CN107903394B - 高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法 - Google Patents

高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法 Download PDF

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CN107903394B
CN107903394B CN201711140252.4A CN201711140252A CN107903394B CN 107903394 B CN107903394 B CN 107903394B CN 201711140252 A CN201711140252 A CN 201711140252A CN 107903394 B CN107903394 B CN 107903394B
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江智渊
赵慧
郑兰荪
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Abstract

高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法，涉及聚酰亚胺。1)制备石墨烯溶液；2)将二氨基二苯醚粉末加到步骤1)制备的石墨烯溶液中混合，得溶液A；3)将均苯四甲酸二酐粉末加入步骤2)制备的混合溶液A中缩合，得溶液B；4)在步骤3)得到的溶液B中加入磁性纳米粒子，搅拌，得溶液C；5)将步骤4)得到的溶液C倾倒在平板上，再放在以水为絮凝剂的絮凝池中，絮凝后烘干；所得的材料的结构特点是带有明显泡沫结构的高聚物/石墨烯@磁性纳米粒子复合材料，并且在电磁波吸收上表现出比较优越的性质。操作简单，可操作性强，重现性好，产率可达95％。

Description

高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法
技术领域
本发明涉及聚酰亚胺，尤其是涉及高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法。
背景技术
聚酰亚胺具有优良的机械性能，一些聚酰亚胺品种不溶于有机溶剂，对稀酸稳定聚酰亚胺具有很高的耐辐照性能，聚酰亚胺是自熄性聚合物，发烟率低。聚酰亚胺作为一种特种工程材料，已广泛应用在航空、航天、微电子、纳米、液晶、分离膜、激光等领域。聚酰亚胺，因其在性能和合成方面的突出特点，不论是作为结构材料或是作为功能性材料，其巨大的应用前景已经得到充分的认识，被称为是"解决问题的能手"，并认为“没有聚酰亚胺就不会有今天的微电子技术”。聚酰亚胺高聚物与石墨烯形成的这种泡沫结构已有研究。(Y.Li,X.L.pei,B.shen,W.T.zhai,L.H.zhang,RSC ADV.5(2015)24342-24351)然而，目前对于聚酰亚胺高聚物/石墨烯与磁性纳米粒子复合形成的泡沫结构研究的不多，同时这种结构的复合材料具有良好的导电性和高饱和磁化强度，在电磁波吸收方面有良好的应用空间，有广阔的应用空间。
发明内容
本发明的目的在于提供工艺步骤较为简单，泡沫结构合成较为均一和高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法。
本发明包括以下步骤：
1)制备石墨烯溶液；
在步骤1)中，所述制备石墨烯溶液的具体方法可为：将石墨烯加入到N,N-二甲基甲酰胺溶液中，超声混合，得石墨烯溶液。
2)将二氨基二苯醚(ODA)粉末加到步骤1)制备的石墨烯溶液中混合，得溶液A；
3)将均苯四甲酸二酐(PMDA)粉末加入步骤2)制备的混合溶液A中缩合，得溶液B；
在步骤3)中，所述将均苯四甲酸二酐(PMDA)粉末加入步骤2)制备的混合溶液A中缩合，可将与二氨基二苯醚(ODA)等摩尔量的PMDA粉末加入步骤2)中制备的溶液中。
4)在步骤3)得到的溶液B中加入磁性纳米粒子，搅拌，得溶液C；
在步骤4)中，所述磁性纳米粒子可选自金属、金属氧化物、合金等中的一种。
5)将步骤4)得到的溶液C倾倒在平板上，再放在以水为絮凝剂的絮凝池中，絮凝后烘干；
在步骤5)中，所述平板可采用玻璃板等；所述烘干的温度可为60℃。
本发明所得的材料的结构特点是带有明显泡沫结构的高聚物/石墨烯@磁性纳米粒子(金属，金属氧化物，合金)复合材料，并且在电磁波吸收上表现出比较优越的性质。
本发明的突出优点在于：
1)利用溶液缩聚法制备得到新型高聚物/石墨烯@磁性纳米粒子(金属，金属氧化物，合金)泡沫复合材料，这种材料在微波吸收上具有潜在的应用前景；
2)本发明操作简单，可操作性强，重现性好，产率可达95％。
3)本发明可大规模制备，实现商品化，在实际应用中具有潜在的应用价值。
4)本发明耐高温，在航空航天方面具有潜在的应用价值。
附图说明
图1为泡沫结构的高聚物/石墨烯的扫描电镜(SEM)图。
图2为泡沫结构的高聚物/石墨烯的红外谱图。
图3为小倍数下的泡沫结构的高聚物/石墨烯@Fe3O4扫描电镜(SEM)图。
图4为放大倍数下的泡沫结构的高聚物/石墨烯@Fe3O4扫描电镜(SEM)图。
图5为泡沫结构的高聚物/石墨烯@Fe3O4所对应的X射线粉末衍射图。
图6为泡沫结构的高聚物/石墨烯@Fe3O4所对应的不同厚度的微波吸收曲线。在图6中，测试频率范围在2～18GHz。
图7为泡沫结构的高聚物/石墨烯@FeCoNi的扫描电镜(SEM)图。
图8为泡沫结构的高聚物/石墨烯@FeCoNi对应的X射线粉末衍射图。
图9为泡沫结构的高聚物/石墨烯@FeCoNi对应不同厚度的微波吸收曲线。在图9中，测试频率范围在2～18GHz。
图10所对应的为泡沫结构的高聚物/石墨烯@Co扫描电镜(SEM)图。
图11所对应的为泡沫结构的高聚物/石墨烯@Co射线粉末衍射图。
具体实施方式
下面通过实施例结合附图对本发明作进一步说明。
实施例1
(1)在100～250ml的圆底烧瓶中，加入一定量的氧化还原石墨烯，量取一定体积的N,N-二甲基溶剂，超声1.5h,称量加入等摩尔量的ODA和PMDA，机械搅拌反应8h,,得到的溶液倾倒在干净的玻璃板上，将其放在以水为絮凝剂的絮凝池中，絮凝大概12h，放在60℃的烘箱中12h。
(2)在100-250ml的圆底烧瓶中，加入一定量的氧化还原石墨烯，量取一定体积的N,N-二甲基溶剂，超声1h,称量加入等摩尔量的ODA和PMDA，机械搅拌5h，之后加入一定量的金属氧化物(以Fe3O4为例)，继续搅拌3h，得到的溶液倾倒在干净的玻璃板上，将其放在以水为絮凝剂的絮凝池中，絮凝大概10h，放在60℃的烘箱中16h。
由图1可以看出用本方法制备出了泡沫结构。由图2可以看出本发明制备聚酰亚胺酸这种高聚物。由图3和图4可以看出，制备了高聚物/石墨烯及磁性金属(金属氧化物，合金)等纳米粒子泡沫结构。图5中的X射线粉末衍射图可以看出：衍射角度18.3°、30.1°、35.5°、37.1°、43.1°、53.5°、56.9°、62.6°、70.9°与体心立方结构的Fe3O4:PDF#65-3107的(111)、(220)和(311)、(222)、(400)、(422)、(511)、(440)、(620)晶面相对应，并且并没有发现其它杂质峰的出现。图6为微波吸收的模拟图，根据模拟数据可以看到，在吸波片层厚度为2mm，低于-10dB吸收频带范围，达到2.4GHz的吸收展宽。
实施例2
(1)在100～250ml的圆底烧瓶中，加入一定量的氧化还原石墨烯，量取一定体积的N,N-二甲基溶剂，超声2h,称量加入等摩尔量的ODA和PMDA，机械搅拌7h,之后加入一定量的金属合金(以FeCoNi为例)，继续搅拌5h，得到的溶液倾倒在干净的玻璃板上，将其放在以水为絮凝剂的絮凝池中，絮凝大概12h，放在60℃的烘箱中12h。
由图7可以看出，制备了高聚物/石墨烯及磁性纳米粒子(金属，合金，金属氧化物)泡沫结构。图8中的X射线粉末衍射图可以看出：衍射角度44.5°、51.8°、76.7°，92.7°与体心立方结构的FeCoNi的(111)、(200)和(220)、(222)、(311)、晶面相对应，并且并没有发现其它杂质峰的出现。图9为微波吸收的模拟图，根据模拟数据可以看到，在吸波片层厚度为2.5mm，低于-10dB吸收频带范围，达到5.9GHz的吸收展宽。
实施例3
(1)在100～250ml的圆底烧瓶中，加入一定量的氧化还原石墨烯，量取一定体积的N,N-二甲基溶剂，超声0.5h,称量加入等摩尔量的ODA和PMDA，机械搅拌10h,之后加入一定量的金属(以Co为例)，继续搅拌5h,得到的溶液倾倒在干净的玻璃板上，将其放在以水为絮凝剂的絮凝池中，絮凝大概10h，放在60℃的烘箱中18h
由图10可以看出，制备了高聚物@石墨烯及磁性金属合金纳米粒子泡沫结构。图11的X射线粉末衍射图可以看出：衍射角度41.7°、44.8°、47.6°，75.9°与六方结构的金属Co:PDF#05-0727的(100)、(002)、(101)、(110)晶面相对应，并且并没有发现其它杂质峰的出现。

