聚苯胺/铁氧体纳米复合材料的制备及吸波性能
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摘要
信息时代造成的电磁污染日趋严重,严重地影响着电子设备的正常运行,也严重干扰着雷达、广播、卫星数字信号等的传输,因而电磁污染问题越来越引起世界各国的共同关注。研究和开发新型的低成本、高吸收和宽频段电磁波吸收材料已成为材料领域的重要研究方向之一。高分子/无机复合材料因其具有新颖的电学性能、光学性能、磁学性能以及轻质价廉等特性,成为研究的热点。聚苯胺(PANI)是最有前景的导电高分子之一,它的合成方法简单、原料易得、化学稳定性好、具有很好导电性,把它和铁氧体纳米材料复合可以得到一类性能独特、兼具高聚物和铁氧体无机材料共同优点的功能材料。
结合目前高分子/无机复合材料以及石墨烯在微波吸收和电磁屏蔽领域的应用优势,我们制备了不同形貌、不同维数的的PANI/铁氧体纳米复合物,包括一维的PANI/镍锌铁氧体(NZFO)复合纳米棒,二维PANI/NZFO和PANI/'锶铁氧体(SrFO)/氧化石墨烯(GO)纳米片、三维多孔结构还原氧化石墨烯(rGO)/SrFO复合水凝胶,并研究了它们的微波吸收性能。具体研究内容如下：
1.利用两步法成功地制备了PANI/NZFO片状纳米复合物。首先用超声辅助氧化聚合的方法合成了PANI纳米片,然后以此为模板,在水热条件下诱导PANI/NZFO复合纳米片的形成。研究发现,尺寸大小约为18nm左右的NZFO颗粒覆盖在PANI纳米片表面,这主要是由于PANII的氮原子与NZFO中的金属离子(铁、镍或锌离子)配位作用的结果。复合物纳米片的微波吸收性能相对于单一铁氧体或者PANI、片均有明显提高,该类复合物在微波吸收材料领域有潜在的应用前景。
2.首次将超声和外磁场引导相结合,原位聚合法成功制备了新颖的一维PANI/NZFO杂化纳米棒。所制备纳米棒具有均匀的形貌、可调的磁性能,较高的比饱和磁化强度和矫顽力。电磁性能测试表明,杂化纳米棒比纯的NZFO具有更高的反射损耗和更宽的微波吸收带。当NZFO含量为59%、涂层厚度为2mm时,在6.2GHz处复合纳米棒存在微波最大反射损耗(RL),达到-27.5dB；最大吸收带宽(RL≤10dB)为8.1GHz。我们还进一步探讨了杂化纳米棒的吸波机理。
3.以GO片为软模板,利用原位聚合的方法合成了PANI/SrFO/GO复合纳米片。SrFO纳米颗粒均匀分布在GO片上,形成粘附层结构。我们初步探讨了这种结构的形成机理,认为PANI、SrFO颗粒与GO片之间既有配位作用,又有氢键和π-π相互作用。产物的微波性能测试表明,当原材料中苯胺、GO和SrFO的质量比分别是10：5：5和10：5：10时,对应的产物PANI/SrFO/GO-1和PANI/SrFO/GO-2都具有优异的电磁波损耗性能,分别在9.1和6.4GHz处达最大吸收值37dB左右,在2-18GHz频段内-10dB带宽都超过10GHz。
4.利用石墨烯片之间的疏水作用和π-π堆积作用,水热还原制备了三维多孔结构的rGO/SrFO复合水凝胶。结果显示,随着SrFO含量的增加,rGO/SrFO复合水凝胶吸波性能呈现明显增强趋势。当原材料GO和SrFO的质量比为10:4时,lmm厚度下,在3GHz处RL达到最大值-51dB；低于-10dB的损耗带宽达到10.5GHz。这说明了我们所制备的三维rGO/SrFeO复合水凝胶具有非常优异的微波吸收性能,这可能是由于凝胶的孔隙类似于一个微波谐振腔,微波在孔隙形成共振而减少反射率。这为设计和组装新型三维多孔、轻质、高强度、宽频段微波吸收材料提供了启示。
In recent years, with the fast development of information technology, the electromagnetic pollution is worsening, which affects the normal running of the electronic equipment and interferes with the radar, broadcast services, and satellite digital data transmission sharply. Therefore, the electromagnetic pollution is getting more and more attention of all countries. Now, the research and development of a new type of microwave absorption material with a cheap price, effective microwave absorption and wide-band frequency become the important direction of electromagnetic wave absorption materials. Polyaniline (PANI) is one of the most promising conducting polymers with excellent chemical stability, simple synthesis method, easy obtainment of the raw material, and high electrical conductivity. The composites containing PANI and ferrite nanoparticles have the advantages of both polymer and ferrite inorganic materials, and novel performance, and they are a type of multi-functional material.
