负载型复合纳米材料的制备及其吸波性能研究
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摘要
吸波材料一直是国防科技和功能材料领域的研究热点。但是,迄今为止,很难找到可在宽频范围内同时满足阻抗匹配特性和强吸收要求的单组元吸波剂材料。因此,国际上在研究吸波效能更高的吸波剂方面形成了一条共识性的思路——吸波剂组成上的复合化。由于负载型复合可提升不同组元间的复配均匀性和稳定性,因而逐步发展成了一种备受关注的吸波剂复合化设计与制备方法。本文制备了三类负载型复合纳米材料,并分别对其控制合成、电磁学和吸波性能进行了研究。在此基础上,分析了三类产物微观结构和物质组成的共通性及其吸波性能的一致性规律,分析和提出了负载型复合纳米材料的多重吸波机制。
建立了一种原位合成方法及其配套热处理技术,实现了磁性纳米粒子在四针状氧化锌晶须(T-ZnOw)表面的均匀负载和磁性粒子成分的可控,制备出了负载型复合产物M-ZnOw及其中间产物Semis.揭示了在Semis的原位合成过程中,聚乙二醇(PEG)既通过物理吸附作用与T-ZnOw结合,又通过氢键和配位键作用而与氧化铁粒子结合,在T-ZnOw和氧化铁粒子之间发挥了桥联作用。电磁学性能研究结果表明：T-ZnOw无磁性,对入射电磁波不具有磁损耗能力。但铁含量高于2wt%、磁性成分为Fe304的M-ZnOw表现铁磁性,具有磁滞损耗、自然共振损耗和交换共振损耗等磁损耗性能。此外,双复介质Fe304在T-ZnOw表面的均匀负载,还使M-ZnOw表现出了优于T-ZnOw的介电损耗能力,其tanδE值明显高于T-ZnOw.吸波性能和吸波机理研究结果表明：在2-18GHz范围内,M-ZnOw表现出了明显优于T-ZnOw的吸波性能,且其吸波性能受铁含量和负载复合均匀性影响。在2-16wt%的研究范围内,铁含量为9wt%的M-ZnOw产物具有最优的吸波性能；具有均匀负载效果的M-ZnOw产物的吸波性能优于非均匀负载的M-ZnOw产物。M-ZnOw表现出了优于与其具有相同组成的简单复合物的吸波性能。M-ZnOw除了具有其构成组元的本征电、磁损耗机制之外,由于其负载复合结构,还可提升纳米损耗效应的发挥和引入异质界面吸波新机制。
采用化学镀及其后续热处理(N2气氛、450℃、4h)技术,实现了纳米Ni-P镀层在碳纳米管(CNTs)表面的负载复合和镀层晶体结构的可控调节,制备了负载型复合纳米材料P-CNTs(负载非晶态Ni-P镀层)和HT-CNTs(负载多晶态的Ni和Ni3P粒子)。通过对纯化和化学镀工艺时间的调控,实现了对P-CNTs产物的微观形貌、负载复合均匀性及负载层厚度的可控。由不同的P-CNTs产物热处理而制备的HT-CNTs产物之间的负载复合均匀性差异与其对应的P-CNTs产物的负载复合均匀性差异相一致。电磁学性能研究结果表明：与原料CNTs相比,P-CNTs产物的电阻损耗性能降低,介电损耗性能在较高频段有所降低,但在较低频段有所增大；P-CNTs为顺磁性物质,具有一定的磁化损耗能力。当P-CNTs通过热处理工艺而转变为HT-CNTs产物后,其tanδE值在全频段范围内高于CNTs,且其tanδM值相对于P-CNTs有进一步的提升,同时HT-CNTs还表现出了磁滞损耗性能。吸波性能和吸波机理研究结果表明：通过负载型复合,能一定程度改善CNTs的吸波性能。更好的负载复合均匀性有利于P-CNTs和HT-CNTs产物的异质界面吸波机制和纳米损耗效应的发挥,从而使产物在更宽的频带范围内具有更好的吸波效果。
通过化学氧化法合成了8042-掺杂的无定形结构的聚吡咯(PPy),通过原位合成方法制备了PEG/Fe3O4水基磁流体。在此基础上,建立了具有核-壳结构的Fe3O4/PPy复合产物的一种软模板合成方法。在所合成的Fe3O4/PPy复合产物中,PPy为无定形结构,Fe304为结晶体,部分PPy分子上的N原子与Fe304中的部分Fe原子之间形成了配位结合。通过在合成反应体系中加入乙腈和逐步增大乙腈用量,实现了对Fe3O4/PPy复合产物的微观形貌、铁含量以及电导率等宏微观参数的综合调控。当腈水比为0：10-3：7时,得到的Fe3O4/PPy产物的微观形貌为单一颗粒状,当腈水比增大到4：6-5：5时,产物表现出具有明显粒径差异的大、小两种颗粒(分别是500nIn左右的核-壳结构Fe3O4/PPy大粒子和70nm左右的本征态PPy小粒子)共存的微观形貌。随着腈水比的逐渐增大,Fe3O4/PPy复合产物的铁含量逐步增大,电导率逐步降低。