聚芳醚酮基杂化吸波材料的制备及性能研究
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摘要
近几十年来，随着无线通信和高频电路器件的发展，电磁干扰成为一种新型的环境污染形式出现在人们的生活中，对通信设备、国防军事设施和人类的健康造成了极大的威胁和损害。因此，开发轻质、高效的电磁屏蔽材料是必要且迫在眉睫的。微波吸收材料作为一种重要的屏蔽材料，能够有效地解决不断扩大的电磁干扰。但是现有的、单一的材料难以实现高效的吸收以及满足运行环境的苛刻要求，人们迫切希望开发高效、轻质、稳定的吸波材料来解决这一重要问题。本论文中，我们以聚芳醚酮树脂为基体，先后探索了以“二氧化硅/磁性纳米粒子”、“聚苯胺/磁性粒子”以及“空心微球”等复合粒子作为吸波剂用于合成高性能的杂化微波吸收材料，成功地制备出综合性能优良的聚芳醚树脂基杂化微波吸收材料，并对其微波吸收性能和机理进行了研究，最终实现制备高性能的新型微波吸收材料这一目标。
第一，我们合成了“二氧化硅/磁性纳米粒子”以及具有活性反应基团的氨基聚芳醚酮，用于合成Co0.2Fe2.8O4@SiO2-聚芳醚酮磁性杂化材料，以3-异氰酸丙基三乙氧基硅烷为偶联剂，通过O-酰化反应与溶胶-凝胶过程，有效调控填料的尺寸、形貌以及分布。该杂化材料两相间具有良好的相容性，表现出了优异的透明性以及很好的微波吸收性能。
第二，我们合成了“聚苯胺/磁性粒子”以及氨基聚芳醚酮，以耐高温的醛基封端聚甲亚胺齐聚物为偶联剂，通过溶胶-凝胶法制备Fe3O4@聚苯胺/聚甲亚胺/聚芳醚酮三元杂化材料。该材料具有快的交联速度以及均匀的尺寸分布，并展示出较宽的微波吸收频带和较高的反射损耗。
第三，合成具有空心结构的复合微球，并结合以上工作基础，进一步将这些微球与聚芳醚酮基体复合，通过溶胶-凝胶法制备空心微球/聚芳醚酮多孔杂化材料。研究了微球结构吸波剂以及多孔结构杂化材料对吸波性能的影响，制备出了高效、轻质、耐高温以及环境耐受性强的微波吸收材料，并得到了很好的吸波性能。
Due to the fast development of electronic devices such as wireless communications andhigh-frequency circuit devices in the recent decades, electromagnetic interferenceemerges as a novel kind of pollution to the environment, which disturbs the stableworking conditions of electronic appliances and may harm the human body.Microwave-absorbing materials are of great interests as an important and crucialtechnology in solving the expanding electromagnetic interference. Materials such asferrites, conductive polymers, carbon, metals and their oxides have been intensivelyinvestigated, due to their significant contribution to radar stealth and electromagneticinterference shielding. However, with the increasing demands of usage in diverse andcomplex environment, it is urgently to develop high-performance microwave-absorbingmaterials with multifunction, such lightweight, efficient, broadband, temperaturestability, corrosion resistance, radiation resistance, and environmentally friendly, etc.The conventional single kind of material is difficult to meet the increasing requirements.Therefore, exploiting polymer-based hybrid materials with superior performanceabsorbers and substrate polymers has aroused considerable concerns for theirlightweight, high efficient, extensive absorption, cellent stability, flexibility and easyprocessing advantages.
Polyaryetherkotone (PAEK) superior engineering thermoplastic is one of the mostideal matrix polymers to improve the comprehensive properties ofmicrowave-absorbing materials with excellent stability to adapt the harsh environment.Attributed to the distinctive aromatic structure of the polymer, the material performs excellent mechanical properties, thermal stability, ammability, radiation resistance,flame and solvent resistance. Moreover, the flexible ether bonds in the moleculestructure also provide a good processing performance as thermoplastic engineeringplastics. What is more, this kind of non-toxic and electrical insulating polymer isregarded as an electromagnetic windows material. However, there is little research onPAEK as the matrix for microwave-absorbing coatings. Mainly because the insolublePAEK increases the difficulties to disperse the absorbers in matrix. In this paper, wedesign and synthesize a new20%amino-functionalized PEEK copolymer containingtrifluoromethyl units on polymer main chains (AFPEEK) from the molecular point ofview. Furthermore, a series of PAEK-based hybird microwave-absorbing materials areprepared by the complex with absorbers with different electromagnetic properties viasol-gel method. And the structures and properties of these hybrid materials are detailedstudied.
