低频段复合吸波材料的制备及电磁性能研究
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摘要
研究吸波材料在国防和民用工业都具有十分重要的意义。目前，吸波材料正朝着“薄、轻、宽、强”的方向发展，但单一组分的吸波材料无法同时满足这些要求，而复合型吸波材料可以克服单一组分的缺点，具有相当的优势，是未来吸波材料的发展方向之一。目前，我国对于低频段（0~6GHz）复合型吸波材料的研究甚少。因此本论文选择了磁损耗型纳米铁氧体、羰基铁和介电损耗型钛酸钡、聚苯胺作为研究对象，利用它们的不同损耗机制、设计开发了在低频段具有优异吸波性能的复合材料Fe_3O_4-SrFe_(12)O_(19)、Ni_(0.5)Zn_(0.5)Fe_2O_4-PANI、BaTiO_3-PANI和Fe(CO)_5/PANI。
在无氮气保护下，采用共沉淀法制备纳米Fe_3O_4，重点探讨制备过程中Fe~(3+)和Fe~(2+)的摩尔比对样品磁性能的影响，在此基础上，采用界面法制备复合材料Fe_3O_4-SrFe_(12)O_(19)，考察不同质量比的Fe_3O_4和SrFe_(12)O_(19)对复合材料的磁性能以及吸波性能的影响。结果表明，当n(Fe~(3+)): n(Fe~(2+))=1:3.5时，制备出具有超顺磁性的粒径在10~15nm之间的球形纳米Fe_3O_4；当ｍ(Fe_3O_4):ｍ(SrFe_(12)O_(19))＝1:0.3时，Fe_3O_4均匀的包覆在SrFe_(12)O_(19)表面，而且复合材料Fe_3O_4-SrFe_(12)O_(19)不仅具有超顺磁性，而且吸波性能也达到最佳，其最大吸收峰值为-17.7dB，优于-5dB频宽为1300MHz，覆盖了2130~3430MHz频域。
首次采用共沉淀法与溶胶-凝胶联合法，制备针状纳米Ni_(0.5)Zn_(0.5)Fe_2O_4，研究制备过程中镍和锌的添加量对纳米Ni_(0.5)Zn_(0.5)Fe_2O_4长径比的影响，通过改变制备过程中镍和锌的添加量达到控制Ni_(0.5)Zn_(0.5)Fe_2O_4长径比的效果；并考察煅烧温度对产物的物相的影响。结果表明，当共沉淀法中nNi:nZn:nFe为0.3:0.3:2时，Ni_(0.5)Zn_(0.5)Fe_2O_4的长径比达到最大为20左右，并且，随着煅烧温度的增加，Ni_(0.5)Zn_(0.5)Fe_2O_4的长径比在减小。再者，采用原位聚合法制备Ni_(0.5)Zn_(0.5)Fe_2O_4-PANI复合材料，研究Ni_(0.5)Zn_(0.5)Fe_2O_4和PANI的键合作用机理以及不同质量比的Ni_(0.5)Zn_(0.5)Fe_2O_4和PANI对复合材料的磁性能和吸波性能的影响。从Ni_(0.5)Zn_(0.5)Fe_2O_4-PANI复合材料的FT-IR光谱分析得出，Ni_(0.5)Zn_(0.5)Fe_2O_4和PANI之间存在一定的键合作用，使复合材料的特征吸收峰发生红移。利用VSM和PNA对产物进行表征和分析得出，随着PANI量的增加，复合材料的矫顽力和饱和磁化强度在减小，而复合材料的吸波性能在0~6000MHz范围内是先增加后减小，当ｍ(Ni_(0.5)Zn_(0.5)Fe_2O_4):ｍ(PANI)＝1:10时，产物具有最佳吸波性能，其最大吸收峰值为-21.5dB，优于-5dB频宽为2900MHz，覆盖了3100~6000MHz频域。
分别采用溶胶-凝胶法和水热法制备纳米BaTiO_3，当水热反应24h制备的纳米BaTiO_3为形貌规则的四方晶型，粒径约60nm；并在此基础上以硅烷偶联剂KH570对纳米BaTiO_3表面进行修饰，采用原位聚合法制备具有核-壳结构的BaTiO_3-PANI复合材料，考察不同质量比的BaTiO_3与PANI和不同吸收厚度对BaTiO_3-PANI复合材料吸波性能的影响，并探讨硅烷偶联剂KH570在制备过程中的反应机理。利用XRD、TEM和FT-IR对复合材料进行表征和分析，得出硅烷偶联剂KH570起到了连接苯胺与钛酸钡的桥梁作用，使PANI成功地包覆纳米BaTiO_3粒子形成具有核-壳结构的BaTiO_3-PANI复合材料，其中BaTiO_3为核，PANI为壳，壳层为40nm，并且包覆后相邻BaTiO_3粒子之间由于高分子的空间位阻而难以相遇，使BaTiO_3分散性更好。利用PNA对复合材料的吸波性能进行分析，得出在0~6000MHz范围内，随着BaTiO_3与PANI质量比和吸收厚度的增加，BaTiO_3-PANI复合材料的反射率RL都是先减小后增大，当BaTiO_3与PANI的质量比为4:1，吸收厚度为3.0mm时，BaTiO_3-PANI复合材料的反射率RL达到最小，其最大吸收峰值为-14.4dB，优于-5dB频宽为1114MHz，覆盖了4798~5912MHz频域。