分析提出了基于吡咯在PEG/Fe3O4胶粒表层和表面以及乙腈胶束内聚合相结合的Fe3O4/PPy产物的合成机理,阐明了系列Fe3O4/PPy产物的宏微观参数的受控机制。电磁学和吸波性能研究结果表明：尽管具有核-壳结构的Fe3O4/PPy复合产物S0的电、磁损耗正切值较PPy并不占优,其在2～18GHz范围内的吸波性能却明显优于PPy。这主要归因于SO产物的核-壳结构有助于提升PPy和Fe304两种吸波组元间的电、磁损耗机制的匹配和互补效应。在系列Fe3O4/PPy产物中,SO产物(其铁含量为5.59wt%)由于其核-壳结构复合效果最佳、PPy分子掺杂程度高和产物电导率最大,表现出了最大的tanδE值以及与Fe含量最高(14.69wt%)的S5产物相当的tanδM值,并在2-18GHz范围内表现出最优的吸波性能,这一方面归因于其本征电、磁损耗机制的匹配与互补效应,另一方面源自其最优的核-壳结构复合效果与最佳的纳米颗粒分散性更有利于促进异质界面吸波效应和纳米损耗效应的充分发挥。
对N-ZnOw、HT-CNTs和Fe3O4/PPy三类负载型复合纳米材料的微观结构、物质组成方的共通性以及其吸波性能和吸波机制方面的一致性规律进行了综合分析,并通过理论分析提出了三类负载型复合纳米材料具有其构成组元的本征电、磁损耗效应和由于负载复合结构而提升或新引入的纳米损耗效应和异质界面损耗效应相结合的多重电磁波损耗机制。分析指出异质界面吸波机制是负载型复合吸波剂区别于单组元吸波剂和简单复合型吸波剂的特有吸波新机制,它可通过增大负载型复合纳米材料的电损耗和磁损耗能力来一定程度的体现。
Microwave absorbing materials have always been a research focus in the fields of national defense technology and functional materials. However, it is quite difficult to find an individual material to meet the requirement of impedance matching and strong absorption capability simultaneously in a broad frequency band. Therefore, a common thought of composite preparation for microwave absorption has been gradually formed in the international range. Among the absorbing composites, one kind of composites with the loading of one component on the surface of another component is more beneficial to improve the composite uniformity and stability between different components, so the loading structured composite has gradually become a focus for the design and preparation of absorbing composite. Three kinds of loading structured nano composites were prepared in this thesis and their controllable synthesis, electromagnetic and microwave absorbing behaviors were investigated. Based on the above research, the commonality of the morphology, structure, composition and the consistent rule of microwave absorption property of the as-prepared three kinds of loading structured composites were analyzed, and the multi-mechanism for microwave absorption of the loading structured nanoscale composites was developed.