Based on the application advantages of polymer/inorganic materials and graphene, in the dissertation, PANI/ferrite/(grapheme) or graphene/ferrite composite nanomaterials with different morphologies and dimensions have been synthesized, including one-dimensional (ID) PANI/Ni0.5Zn0.5Fe2O4(NZFO) hybrid nanorods,2D PANI/NZFO and PANI/GO/SrFe12O16(SrFO) composite nanoslices, and3D porous rGO/SrFO composite hydrogel. Their electromagnetic wave absorption properties were also investigated.
The main results can be summarized as follows:
1. PANI/NZFO ferrite composite nanoslices were successfully prepared by two steps. Firstly pure PANI nanoslices were synthesized via ultrasound assisted chemically oxidative polymerization. Then the nanoslices were used as templates to induce the formation of PANI/NZFO composites under hydrothermal conditions. The investigation results indicate that PANI nanoslices were coated by the NZFO nanoparticals with average size of18nm, and there exists the coordination interaction between M2+(M=Fe, Ni, Zn) on the surface of NZFO nanoparticles and PANI. The PANI/NZFO composite nanoslices show better microwave absorption properties than pure PANI or pure NZFO. These composite materials may be applied in microwave absorption and electromagnetic interference shielding fields.
2. The novel uniform PANI/NZFO one-dimensional (ID) hybrid nanorods were firstly in situ synthesized by ultrasonic-assisted magnetic field guidance methods. The as-synthesized hybrid nanorods possess uniform shape, adjusted magnetic properties, high saturated magnetization and high coercivity. The electromagnetic data demonstrate that hybrid nanorods present stronger reflection loss and a wider absorption band in comparison to pure NZFO. PANI/NZFO hybrid nanorods with addition of59%NZFO exhibit excellent microwave absorption performances, with a maximum reflection loss (RL) of-27.5dB observed at6.2GHz, and the widest absorption band (RL<-10dB) is8.1GHz, corresponding to a matching thin thickness of2mm. Besides, microwave absorption mechanism of hybrid nanorods was explored further.
3. Using GO nanosheets as soft template, the PANI/SrFO/GO composite nanoflakes were in situ synthesized by chemical oxidation polymorization method. The results show that SrFO nanoparticles and PANI were tightly bound to the surface of graphene sheets to form interlayer structure. The formation mechanism of the as-synthesized composites was discussed. The coordination effect, π-π interaction and hydrogen bonding exist among polyaniline, SrFO nanoparticles and graphene nanosheets. The microwave performance measurement of the products shows that PANI/SrFO/GO-1(weight ratio of aniline/GO/SrFO is10:5:5) and PANI/SrFO/GO-2(weight ratio of aniline/GO/SrFO is10:5:10) both possess excellent electromagnetic loss performances, with a maximum absorption value of about37dB at9.1and6.4 GHz, respectively. And their-10dB bandwidth surpassed10GHz in2-18GHz ranges.
4. A novel3D porous rGO/SrFO composite hydrogel was synthesized by one step hydfothermal method in the presence of graphene oxide nanosheets and SrFO nanoparticles due to the hydrophobic effect and π-π interaction between rGO nanosheets. The microwave absorbability of products with the different of SrFO contents were tested in the frequency range of2-18GHz. The results show that the product with weight ratios of10:4for GO to SrFO exhibits strongest wave absorption performance. The maximum absorption reaches51dB at frequency of3GHz, and the widest absorption band (RL≤-10dB) is10.5GHz, corresponding to a matching thin thickness of1mm. It is evidently that the3D porous structure of composite hydrogel plays an important role in cavity resonator and lowers microwave reflectivity. It is a way to design and prepare3D porous lightweight and high performance electromagnetic wave absorption materials based on graphene and other nanomaterials.