采用物理共混法制备复合材料Fe(CO)_5/PANI，研究不同质量比的Fe(CO)_5与PANI以及不同吸收厚度对复合材料吸波性能的影响，同时考察复合后对Fe(CO)_5磁性能的影响。结果表明，复合材料Fe(CO)_5/PANI的矫顽力较纯Fe(CO)_5略微增加，而饱和磁化强度却减小。在0~6000MHz范围内，随着PANI的掺入量和吸收厚度的增加，Fe(CO)_5/PANI复合材料的反射率RL都是先减小后增大。当wPANI=6%，吸收厚度为3.0mm时，复合材料的吸波性能最好，其最大吸收峰值为-39.1dB，优于-10dB频宽为1639MHz，覆盖了4361~6000MHz频域。
It would have great significance to study the microwave absorption material, which isapplied widely to national defense and civil industry. At present, the microwave absorbingmaterial is developing towards "thin, light, wide and strong". But single absorbing materialhas been difficult to meet these requirements at the same time. Moreover, the microwaveabsorption composite, which overcomes the disadvantage of the single absorbing material, isone of development directions of microwave absorbing material in the future. The microwaveabsorption composite in low frequency has been researched very little in our country atpresent. Therefore, the magnetic loss nano ferrite, carbonyl iron, dielectric loss barium titanateand polyaniline are chose for research in this work. And due to the advantages of theirdifferent loss mechanism, the composites Fe_3O_4-SrFe_(12)O_(19), Ni_(0.5)Zn_(0.5)Fe_2O_4-PANI,BaTiO_3-PANI and Fe(CO)_5/PANI, which display excellent microwave absorption ability inlow frequency, are designed and developed.
Nanoparticles Fe_3O_4were prepared by coprecipitation method in the absence of nitrogen.The effect of different molar ratio of Fe~(3+)to Fe~(2+)on magnetic performance of sample hasbeen investigated in detail. On this basis, the composite Fe_3O_4-SrFe_(12)O_(19)was prepared byinterface method. The effect of different mass ratio of Fe_3O_4and SrFe_(12)O_(19)on magnetic andmicrowave absorbing properties had been studied. The results show that, when the molar ratioof Fe~(3+)to Fe~(2+)is1:3.5, the spherical Fe_3O_4exhibits superparamagnetic and grain size isbetween10~15nm; when the mass ratio of Fe_3O_4to SrFe_(12)O_(19)is1:0.3, the SrFe_(12)O_(19)wascoated uniformly with Fe_3O_4. Meanwhile, the composite Fe_3O_4-SrFe_(12)O_(19)not only exhibitssuperparamagnetic, but also has the best wave absorbing property, which of the maximumabsorption can reach-17.7dB, the-5dB bandwidth is1300MHz (2130MHz~3430MHz).