Nanoscaled magnetic particles were uniformly loaded on the surface of tetra-needle like ZnO whisker(abbr. T-ZnOw) and the composition of the particles was controlled by an in situ synthesis and heat treatment method. The loading structured product of M-ZnOw and its intermediate product (noted as Semis) were obtained. The study on the in situ synthesis mechanism showed that plolyethylene glycol(abbr. PEG) played the role of bridging T-ZnOw and nanoscaled magnetic particles through the hydrogen bond and coordinate combination between iron oxide particles and PEG molecule as well as the physical absorption between T-ZnOw and PEG molecule. As shown in the electromagnetic properties, T-ZnOw had no magnetic property and couldn't attenuate the energy of microwave by magnetic loss; M-ZnOw with a magnetic component of Fe3O4and an iron content over than2wt%appeared ferromagnetic property and could absorb microwave through such magnetic loss mechanisms as magnetic hysteresis loss, natural magnetic resonance loss and exchange magnetic resonance loss. In addition, M-ZnOw appeared much better dielectric loss property than T-ZnOw because the double-complex medium of Fe3O4was loaded on the surface of T-ZnOw, and the dielectric loss tangent (tanδE) of M-ZnOw was obviously greater than that of T-ZnOw. Also, M-ZnOw appeared obviously stronger absorbing ability than T-ZnOw in the frequency band of2-18GHz. The absorbing behavior of M-ZnOw was influenced by the iron content and loading uniformity. M-ZnOw with an iron content of9wt%showed the best absorbing property in the researched iron content range of2-16wt%, and M-ZnOw with uniform loading composite effect showed superiorer absorbing capability to that with irregular loading effect. Furthermore, M-ZnOw appeared higher absorbing capability than the handcrafted composite which had the same composition and component contents as M-ZnOw. As far as the microwave absorbing mechanisms of M-ZnOw were concerned, it was concluded that besides the intrinsic electric and magnetic loss mechanisms resulting from the components in M-ZnOw, nano loss effect was improved and heterogenous interface loss effect was brought to M-ZnOw because of its loading composite structure.
Nanoscaled Ni-P plating was coated on the surface of carbon nanotubes (CNTs) and the crystal structure of the plating was adjusted by an electroless plating and heat treatment (N2,450℃,4h) method. Thus, the loading structured products of P-CNTs (with amorphous Ni-P plating) and HT-CNTs (with polycrystalline Ni and Ni3P plating) were obtained. Moreover, the morphology, loading uniformity and plating thickness of P-CNTs were controlled by adjusting the process time of purification and electroless plating. Further study indicated that different HT-CNTs prepared through heat treatment of different P-CNTs showed a consistent difference on loading uniformity as their corresponding P-CNTs. The electromagnetic properties showed that P-CNTs appeared lower resistive loss than CNTs; the dielectric loss of P-CNTs was lower or higher than that of CNTs respectively in the relatively high or low frequency band. P-CNTs was paramagnetic materials and had magnetization loss property to a certain extent. As P-CNTs was heat treated and transformed to HT-CNTs, the tan δE was higher than that of CNTs in the whole frequency band of2-18GHz, and the magnetic loss tangent (tan δM) was further increased compared with P-CNTs, and magnetic hysteresis loss effect was also obtained. Further study showed that the absorbing property of CNTs could be improved to a certain extent through loading structured composite, and better uniformity of loading composite was more beneficial to the increase of heterogenous interface loss effect and nano loss effect, which finally leaded the P-CNTs and HT-CNTs products to appear much stronger absorption in much wider frequency band.