First of all, we synthesize Co0.2Fe2.8O4nanoparticles, which are modified withsilica-protected layers to provide reliable chemical stabilization. The Co0.2Fe2.8O4@SiO2nanoparticles are used as the absorbers to prepare Co0.2Fe2.8O4@SiO2-PEEK hybridmicrowave-absorbing materials for their dielectric and magnetic permeability. Inchapter3, a simple and effective in-situ sol-gel technique is used to improvecompatibility and dispersibility between phases.3-isocyanatopropyltriethoxysilane(IPTS) is introduced as a bridge between the hydrophilic nanoparticles absorbers andthe hydrophobic AFPEEK matrix for its high reactivity with SiO2and amino groups onthe side chain of the polymer. SEM and TEM images demonstrate that the stronginteraction between inorganic-organic phases results in great improvement of dispersionand compatibility at even40wt%nanoparticles contents. The functional integration oforganic polymer and inorganic nanoparticles leads to excellent comprehensiveperformances such as high transparency, solvent resistance, thermal stability andmechanical properties of the hybrid material, as well as the high adhesion with substrate,which benefits its application as coating materials. As the amendment of the shape, sizeand distribution of the fillers in the matrix may strongly change the frequencydependence of permeability. This hybrid membrane exhibits good superparamagnetic behaviors and microwave electromagnetic properties (reflecting loss～-13dB at14.3GHz, d=2mm). It is expected as a promising microwave-absorbing material for thefacile synthesis process and good comprehensive properties.
However, due to low complex permittivity and complex permeability, the loss ofelectromagnetic waves for Co0.2Fe2.8O4@SiO2-PEEK hybrid material is limited, whichis difficult to achieve effective absorption of electromagnetic waves in the range of2-18GHz, even adjust the thickness. The emerging conductive polymer and magneticnanoparticle composite materials are under currently concerned as an ideal absorbers fortheir unique physical and chemical properties. Therefore, in chapter4, we improve andregulate the electromagnetic parameters to achieve better matching by the complexabsorbers of polyaniline conductive polymer composition and magnetic iron oxidenanoparticles(Fe3O4@PANI). Furthermore, through a simple and effectiveamine-aldehyde condensation reaction between the aldehyde-terminated PAM oligomercoupling agent and amino groups (on Fe3O4@PANI nanocomposites and AFPEEK), theternary Fe3O4@PANI/PAM/PEEK hybrid materials are prepared via a sol-gel process.The high stability crosslinked hybrid materials performe excellent thermal stability(Tg>160°C, Td-5%>300°C) and solvent resistance, and exhibit significantmicrowave-absorbing property (RL～-18dB at14GHz, d=2mm) with40wt%nanocomposites contents. The primary mechanism of the microwave absorption isdielectric and magnetic loss, while the magnetic Fe3O4is regarded as a promoter toincrease the complex permeability of PANI. The combination of conductive andmagnetic properties enhances the microwave absorption. Therefore, the intensity andbandwidth of the absorption for hybrid materials increase significantly, the hybridmaterials can achieve effective absorption (>90%) within the range of2-18GHz byregulating the thicknes.
Although Fe3O4@PANI/PAM/PEEK hybrid materials exhibit excellent absorbingproperties, there is still a problem about the high filler contents, which makes thedisadvantages such as lightweight and high efficient. Therefore, in chapter5,considering the balanced of the attenuation characteristics and impedance matching, weoptimize the composition and structure of the absorbing materials. PANI/C/Fe3O4 hollow microspheres with high electromagnetic loss are prepared and introduced as themicrowave absorbers to fabricate a series of porous PAEK-based hybrid materials withvarious absorbers contents, according to the method mentioned in previous chapter. It isexcepted to improve the electromagnetic parameters, as well as adjust the impedancematching, in order to achieve lightweight and high absorption of the materials. Thehybrid material exhibits excellent microwave-absorbing behaviors with30wt%fillercontents, attribute to the unique structure and composition. Firstly, the permeabilitycomponents (matrix and porosity) of the material can make as many waves incident onthe surface and transmission in its interior, which reduces reflection losses. Meanwhile,the absorbing components (absorbers) with high electromagnetic parameters providequick and efficient absroption on the waves. Furthermore, the porous structure results inmultiple reflections in and between the microspheres, which greatly increase theelectromagnetic wave transmission path in the material and the friction with theprobability of absorbers. Therefore, the absorption intensity and the bandwidth of thematerials are improved significantly (RL～-32dB,15GHz, d=2mm). And a strongerabsorption can be achieved (>90%) within the range of4.5-18GHz by adjusting thethickness (2mm,3mm,4mm,5mm). In addition, the material also exhibits highthermal stability (Td-5%>510°C, Tg>180°C). This hybrid technique provides a novelroute for preparation of high performance microwave-absorbing materials.