Coprecipitation and sol-gel combined method was first used to prepare acicularnano-Ni_(0.5)Zn_(0.5)Fe_2O_4. The influence of Ni and Zn addition on aspect ratio of nano-Ni0.5Zn0.5Fe2O4was studied. The aspect ratio of nano-Ni_(0.5)Zn_(0.5)Fe_2O_4were controlled by the dopedmass of Ni and Zn in the coprecipitation process. The effect of calcination temperature on the phase of samples was studied. The results show that, as the molar ratio of Ni:Zn:Fe equals to0.3:0.3:2, the aspect ratio is at its maximum (about20). And the aspect ratio of samplesreduces with the increasing calcination temperature. Then, the compositeNi_(0.5)Zn_(0.5)Fe_2O_4-PANI was prepared by in situ polymerization. The bonding action betweenNi_(0.5)Zn_(0.5)Fe_2O_4and PANI and different mass ratio of Ni_(0.5)Zn_(0.5)Fe_2O_4and PANI on magneticand microwave absorbing properties have been studied. The FT-IR spectrogram indicatesthat the characteristic absorption peaks of composite show bathochromic shift because ofstronger interaction between Ni_(0.5)Zn_(0.5)Fe_2O_4and PANI. The performance of composite wereanalyzed and characterized by VSM and PNA. The results show that, the coercive force andsaturation magnetization of composite decrease with the increase of amount of PANI. Thewave absorbing properties of composite first increase and then decrease with the increase ofamount of PANI in0~6000MHz. When the mass ratio of Ni_(0.5)Zn_(0.5)Fe_2O_4to PANI is1:10, ithas the best wave absorbing property, which of the maximum absorption can reach-21.5dB,the-5dB bandwidth is2900MHz (3100MHz~6000MHz).
Nanoparticles BaTiO_3were prepared by sol-gel method and hydrothermal methodrespectively. The grain average size of square crystalloid BaTiO_3is about60nm, which waswas synthesized from the hydrothermal reaction for24h. On this basis, the surface of BaTiO_3was modified by silane coupling agent KH570, and the BaTiO_3-PANI composite with core-shell structure was prepared by in-situ polymerization. The composite was characterized andanalysed by the aid of XRD, TEM, FT-IR and PNA. The mechanism of silane coupling agentKH570in preparing process had been discussesed.The effect of the mass ratio of BaTiO_3toPANI and absorption thickness on microwave absorbing properties of samples had beenresearched. The results show that KH570playes a bridge role for aniline and BaTiO_3, andmakes the BaTiO_3coated with PANI, so BaTiO_3-PANI with core-shell structure is resulted, inwhich the core and shell is BaTiO_3and PANI respectively, shell layer is40nm. Besides, theBaTiO_3after being coated has better dispersion due to the steric hindrance. Also the PNAresults show that the reflectivity RLof composite presented the trend of first decrease thenincrease with the increase of the PANI content and absorption thickness during the range of0~6000MHz. When the mass ratio of BaTiO_3to PANI is4:1and absorption thickness is3mm,BaTiO_3-PANI exhibits the best wave absorbing property with the maximum absorption of-14.4dB and the-5dB bandwidth of1114MHz (4798MHz~5912MHz).