结合目前高分子/无机复合材料以及石墨烯在微波吸收和电磁屏蔽领域的应用优势,我们制备了不同形貌、不同维数的的PANI/铁氧体纳米复合物,包括一维的PANI/镍锌铁氧体(NZFO)复合纳米棒,二维PANI/NZFO和PANI/'锶铁氧体(SrFO)/氧化石墨烯(GO)纳米片、三维多孔结构还原氧化石墨烯(rGO)/SrFO复合水凝胶,并研究了它们的微波吸收性能。具体研究内容如下：
1.利用两步法成功地制备了PANI/NZFO片状纳米复合物。首先用超声辅助氧化聚合的方法合成了PANI纳米片,然后以此为模板,在水热条件下诱导PANI/NZFO复合纳米片的形成。研究发现,尺寸大小约为18nm左右的NZFO颗粒覆盖在PANI纳米片表面,这主要是由于PANII的氮原子与NZFO中的金属离子(铁、镍或锌离子)配位作用的结果。复合物纳米片的微波吸收性能相对于单一铁氧体或者PANI、片均有明显提高,该类复合物在微波吸收材料领域有潜在的应用前景。
2.首次将超声和外磁场引导相结合,原位聚合法成功制备了新颖的一维PANI/NZFO杂化纳米棒。所制备纳米棒具有均匀的形貌、可调的磁性能,较高的比饱和磁化强度和矫顽力。电磁性能测试表明,杂化纳米棒比纯的NZFO具有更高的反射损耗和更宽的微波吸收带。当NZFO含量为59%、涂层厚度为2mm时,在6.2GHz处复合纳米棒存在微波最大反射损耗(RL),达到-27.5dB；最大吸收带宽(RL≤10dB)为8.1GHz。我们还进一步探讨了杂化纳米棒的吸波机理。
3.以GO片为软模板,利用原位聚合的方法合成了PANI/SrFO/GO复合纳米片。SrFO纳米颗粒均匀分布在GO片上,形成粘附层结构。我们初步探讨了这种结构的形成机理,认为PANI、SrFO颗粒与GO片之间既有配位作用,又有氢键和π-π相互作用。产物的微波性能测试表明,当原材料中苯胺、GO和SrFO的质量比分别是10：5：5和10：5：10时,对应的产物PANI/SrFO/GO-1和PANI/SrFO/GO-2都具有优异的电磁波损耗性能,分别在9.1和6.4GHz处达最大吸收值37dB左右,在2-18GHz频段内-10dB带宽都超过10GHz。
4.利用石墨烯片之间的疏水作用和π-π堆积作用,水热还原制备了三维多孔结构的rGO/SrFO复合水凝胶。结果显示,随着SrFO含量的增加,rGO/SrFO复合水凝胶吸波性能呈现明显增强趋势。当原材料GO和SrFO的质量比为10:4时,lmm厚度下,在3GHz处RL达到最大值-51dB；低于-10dB的损耗带宽达到10.5GHz。这说明了我们所制备的三维rGO/SrFeO复合水凝胶具有非常优异的微波吸收性能,这可能是由于凝胶的孔隙类似于一个微波谐振腔,微波在孔隙形成共振而减少反射率。这为设计和组装新型三维多孔、轻质、高强度、宽频段微波吸收材料提供了启示。
In recent years, with the fast development of information technology, the electromagnetic pollution is worsening, which affects the normal running of the electronic equipment and interferes with the radar, broadcast services, and satellite digital data transmission sharply. Therefore, the electromagnetic pollution is getting more and more attention of all countries. Now, the research and development of a new type of microwave absorption material with a cheap price, effective microwave absorption and wide-band frequency become the important direction of electromagnetic wave absorption materials. Polyaniline (PANI) is one of the most promising conducting polymers with excellent chemical stability, simple synthesis method, easy obtainment of the raw material, and high electrical conductivity. The composites containing PANI and ferrite nanoparticles have the advantages of both polymer and ferrite inorganic materials, and novel performance, and they are a type of multi-functional material.
