌溶解得到溶液A；将水性聚乙烯醇PVA溶解于Sc(NO3)3水溶液中得到溶液B；
（2）将溶液A和溶液B混合均匀并搅拌12~14 h得到均质溶胶C；均质溶胶C中Sc与Fe的摩尔比为1:1~1:1.5；
（3）将均质溶胶C匀速升温至温度为200~300℃并保温6~8h，在匀速升温至温度为900~1100℃煅烧6~ 8h得到ScFeO3粉末；
（4）将氧化石墨烯GO加入至去离子水中，超声分散10~12h得到GO悬浮液；将ScFeO3粉末加入到GO悬浮液中混匀得到前驱体溶液；ScFeO3粉末占氧化石墨烯GO质量的1~3%；
（5）将前驱体溶液冷冻干燥，然后置于氩气氛围、温度为1000~1200℃下保温2~4 h得到三维还原氧化石墨烯rGO/ScFeO3复合吸波材料。
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