The Fe(CO)_5/PANI composite was prepared by physical blending. The effect of the mass ratio of Fe(CO)_5to PANI and absorption thickness on microwave absorbing properties ofcomposite had been studied. And the magnetic property of Fe(CO)_5/PANI composite hadbeen disscussed. The results show that the coercive force of Fe(CO)_5/PANI composite isslightly larger than that of pure Fe(CO)_5, but the its saturation magnetization decreasecompared with pure Fe(CO)_5. The reflectivity RLof composite decreases with the increasingPANI content and absorption thickness in the range of0~6000MHz, and then increases. Whenthe PANI content is6%and absorption thickness is3mm, the wave absorbing property ofcomposite is the best, and the maximum absorption can reach-39.1dB, and the-10dBbandwidth is1639MHz (4361MHz~6000MHz).
在无氮气保护下，采用共沉淀法制备纳米Fe_3O_4，重点探讨制备过程中Fe~(3+)和Fe~(2+)的摩尔比对样品磁性能的影响，在此基础上，采用界面法制备复合材料Fe_3O_4-SrFe_(12)O_(19)，考察不同质量比的Fe_3O_4和SrFe_(12)O_(19)对复合材料的磁性能以及吸波性能的影响。结果表明，当n(Fe~(3+)): n(Fe~(2+))=1:3.5时，制备出具有超顺磁性的粒径在10~15nm之间的球形纳米Fe_3O_4；当ｍ(Fe_3O_4):ｍ(SrFe_(12)O_(19))＝1:0.3时，Fe_3O_4均匀的包覆在SrFe_(12)O_(19)表面，而且复合材料Fe_3O_4-SrFe_(12)O_(19)不仅具有超顺磁性，而且吸波性能也达到最佳，其最大吸收峰值为-17.7dB，优于-5dB频宽为1300MHz，覆盖了2130~3430MHz频域。
首次采用共沉淀法与溶胶-凝胶联合法，制备针状纳米Ni_(0.5)Zn_(0.5)Fe_2O_4，研究制备过程中镍和锌的添加量对纳米Ni_(0.5)Zn_(0.5)Fe_2O_4长径比的影响，通过改变制备过程中镍和锌的添加量达到控制Ni_(0.5)Zn_(0.5)Fe_2O_4长径比的效果；并考察煅烧温度对产物的物相的影响。结果表明，当共沉淀法中nNi:nZn:nFe为0.3:0.3:2时，Ni_(0.5)Zn_(0.5)Fe_2O_4的长径比达到最大为20左右，并且，随着煅烧温度的增加，Ni_(0.5)Zn_(0.5)Fe_2O_4的长径比在减小。再者，采用原位聚合法制备Ni_(0.5)Zn_(0.5)Fe_2O_4-PANI复合材料，研究Ni_(0.5)Zn_(0.5)Fe_2O_4和PANI的键合作用机理以及不同质量比的Ni_(0.5)Zn_(0.5)Fe_2O_4和PANI对复合材料的磁性能和吸波性能的影响。从Ni_(0.5)Zn_(0.5)Fe_2O_4-PANI复合材料的FT-IR光谱分析得出，Ni_(0.5)Zn_(0.5)Fe_2O_4和PANI之间存在一定的键合作用，使复合材料的特征吸收峰发生红移。利用VSM和PNA对产物进行表征和分析得出，随着PANI量的增加，复合材料的矫顽力和饱和磁化强度在减小，而复合材料的吸波性能在0~6000MHz范围内是先增加后减小，当ｍ(Ni_(0.5)Zn_(0.5)Fe_2O_4):ｍ(PANI)＝1:10时，产物具有最佳吸波性能，其最大吸收峰值为-21.5dB，优于-5dB频宽为2900MHz，覆盖了3100~6000MHz频域。
分别采用溶胶-凝胶法和水热法制备纳米BaTiO_3，当水热反应24h制备的纳米BaTiO_3为形貌规则的四方晶型，粒径约60nm；并在此基础上以硅烷偶联剂KH570对纳米BaTiO_3表面进行修饰，采用原位聚合法制备具有核-壳结构的BaTiO_3-PANI复合材料，考察不同质量比的BaTiO_3与PANI和不同吸收厚度对BaTiO_3-PANI复合材料吸波性能的影响，并探讨硅烷偶联剂KH570在制备过程中的反应机理。利用XRD、TEM和FT-IR对复合材料进行表征和分析，得出硅烷偶联剂KH570起到了连接苯胺与钛酸钡的桥梁作用，使PANI成功地包覆纳米BaTiO_3粒子形成具有核-壳结构的BaTiO_3-PANI复合材料，其中BaTiO_3为核，PANI为壳，壳层为40nm，并且包覆后相邻BaTiO_3粒子之间由于高分子的空间位阻而难以相遇，使BaTiO_3分散性更好。利用PNA对复合材料的吸波性能进行分析，得出在0~6000MHz范围内，随着BaTiO_3与PANI质量比和吸收厚度的增加，BaTiO_3-PANI复合材料的反射率RL都是先减小后增大，当BaTiO_3与PANI的质量比为4:1，吸收厚度为3.0mm时，BaTiO_3-PANI复合材料的反射率RL达到最小，其最大吸收峰值为-14.4dB，优于-5dB频宽为1114MHz，覆盖了4798~5912MHz频域。