Based on the application advantages of polymer/inorganic materials and graphene, in the dissertation, PANI/ferrite/(grapheme) or graphene/ferrite composite nanomaterials with different morphologies and dimensions have been synthesized, including one-dimensional (ID) PANI/Ni0.5Zn0.5Fe2O4(NZFO) hybrid nanorods,2D PANI/NZFO and PANI/GO/SrFe12O16(SrFO) composite nanoslices, and3D porous rGO/SrFO composite hydrogel. Their electromagnetic wave absorption properties were also investigated.
The main results can be summarized as follows:
1. PANI/NZFO ferrite composite nanoslices were successfully prepared by two steps. Firstly pure PANI nanoslices were synthesized via ultrasound assisted chemically oxidative polymerization. Then the nanoslices were used as templates to induce the formation of PANI/NZFO composites under hydrothermal conditions. The investigation results indicate that PANI nanoslices were coated by the NZFO nanoparticals with average size of18nm, and there exists the coordination interaction between M2+(M=Fe, Ni, Zn) on the surface of NZFO nanoparticles and PANI. The PANI/NZFO composite nanoslices show better microwave absorption properties than pure PANI or pure NZFO. These composite materials may be applied in microwave absorption and electromagnetic interference shielding fields.
2. The novel uniform PANI/NZFO one-dimensional (ID) hybrid nanorods were firstly in situ synthesized by ultrasonic-assisted magnetic field guidance methods. The as-synthesized hybrid nanorods possess uniform shape, adjusted magnetic properties, high saturated magnetization and high coercivity. The electromagnetic data demonstrate that hybrid nanorods present stronger reflection loss and a wider absorption band in comparison to pure NZFO. PANI/NZFO hybrid nanorods with addition of59%NZFO exhibit excellent microwave absorption performances, with a maximum reflection loss (RL) of-27.5dB observed at6.2GHz, and the widest absorption band (RL<-10dB) is8.1GHz, corresponding to a matching thin thickness of2mm. Besides, microwave absorption mechanism of hybrid nanorods was explored further.
3. Using GO nanosheets as soft template, the PANI/SrFO/GO composite nanoflakes were in situ synthesized by chemical oxidation polymorization method. The results show that SrFO nanoparticles and PANI were tightly bound to the surface of graphene sheets to form interlayer structure. The formation mechanism of the as-synthesized composites was discussed. The coordination effect, π-π interaction and hydrogen bonding exist among polyaniline, SrFO nanoparticles and graphene nanosheets. The microwave performance measurement of the products shows that PANI/SrFO/GO-1(weight ratio of aniline/GO/SrFO is10:5:5) and PANI/SrFO/GO-2(weight ratio of aniline/GO/SrFO is10:5:10) both possess excellent electromagnetic loss performances, with a maximum absorption value of about37dB at9.1and6.4 GHz, respectively. And their-10dB bandwidth surpassed10GHz in2-18GHz ranges.
4. A novel3D porous rGO/SrFO composite hydrogel was synthesized by one step hydfothermal method in the presence of graphene oxide nanosheets and SrFO nanoparticles due to the hydrophobic effect and π-π interaction between rGO nanosheets. The microwave absorbability of products with the different of SrFO contents were tested in the frequency range of2-18GHz. The results show that the product with weight ratios of10:4for GO to SrFO exhibits strongest wave absorption performance. The maximum absorption reaches51dB at frequency of3GHz, and the widest absorption band (RL≤-10dB) is10.5GHz, corresponding to a matching thin thickness of1mm. It is evidently that the3D porous structure of composite hydrogel plays an important role in cavity resonator and lowers microwave reflectivity. It is a way to design and prepare3D porous lightweight and high performance electromagnetic wave absorption materials based on graphene and other nanomaterials.
引文
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