Amorphous polypyrrole (PPy) doped with SO42-was synthesized by a chemical oxidation method and PEG/Fe3O4water-based ferrofluid was prepared through an in situ synthesis method. Furthermore, core-shell structured Fe3O4/PPy composite was prepared by a soft-template synthesis method esatbolished in this thesis. In this special loading structured composite, PPy was still amorphous and Fe3O4was crystalline, and coordinate combination was formed between some N atoms of PPy and some Fe atoms of Fe3O4. the morphology, iron content and conductivity of Fe3O4/PPy composite was controlled by adding acetonitrile into the reaction mixture and gradually rising the content of acetonitrile. When the volume ratio of acetonitrile to water (abbr. VRAW) was in the range of0:10-3:7, the prepared Fe3O4/PPy composites were in the morphology of particles with uniform diameter. However, when VRAW was further increased to4:6-5:5, the obtained Fe3O4/PPy composites were in the morphology of two kinds of particles which had obviously different diameter (the large particles were core-shell structured Fe3O4/PPy in diameter of about500nm, and the small particles were intrinsic PPy in diameter of about70nm). As the gradual increase of VRAW, the iron content and conductivity of the as-prepared Fe3O4/PPy composites were gradually increased and decreased, respectively. The synthesis mechanism of Fe3O4/PPy composites based on the combination of pyrrole's polymerization at the surface and surface layer of PEG/Fe3O4colloidal particles and in the acetonitrile micells was put forward. Moreover, the controllable mechanism of the macro and micro parameters of the as-prepared Fe3O4/PPy composites was theoretically clarified by the proposed synthesis mechanism. As the further study shown, although the dielectric and magnetic loss tangent of SO were not superior to that of PPy, the core-shell structured Fe3O4/VPPy product of SO appeared obviously better absorbing property than pure PPy, which was mainly attributed to the core-shell structure of SO redounded to improve matching and complementary effects of electric and magnetic loss which were resulted from PPy and Fe3O4, respectively. Among the prepared Fe3O4/PPy products, SO (with an iron content of5.59wt%) showed the highest tanδE and the comparable tanδM to S5which had the highest iron content (14.69wt%) because SO had the best core-shell composite effect, a high doping degree of PPy molecular and the largest conductivity. SO also appeared the best microwave absorbing behavior among the as prepared Fe3O4/PPy composites in2-18GHz, which was attributed to its best matching and complementary effects of electric and magnetic loss as well as the improvement of its best core-shell composite effect and dispersion property of nano particles to the heterogenous interface absorbing effect and nano loss effect.