采用物理共混法制备复合材料Fe(CO)_5/PANI，研究不同质量比的Fe(CO)_5与PANI以及不同吸收厚度对复合材料吸波性能的影响，同时考察复合后对Fe(CO)_5磁性能的影响。结果表明，复合材料Fe(CO)_5/PANI的矫顽力较纯Fe(CO)_5略微增加，而饱和磁化强度却减小。在0~6000MHz范围内，随着PANI的掺入量和吸收厚度的增加，Fe(CO)_5/PANI复合材料的反射率RL都是先减小后增大。当wPANI=6%，吸收厚度为3.0mm时，复合材料的吸波性能最好，其最大吸收峰值为-39.1dB，优于-10dB频宽为1639MHz，覆盖了4361~6000MHz频域。
It would have great significance to study the microwave absorption material, which isapplied widely to national defense and civil industry. At present, the microwave absorbingmaterial is developing towards "thin, light, wide and strong". But single absorbing materialhas been difficult to meet these requirements at the same time. Moreover, the microwaveabsorption composite, which overcomes the disadvantage of the single absorbing material, isone of development directions of microwave absorbing material in the future. The microwaveabsorption composite in low frequency has been researched very little in our country atpresent. Therefore, the magnetic loss nano ferrite, carbonyl iron, dielectric loss barium titanateand polyaniline are chose for research in this work. And due to the advantages of theirdifferent loss mechanism, the composites Fe_3O_4-SrFe_(12)O_(19), Ni_(0.5)Zn_(0.5)Fe_2O_4-PANI,BaTiO_3-PANI and Fe(CO)_5/PANI, which display excellent microwave absorption ability inlow frequency, are designed and developed.
Nanoparticles Fe_3O_4were prepared by coprecipitation method in the absence of nitrogen.The effect of different molar ratio of Fe~(3+)to Fe~(2+)on magnetic performance of sample hasbeen investigated in detail. On this basis, the composite Fe_3O_4-SrFe_(12)O_(19)was prepared byinterface method. The effect of different mass ratio of Fe_3O_4and SrFe_(12)O_(19)on magnetic andmicrowave absorbing properties had been studied. The results show that, when the molar ratioof Fe~(3+)to Fe~(2+)is1:3.5, the spherical Fe_3O_4exhibits superparamagnetic and grain size isbetween10~15nm; when the mass ratio of Fe_3O_4to SrFe_(12)O_(19)is1:0.3, the SrFe_(12)O_(19)wascoated uniformly with Fe_3O_4. Meanwhile, the composite Fe_3O_4-SrFe_(12)O_(19)not only exhibitssuperparamagnetic, but also has the best wave absorbing property, which of the maximumabsorption can reach-17.7dB, the-5dB bandwidth is1300MHz (2130MHz~3430MHz).