Claims (6)

1.高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法，其特征在于包括以下步骤：
1)制备石墨烯溶液；
2)将二氨基二苯醚(ODA)粉末加到步骤1)制备的石墨烯溶液中混合，得溶液A；
3)将均苯四甲酸二酐(PMDA)粉末加入步骤2)制备的混合溶液A中缩合，得溶液B；
4)在步骤3)得到的溶液B中加入磁性纳米粒子，搅拌，得溶液C；
5)将步骤4)得到的溶液C倾倒在平板上，再放在以水为絮凝剂的絮凝池中，絮凝后烘干。
2.如权利要求1所述高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法，其特征在于在步骤1)中，所述制备石墨烯溶液的具体方法为：将石墨烯加入到N,N-二甲基甲酰胺溶液中，超声混合，得石墨烯溶液。
3.如权利要求1所述高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法，其特征在于在步骤3)中，所述将均苯四甲酸二酐粉末加入步骤2)制备的混合溶液A中缩合，是将与二氨基二苯醚等摩尔量的PMDA粉末加入步骤2)中制备的溶液中。
4.如权利要求1所述高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法，其特征在于在步骤4)中，所述磁性纳米粒子选自金属、金属氧化物、合金中的一种。
5.如权利要求1所述高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法，其特征在于在步骤5)中，所述平板采用玻璃板。
6.如权利要求1所述高聚物/石墨烯@磁性纳米粒子泡沫复合材料的合成方法，其特征在于在步骤5)中，所述烘干的温度为60℃。
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