Multi-mechanism for microwave absorption of loading structured nano composite were analyzed and brought forward through the comparison and investigation on the commonality of micro structure and composition as well as the consistent rule of the as-prepared three kinds of loading structured composites (M-ZnOw, HT-CNTs and Fe3O4/PPy), which were concluded as the combination of intrinsic electric and magnetic loss effects resulted from the composite components with the improved or newly induced absorption mechanisms of nano loss effect and heterogenous interface loss effect. Heterogeneous interface absorbing mechanism was a peculiar absorbing mechanism that loading composite absorber differed from single component absorber and handcrafted composite absorber, which could be embodied to a certain extent through enhancing electric and magnetic loss of the loading composite absorber.
建立了一种原位合成方法及其配套热处理技术,实现了磁性纳米粒子在四针状氧化锌晶须(T-ZnOw)表面的均匀负载和磁性粒子成分的可控,制备出了负载型复合产物M-ZnOw及其中间产物Semis.揭示了在Semis的原位合成过程中,聚乙二醇(PEG)既通过物理吸附作用与T-ZnOw结合,又通过氢键和配位键作用而与氧化铁粒子结合,在T-ZnOw和氧化铁粒子之间发挥了桥联作用。电磁学性能研究结果表明：T-ZnOw无磁性,对入射电磁波不具有磁损耗能力。但铁含量高于2wt%、磁性成分为Fe304的M-ZnOw表现铁磁性,具有磁滞损耗、自然共振损耗和交换共振损耗等磁损耗性能。此外,双复介质Fe304在T-ZnOw表面的均匀负载,还使M-ZnOw表现出了优于T-ZnOw的介电损耗能力,其tanδE值明显高于T-ZnOw.吸波性能和吸波机理研究结果表明：在2-18GHz范围内,M-ZnOw表现出了明显优于T-ZnOw的吸波性能,且其吸波性能受铁含量和负载复合均匀性影响。在2-16wt%的研究范围内,铁含量为9wt%的M-ZnOw产物具有最优的吸波性能；具有均匀负载效果的M-ZnOw产物的吸波性能优于非均匀负载的M-ZnOw产物。M-ZnOw表现出了优于与其具有相同组成的简单复合物的吸波性能。M-ZnOw除了具有其构成组元的本征电、磁损耗机制之外,由于其负载复合结构,还可提升纳米损耗效应的发挥和引入异质界面吸波新机制。
采用化学镀及其后续热处理(N2气氛、450℃、4h)技术,实现了纳米Ni-P镀层在碳纳米管(CNTs)表面的负载复合和镀层晶体结构的可控调节,制备了负载型复合纳米材料P-CNTs(负载非晶态Ni-P镀层)和HT-CNTs(负载多晶态的Ni和Ni3P粒子)。通过对纯化和化学镀工艺时间的调控,实现了对P-CNTs产物的微观形貌、负载复合均匀性及负载层厚度的可控。由不同的P-CNTs产物热处理而制备的HT-CNTs产物之间的负载复合均匀性差异与其对应的P-CNTs产物的负载复合均匀性差异相一致。电磁学性能研究结果表明：与原料CNTs相比,P-CNTs产物的电阻损耗性能降低,介电损耗性能在较高频段有所降低,但在较低频段有所增大；P-CNTs为顺磁性物质,具有一定的磁化损耗能力。当P-CNTs通过热处理工艺而转变为HT-CNTs产物后,其tanδE值在全频段范围内高于CNTs,且其tanδM值相对于P-CNTs有进一步的提升,同时HT-CNTs还表现出了磁滞损耗性能。吸波性能和吸波机理研究结果表明：通过负载型复合,能一定程度改善CNTs的吸波性能。更好的负载复合均匀性有利于P-CNTs和HT-CNTs产物的异质界面吸波机制和纳米损耗效应的发挥,从而使产物在更宽的频带范围内具有更好的吸波效果。
通过化学氧化法合成了8042-掺杂的无定形结构的聚吡咯(PPy),通过原位合成方法制备了PEG/Fe3O4水基磁流体。在此基础上,建立了具有核-壳结构的Fe3O4/PPy复合产物的一种软模板合成方法。在所合成的Fe3O4/PPy复合产物中,PPy为无定形结构,Fe304为结晶体,部分PPy分子上的N原子与Fe304中的部分Fe原子之间形成了配位结合。通过在合成反应体系中加入乙腈和逐步增大乙腈用量,实现了对Fe3O4/PPy复合产物的微观形貌、铁含量以及电导率等宏微观参数的综合调控。当腈水比为0：10-3：7时,得到的Fe3O4/PPy产物的微观形貌为单一颗粒状,当腈水比增大到4：6-5：5时,产物表现出具有明显粒径差异的大、小两种颗粒(分别是500nIn左右的核-壳结构Fe3O4/PPy大粒子和70nm左右的本征态PPy小粒子)共存的微观形貌。随着腈水比的逐渐增大,Fe3O4/PPy复合产物的铁含量逐步增大,电导率逐步降低。分析提出了基于吡咯在PEG/Fe3O4胶粒表层和表面以及乙腈胶束内聚合相结合的Fe3O4/PPy产物的合成机理,阐明了系列Fe3O4/PPy产物的宏微观参数的受控机制。电磁学和吸波性能研究结果表明：尽管具有核-壳结构的Fe3O4/PPy复合产物S0的电、磁损耗正切值较PPy并不占优,其在2～18GHz范围内的吸波性能却明显优于PPy。这主要归因于SO产物的核-壳结构有助于提升PPy和Fe304两种吸波组元间的电、磁损耗机制的匹配和互补效应。在系列Fe3O4/PPy产物中,SO产物(其铁含量为5.59wt%)由于其核-壳结构复合效果最佳、PPy分子掺杂程度高和产物电导率最大,表现出了最大的tanδE值以及与Fe含量最高(14.69wt%)的S5产物相当的tanδM值,并在2-18GHz范围内表现出最优的吸波性能,这一方面归因于其本征电、磁损耗机制的匹配与互补效应,另一方面源自其最优的核-壳结构复合效果与最佳的纳米颗粒分散性更有利于促进异质界面吸波效应和纳米损耗效应的充分发挥。
对N-ZnOw、HT-CNTs和Fe3O4/PPy三类负载型复合纳米材料的微观结构、物质组成方的共通性以及其吸波性能和吸波机制方面的一致性规律进行了综合分析,并通过理论分析提出了三类负载型复合纳米材料具有其构成组元的本征电、磁损耗效应和由于负载复合结构而提升或新引入的纳米损耗效应和异质界面损耗效应相结合的多重电磁波损耗机制。分析指出异质界面吸波机制是负载型复合吸波剂区别于单组元吸波剂和简单复合型吸波剂的特有吸波新机制,它可通过增大负载型复合纳米材料的电损耗和磁损耗能力来一定程度的体现。