第一，我们合成了“二氧化硅/磁性纳米粒子”以及具有活性反应基团的氨基聚芳醚酮，用于合成Co0.2Fe2.8O4@SiO2-聚芳醚酮磁性杂化材料，以3-异氰酸丙基三乙氧基硅烷为偶联剂，通过O-酰化反应与溶胶-凝胶过程，有效调控填料的尺寸、形貌以及分布。该杂化材料两相间具有良好的相容性，表现出了优异的透明性以及很好的微波吸收性能。
第二，我们合成了“聚苯胺/磁性粒子”以及氨基聚芳醚酮，以耐高温的醛基封端聚甲亚胺齐聚物为偶联剂，通过溶胶-凝胶法制备Fe3O4@聚苯胺/聚甲亚胺/聚芳醚酮三元杂化材料。该材料具有快的交联速度以及均匀的尺寸分布，并展示出较宽的微波吸收频带和较高的反射损耗。
第三，合成具有空心结构的复合微球，并结合以上工作基础，进一步将这些微球与聚芳醚酮基体复合，通过溶胶-凝胶法制备空心微球/聚芳醚酮多孔杂化材料。研究了微球结构吸波剂以及多孔结构杂化材料对吸波性能的影响，制备出了高效、轻质、耐高温以及环境耐受性强的微波吸收材料，并得到了很好的吸波性能。
Due to the fast development of electronic devices such as wireless communications andhigh-frequency circuit devices in the recent decades, electromagnetic interferenceemerges as a novel kind of pollution to the environment, which disturbs the stableworking conditions of electronic appliances and may harm the human body.Microwave-absorbing materials are of great interests as an important and crucialtechnology in solving the expanding electromagnetic interference. Materials such asferrites, conductive polymers, carbon, metals and their oxides have been intensivelyinvestigated, due to their significant contribution to radar stealth and electromagneticinterference shielding. However, with the increasing demands of usage in diverse andcomplex environment, it is urgently to develop high-performance microwave-absorbingmaterials with multifunction, such lightweight, efficient, broadband, temperaturestability, corrosion resistance, radiation resistance, and environmentally friendly, etc.The conventional single kind of material is difficult to meet the increasing requirements.Therefore, exploiting polymer-based hybrid materials with superior performanceabsorbers and substrate polymers has aroused considerable concerns for theirlightweight, high efficient, extensive absorption, cellent stability, flexibility and easyprocessing advantages.
Polyaryetherkotone (PAEK) superior engineering thermoplastic is one of the mostideal matrix polymers to improve the comprehensive properties ofmicrowave-absorbing materials with excellent stability to adapt the harsh environment.Attributed to the distinctive aromatic structure of the polymer, the material performs excellent mechanical properties, thermal stability, ammability, radiation resistance,flame and solvent resistance. Moreover, the flexible ether bonds in the moleculestructure also provide a good processing performance as thermoplastic engineeringplastics. What is more, this kind of non-toxic and electrical insulating polymer isregarded as an electromagnetic windows material. However, there is little research onPAEK as the matrix for microwave-absorbing coatings. Mainly because the insolublePAEK increases the difficulties to disperse the absorbers in matrix. In this paper, wedesign and synthesize a new20%amino-functionalized PEEK copolymer containingtrifluoromethyl units on polymer main chains (AFPEEK) from the molecular point ofview. Furthermore, a series of PAEK-based hybird microwave-absorbing materials areprepared by the complex with absorbers with different electromagnetic properties viasol-gel method. And the structures and properties of these hybrid materials are detailedstudied.