Coprecipitation and sol-gel combined method was first used to prepare acicularnano-Ni_(0.5)Zn_(0.5)Fe_2O_4. The influence of Ni and Zn addition on aspect ratio of nano-Ni0.5Zn0.5Fe2O4was studied. The aspect ratio of nano-Ni_(0.5)Zn_(0.5)Fe_2O_4were controlled by the dopedmass of Ni and Zn in the coprecipitation process. The effect of calcination temperature on the phase of samples was studied. The results show that, as the molar ratio of Ni:Zn:Fe equals to0.3:0.3:2, the aspect ratio is at its maximum (about20). And the aspect ratio of samplesreduces with the increasing calcination temperature. Then, the compositeNi_(0.5)Zn_(0.5)Fe_2O_4-PANI was prepared by in situ polymerization. The bonding action betweenNi_(0.5)Zn_(0.5)Fe_2O_4and PANI and different mass ratio of Ni_(0.5)Zn_(0.5)Fe_2O_4and PANI on magneticand microwave absorbing properties have been studied. The FT-IR spectrogram indicatesthat the characteristic absorption peaks of composite show bathochromic shift because ofstronger interaction between Ni_(0.5)Zn_(0.5)Fe_2O_4and PANI. The performance of composite wereanalyzed and characterized by VSM and PNA. The results show that, the coercive force andsaturation magnetization of composite decrease with the increase of amount of PANI. Thewave absorbing properties of composite first increase and then decrease with the increase ofamount of PANI in0~6000MHz. When the mass ratio of Ni_(0.5)Zn_(0.5)Fe_2O_4to PANI is1:10, ithas the best wave absorbing property, which of the maximum absorption can reach-21.5dB,the-5dB bandwidth is2900MHz (3100MHz~6000MHz).
Nanoparticles BaTiO_3were prepared by sol-gel method and hydrothermal methodrespectively. The grain average size of square crystalloid BaTiO_3is about60nm, which waswas synthesized from the hydrothermal reaction for24h. On this basis, the surface of BaTiO_3was modified by silane coupling agent KH570, and the BaTiO_3-PANI composite with core-shell structure was prepared by in-situ polymerization. The composite was characterized andanalysed by the aid of XRD, TEM, FT-IR and PNA. The mechanism of silane coupling agentKH570in preparing process had been discussesed.The effect of the mass ratio of BaTiO_3toPANI and absorption thickness on microwave absorbing properties of samples had beenresearched. The results show that KH570playes a bridge role for aniline and BaTiO_3, andmakes the BaTiO_3coated with PANI, so BaTiO_3-PANI with core-shell structure is resulted, inwhich the core and shell is BaTiO_3and PANI respectively, shell layer is40nm. Besides, theBaTiO_3after being coated has better dispersion due to the steric hindrance. Also the PNAresults show that the reflectivity RLof composite presented the trend of first decrease thenincrease with the increase of the PANI content and absorption thickness during the range of0~6000MHz. When the mass ratio of BaTiO_3to PANI is4:1and absorption thickness is3mm,BaTiO_3-PANI exhibits the best wave absorbing property with the maximum absorption of-14.4dB and the-5dB bandwidth of1114MHz (4798MHz~5912MHz).
The Fe(CO)_5/PANI composite was prepared by physical blending. The effect of the mass ratio of Fe(CO)_5to PANI and absorption thickness on microwave absorbing properties ofcomposite had been studied. And the magnetic property of Fe(CO)_5/PANI composite hadbeen disscussed. The results show that the coercive force of Fe(CO)_5/PANI composite isslightly larger than that of pure Fe(CO)_5, but the its saturation magnetization decreasecompared with pure Fe(CO)_5. The reflectivity RLof composite decreases with the increasingPANI content and absorption thickness in the range of0~6000MHz, and then increases. Whenthe PANI content is6%and absorption thickness is3mm, the wave absorbing property ofcomposite is the best, and the maximum absorption can reach-39.1dB, and the-10dBbandwidth is1639MHz (4361MHz~6000MHz).
引文
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