Microwave absorbing materials have always been a research focus in the fields of national defense technology and functional materials. However, it is quite difficult to find an individual material to meet the requirement of impedance matching and strong absorption capability simultaneously in a broad frequency band. Therefore, a common thought of composite preparation for microwave absorption has been gradually formed in the international range. Among the absorbing composites, one kind of composites with the loading of one component on the surface of another component is more beneficial to improve the composite uniformity and stability between different components, so the loading structured composite has gradually become a focus for the design and preparation of absorbing composite. Three kinds of loading structured nano composites were prepared in this thesis and their controllable synthesis, electromagnetic and microwave absorbing behaviors were investigated. Based on the above research, the commonality of the morphology, structure, composition and the consistent rule of microwave absorption property of the as-prepared three kinds of loading structured composites were analyzed, and the multi-mechanism for microwave absorption of the loading structured nanoscale composites was developed.
Nanoscaled magnetic particles were uniformly loaded on the surface of tetra-needle like ZnO whisker(abbr. T-ZnOw) and the composition of the particles was controlled by an in situ synthesis and heat treatment method. The loading structured product of M-ZnOw and its intermediate product (noted as Semis) were obtained. The study on the in situ synthesis mechanism showed that plolyethylene glycol(abbr. PEG) played the role of bridging T-ZnOw and nanoscaled magnetic particles through the hydrogen bond and coordinate combination between iron oxide particles and PEG molecule as well as the physical absorption between T-ZnOw and PEG molecule. As shown in the electromagnetic properties, T-ZnOw had no magnetic property and couldn't attenuate the energy of microwave by magnetic loss; M-ZnOw with a magnetic component of Fe3O4and an iron content over than2wt%appeared ferromagnetic property and could absorb microwave through such magnetic loss mechanisms as magnetic hysteresis loss, natural magnetic resonance loss and exchange magnetic resonance loss. In addition, M-ZnOw appeared much better dielectric loss property than T-ZnOw because the double-complex medium of Fe3O4was loaded on the surface of T-ZnOw, and the dielectric loss tangent (tanδE) of M-ZnOw was obviously greater than that of T-ZnOw. Also, M-ZnOw appeared obviously stronger absorbing ability than T-ZnOw in the frequency band of2-18GHz. The absorbing behavior of M-ZnOw was influenced by the iron content and loading uniformity. M-ZnOw with an iron content of9wt%showed the best absorbing property in the researched iron content range of2-16wt%, and M-ZnOw with uniform loading composite effect showed superiorer absorbing capability to that with irregular loading effect. Furthermore, M-ZnOw appeared higher absorbing capability than the handcrafted composite which had the same composition and component contents as M-ZnOw. As far as the microwave absorbing mechanisms of M-ZnOw were concerned, it was concluded that besides the intrinsic electric and magnetic loss mechanisms resulting from the components in M-ZnOw, nano loss effect was improved and heterogenous interface loss effect was brought to M-ZnOw because of its loading composite structure.