First of all, we synthesize Co0.2Fe2.8O4nanoparticles, which are modified withsilica-protected layers to provide reliable chemical stabilization. The Co0.2Fe2.8O4@SiO2nanoparticles are used as the absorbers to prepare Co0.2Fe2.8O4@SiO2-PEEK hybridmicrowave-absorbing materials for their dielectric and magnetic permeability. Inchapter3, a simple and effective in-situ sol-gel technique is used to improvecompatibility and dispersibility between phases.3-isocyanatopropyltriethoxysilane(IPTS) is introduced as a bridge between the hydrophilic nanoparticles absorbers andthe hydrophobic AFPEEK matrix for its high reactivity with SiO2and amino groups onthe side chain of the polymer. SEM and TEM images demonstrate that the stronginteraction between inorganic-organic phases results in great improvement of dispersionand compatibility at even40wt%nanoparticles contents. The functional integration oforganic polymer and inorganic nanoparticles leads to excellent comprehensiveperformances such as high transparency, solvent resistance, thermal stability andmechanical properties of the hybrid material, as well as the high adhesion with substrate,which benefits its application as coating materials. As the amendment of the shape, sizeand distribution of the fillers in the matrix may strongly change the frequencydependence of permeability. This hybrid membrane exhibits good superparamagnetic behaviors and microwave electromagnetic properties (reflecting loss～-13dB at14.3GHz, d=2mm). It is expected as a promising microwave-absorbing material for thefacile synthesis process and good comprehensive properties.
However, due to low complex permittivity and complex permeability, the loss ofelectromagnetic waves for Co0.2Fe2.8O4@SiO2-PEEK hybrid material is limited, whichis difficult to achieve effective absorption of electromagnetic waves in the range of2-18GHz, even adjust the thickness. The emerging conductive polymer and magneticnanoparticle composite materials are under currently concerned as an ideal absorbers fortheir unique physical and chemical properties. Therefore, in chapter4, we improve andregulate the electromagnetic parameters to achieve better matching by the complexabsorbers of polyaniline conductive polymer composition and magnetic iron oxidenanoparticles(Fe3O4@PANI). Furthermore, through a simple and effectiveamine-aldehyde condensation reaction between the aldehyde-terminated PAM oligomercoupling agent and amino groups (on Fe3O4@PANI nanocomposites and AFPEEK), theternary Fe3O4@PANI/PAM/PEEK hybrid materials are prepared via a sol-gel process.The high stability crosslinked hybrid materials performe excellent thermal stability(Tg>160°C, Td-5%>300°C) and solvent resistance, and exhibit significantmicrowave-absorbing property (RL～-18dB at14GHz, d=2mm) with40wt%nanocomposites contents. The primary mechanism of the microwave absorption isdielectric and magnetic loss, while the magnetic Fe3O4is regarded as a promoter toincrease the complex permeability of PANI. The combination of conductive andmagnetic properties enhances the microwave absorption. Therefore, the intensity andbandwidth of the absorption for hybrid materials increase significantly, the hybridmaterials can achieve effective absorption (>90%) within the range of2-18GHz byregulating the thicknes.
Although Fe3O4@PANI/PAM/PEEK hybrid materials exhibit excellent absorbingproperties, there is still a problem about the high filler contents, which makes thedisadvantages such as lightweight and high efficient. Therefore, in chapter5,considering the balanced of the attenuation characteristics and impedance matching, weoptimize the composition and structure of the absorbing materials. PANI/C/Fe3O4 hollow microspheres with high electromagnetic loss are prepared and introduced as themicrowave absorbers to fabricate a series of porous PAEK-based hybrid materials withvarious absorbers contents, according to the method mentioned in previous chapter. It isexcepted to improve the electromagnetic parameters, as well as adjust the impedancematching, in order to achieve lightweight and high absorption of the materials. Thehybrid material exhibits excellent microwave-absorbing behaviors with30wt%fillercontents, attribute to the unique structure and composition. Firstly, the permeabilitycomponents (matrix and porosity) of the material can make as many waves incident onthe surface and transmission in its interior, which reduces reflection losses. Meanwhile,the absorbing components (absorbers) with high electromagnetic parameters providequick and efficient absroption on the waves. Furthermore, the porous structure results inmultiple reflections in and between the microspheres, which greatly increase theelectromagnetic wave transmission path in the material and the friction with theprobability of absorbers. Therefore, the absorption intensity and the bandwidth of thematerials are improved significantly (RL～-32dB,15GHz, d=2mm). And a strongerabsorption can be achieved (>90%) within the range of4.5-18GHz by adjusting thethickness (2mm,3mm,4mm,5mm). In addition, the material also exhibits highthermal stability (Td-5%>510°C, Tg>180°C). This hybrid technique provides a novelroute for preparation of high performance microwave-absorbing materials.
引文
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