Nanoscaled Ni-P plating was coated on the surface of carbon nanotubes (CNTs) and the crystal structure of the plating was adjusted by an electroless plating and heat treatment (N2,450℃,4h) method. Thus, the loading structured products of P-CNTs (with amorphous Ni-P plating) and HT-CNTs (with polycrystalline Ni and Ni3P plating) were obtained. Moreover, the morphology, loading uniformity and plating thickness of P-CNTs were controlled by adjusting the process time of purification and electroless plating. Further study indicated that different HT-CNTs prepared through heat treatment of different P-CNTs showed a consistent difference on loading uniformity as their corresponding P-CNTs. The electromagnetic properties showed that P-CNTs appeared lower resistive loss than CNTs; the dielectric loss of P-CNTs was lower or higher than that of CNTs respectively in the relatively high or low frequency band. P-CNTs was paramagnetic materials and had magnetization loss property to a certain extent. As P-CNTs was heat treated and transformed to HT-CNTs, the tan δE was higher than that of CNTs in the whole frequency band of2-18GHz, and the magnetic loss tangent (tan δM) was further increased compared with P-CNTs, and magnetic hysteresis loss effect was also obtained. Further study showed that the absorbing property of CNTs could be improved to a certain extent through loading structured composite, and better uniformity of loading composite was more beneficial to the increase of heterogenous interface loss effect and nano loss effect, which finally leaded the P-CNTs and HT-CNTs products to appear much stronger absorption in much wider frequency band.
Amorphous polypyrrole (PPy) doped with SO42-was synthesized by a chemical oxidation method and PEG/Fe3O4water-based ferrofluid was prepared through an in situ synthesis method. Furthermore, core-shell structured Fe3O4/PPy composite was prepared by a soft-template synthesis method esatbolished in this thesis. In this special loading structured composite, PPy was still amorphous and Fe3O4was crystalline, and coordinate combination was formed between some N atoms of PPy and some Fe atoms of Fe3O4. the morphology, iron content and conductivity of Fe3O4/PPy composite was controlled by adding acetonitrile into the reaction mixture and gradually rising the content of acetonitrile. When the volume ratio of acetonitrile to water (abbr. VRAW) was in the range of0:10-3:7, the prepared Fe3O4/PPy composites were in the morphology of particles with uniform diameter. However, when VRAW was further increased to4:6-5:5, the obtained Fe3O4/PPy composites were in the morphology of two kinds of particles which had obviously different diameter (the large particles were core-shell structured Fe3O4/PPy in diameter of about500nm, and the small particles were intrinsic PPy in diameter of about70nm). As the gradual increase of VRAW, the iron content and conductivity of the as-prepared Fe3O4/PPy composites were gradually increased and decreased, respectively. The synthesis mechanism of Fe3O4/PPy composites based on the combination of pyrrole's polymerization at the surface and surface layer of PEG/Fe3O4colloidal particles and in the acetonitrile micells was put forward. Moreover, the controllable mechanism of the macro and micro parameters of the as-prepared Fe3O4/PPy composites was theoretically clarified by the proposed synthesis mechanism. As the further study shown, although the dielectric and magnetic loss tangent of SO were not superior to that of PPy, the core-shell structured Fe3O4/VPPy product of SO appeared obviously better absorbing property than pure PPy, which was mainly attributed to the core-shell structure of SO redounded to improve matching and complementary effects of electric and magnetic loss which were resulted from PPy and Fe3O4, respectively. Among the prepared Fe3O4/PPy products, SO (with an iron content of5.59wt%) showed the highest tanδE and the comparable tanδM to S5which had the highest iron content (14.69wt%) because SO had the best core-shell composite effect, a high doping degree of PPy molecular and the largest conductivity. SO also appeared the best microwave absorbing behavior among the as prepared Fe3O4/PPy composites in2-18GHz, which was attributed to its best matching and complementary effects of electric and magnetic loss as well as the improvement of its best core-shell composite effect and dispersion property of nano particles to the heterogenous interface absorbing effect and nano loss effect.
Multi-mechanism for microwave absorption of loading structured nano composite were analyzed and brought forward through the comparison and investigation on the commonality of micro structure and composition as well as the consistent rule of the as-prepared three kinds of loading structured composites (M-ZnOw, HT-CNTs and Fe3O4/PPy), which were concluded as the combination of intrinsic electric and magnetic loss effects resulted from the composite components with the improved or newly induced absorption mechanisms of nano loss effect and heterogenous interface loss effect. Heterogeneous interface absorbing mechanism was a peculiar absorbing mechanism that loading composite absorber differed from single component absorber and handcrafted composite absorber, which could be embodied to a certain extent through enhancing electric and magnetic loss of the loading composite absorber.
引文
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