稀土取代W型铁氧体及其聚苯胺复合材料的制备及性能研究
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摘要
微波吸收材料是为解决电磁波干扰和辐射问题应运而生的一类特殊功能材料。它在航空航天、军事战略装备、卫星通讯、微波暗室以及各种科技测试仪器、电子设备、家用电器等方面都有着广泛的应用。但随着科技的发展，对其功能提出了更多更高的要求。磁铅石型铁氧体是一种具有较高的饱和磁化强度的磁性材料，因其在高频时还具有较高的磁损耗特性，也常被用作高频微波吸收材料，但由于铁氧体的质量大，吸收频带窄等缺点限制了其在实际当中的应用。因此有必要对铁氧体的性能进行优化和调整，以制备适用范围更广的微波吸收材料。本文首先利用不同的稀土离子取代了磁铅石W型铁氧体中的Ba2+离子，制备出各种稀土离子取代的W型铁氧体。然后使之与导电聚苯胺复合，制备出聚苯胺-W型铁氧体复合材料。以期利用稀土离子优良的磁性和较强的自旋-轨道耦合作用和导电聚苯胺优良的介电特性，来改善W型铁氧体的静磁性能、电磁性能和微波吸收性能。根据微观结构和电磁性能之间的内在联系探讨了稀土离子影响的一般规律。利用多种表征手段，如X射线衍射、振动样品磁强计、X射线光电子能谱和微波矢量网络分析仪等对所制备产物的性能进行了表征。主要得出以下结论：
1．采用高温固相法制备了轻稀土离子取代Ba2+的W型铁氧体Ba0.9RE0.1Co2Fe16O27(RE=La3+，Nd3+，Sm3+，相应产物分别标记为LaBF，NdBF，SmBF)。产物的XRD和微观结构参数的研究结果显示，稀土离子取代使W型铁氧体的晶胞参数减小，并且取代后产物的晶胞参数a、c和晶胞体积Vcell随稀土离子半径的减小而有规律的减小，空隙率P随稀土离子半径的减小而增大。对产物静磁性能的研究结果表明，三种稀土离子取代都改善了产物的静磁性能，并随着稀土离子半径的增大呈规律性变化，其饱和磁化强度Ms增大的顺序为：SmBF 2．采用溶胶-凝胶自蔓延燃烧法制备不同La3+掺量的W型铁氧体Ba1-xLaxCo2Fe16O27(x=0.00，0.05，0.10，0.15，0.20)。此法制备纯相La3+取代W型铁氧体的最佳热处理条件是1200℃/1h，有效的降低了烧结温度，缩短了烧结时间，减小了能耗。对产物的微观结构参数和静磁性能研究发现，随着La3+掺量的增加，样品的晶胞参数和晶胞体积减小，空隙率增加；由于La3+离子对Fe离子亚晶位超精细场的作用，使饱和磁化强度Ms先增加后减小，矫顽力Hc先减小后增加。X射线光电子能谱测试La3+取代Ba2+前后Fe和Co离子的存在价态发现，取代前Fe和Co分别主要以Fe(III)和Co(II)价态存在，取代后，Fe则以Fe(III)+Fe(II)混合价态存在，而Co的存在价态没有改变。利用X射线光电子能谱实验数据验证了La3+取代能使部分Fe3+转变成Fe2+。
3．合成了不同聚苯胺含量的聚苯胺-La掺杂W型铁氧体复合材料PANI/Ba0.85La0.15Co2Fe16O27。振动样品磁强计的测试结果发现，复合产物的饱和磁化强度随着聚苯胺含量的增加而逐渐减小；复合产物的复介电常数随着聚苯胺含量在增加而有规律的增加，当PANI:Ba0.85La0.15Co2Fe16O27的质量比为7:5时，复合产物在~9.3GHz处的反射损耗RL达到最大-14.95dB，比单相铁氧体Ba0.85La0.15Co2Fe16O27的反射损耗(RL=-7.1dB)增高近2.1倍。对其性能主要影响机制的研究发现，聚苯胺加强了复合材料的取向极化和界面极化作用，使复合材料的介电损耗部分得到加强，从而使复合材料反射损耗RL提高，微波吸收性能加强。
4．采用溶胶-凝胶自蔓延燃烧法制备不同重稀土离子取代Ba2+的W型铁氧体Ba0.85RE0.15Co2Fe16O27(RE=Gd3+，Tb3+，Ho3+)。根据Gd3+, Tb3+和Ho3+之间的离子半径和离子磁矩的差异，对产物的微观结构参数的和静磁性能的研究发现，产物的晶胞参数a、c和晶胞体积Vcell随稀土离子半径的减小而逐渐增大，饱和磁化强度随稀土离子半径的减小而逐渐增大。将三种稀土离子取代产物分别与等量的聚苯胺复合，制备了PANI/Ba0.85RE0.15Co2Fe16O27复合材料。用微波矢量网络分析仪测试复合产物的复介电常数和复磁导率，结果发现，聚苯胺复合产物的取向极化、界面极化作用和阻抗匹配都有所加强，从而使复介电常数提高，介电损耗加强，改善了复合材料的微波吸收性能。比较三种稀土离子取代铁氧体的聚苯胺复合产物，稀土离子Ho3+掺杂的复合产物PANI/Ba0.85Ho0.15Co2Fe16O27在~9GHz处的反射损耗RL为-15.1dB，反射损耗RL最高，微波吸收性能最佳。
W-type hexaferrite is a kind of magnetic material with high saturationmagnetization, which is usually used as high-frequency microwave absorbingmaterial due to its large reflection loss at high frequency. However, the application ofthe hexaferrite microwave absorber was restricted by some disadvantages such asheavy weight, low absorption and narrow absorb bandwidth. In order to enlarge theapplication field of the W-type hexaferrite microwave absorber, it is necessary toadjust and optimize the performance of the hexaferrite. This paper prepared a varietyof rare earth ions substituted W-type hexaferrites, then, take the conductivepolyaniline as shell and the substituted hexaferrite as core, synthesized a series ofpolyaniline-W-type hexaferrite composites. In hope that the strong spin-orbitcoupling effect of the rare earth ions and the excellent dielectric properties of theconductive polyaniline can improve the static magnetic and electromagneticproperties and microwave absorption performance. Based on the internal interactionbetween the microstructure and electromagnetic properties, the general influence ofthe rare earth ions on W-type hexaferrite was discussed in detail. Thecharacterization and performance of the prepared samples were investigated byX-ray diffraction spectrometer, vibrating sample magnetometer, X-ray photoelectronspectroscopy and microwave vector network analyzer etc. The main conclusions areas following:
1．The light rare earth ions substituted W-type hexaferriteBa0.9RE0.1Co2Fe16O27(RE=La3+，Nd3+，Sm3+) were synthesized via solid statereaction method. The research results of XRD patterns and microstructureparameters show that the replacement of Ba2+by light rare earth ions reduces the crystal cell parameters. And the crystal cell parameter a, c and crystal cell volumeVcellof the substituted hexaferrite decrease regularly with the decrease of ionicradius of rare earth, the porosity of the substituted hexaferrite increases with thedecrease of ionic radius of rare earth. The static magnetic properties investigationsshow that the light rare earth ions substitution can improve the magnetic propertiesof W-type hexaferrite, and the saturation magnetization Msshows a change regularlywith the increase of rare earth ionic radius: SmBF 2．The W-type hexaferrite Ba1-xLaxCo2Fe16O27(x=0.00,0.05,0.01,0.05,0.20)was prepared by sol-gel self-propagating combustion method with different La3+content. The optimum heat treatment condition of pure W-type hexaferrite phase was1200℃/1hby this method, which reduce the sintering temperature and shorten thesintering time effectively. The crystal cell parameters and crystal cell volumedecrease and the porosity increase with the increasing of La3+content. The saturationmagnetization increases at first and then decreases, while the coercivity decreases atfirst and then increases. The X-ray photoelectron spectroscopy was used to measurethe valence states of Fe and co exists in La-substituted and un-substituted hexaferrite.The results show that the valence states of Fe and Co in un-substituted hexaferrite were Fe (III) and Co (II) respectively, while its change to Fe (III)+Fe (II) and Co (II)in La-substituted hexaferrite respectively. It was proved via statistic data that thereplacement of Ba2+by La3+can change a part of Fe3+to Fe2+.
3．The polyaniline/hexaferrite composite PANI/Ba0.85La0.15Co2Fe16O27wassynthesized with different polyaniline content. The measurement result of vibratingsample magnetometer show that the saturation magnetization of the compositesdecreases with the increasing of polyaniline content. The complex permittivity of thecomposites increase regularly with the increasing of polyaniline content. Themaximum reflection loss of the composite was-14.95dB at the frequency about9.7GHz, when the PANI:Ba0.85La0.15Co2Fe16O27mass ratio of is7:5, which was morethan double that of pure hexaferrite Ba0.85La0.15Co2Fe16O27(-7.1dB). The discussionon the mechanism shows that the orientation polarization and interface polarizationof the composite were enhanced by the coating of polyaniline effectively, and thedielectric loss part of the composite was improved, consequently, the microwaveabsorbing performance of the composite was enhanced.
4．The W-type hexaferrite Ba0.85RE0.15Co2Fe16O27(RE=Gd3+, Tb3+, Ho3+)with different heavy rare earth ions substituted were synthesized via sol-gelself-propagating combustion method. The microstructure parameters and staticmagnetic properties of the synthesized sample was investigated based on thedifference of ionic radius and ionic magnetic moment of rare earth ions. The resultsshows that the crystal cell parameter a, c and crystal cell volume Vcellincrease withthe decreasing of ionic radius of rare earth, and the saturation magnetizationincreases with the decreasing of ionic radius of rare earth. Furthermore, the Gd3+,Tb3+and Ho3+substituted hexaferrites Ba0.85RE0.15Co2Fe16O27were combined withconductive polyaniline under the equal mass ratio to prepared thePANI/Ba0.85RE0.15Co2Fe16O27composite material. The complex permittivity andpermeability of the composite were investigated by microwave vector networkanalyzer. And the results showed that the orientation polarization, interfacepolarization and the impedance matching of the composite were improved by thecoating of polyaniline, which was better for strengthening the dielectric loss part of the composite. Consequently, the microwave absorbing performance of thecomposite was enhanced. The maximum reflection loss ofPANI/Ba0.85Ho0.15Co2Fe16O27composite at about9GHz was-15.1dB, which wasexcellent in the three composite materials.
1．采用高温固相法制备了轻稀土离子取代Ba2+的W型铁氧体Ba0.9RE0.1Co2Fe16O27(RE=La3+，Nd3+，Sm3+，相应产物分别标记为LaBF，NdBF，SmBF)。产物的XRD和微观结构参数的研究结果显示，稀土离子取代使W型铁氧体的晶胞参数减小，并且取代后产物的晶胞参数a、c和晶胞体积Vcell随稀土离子半径的减小而有规律的减小，空隙率P随稀土离子半径的减小而增大。对产物静磁性能的研究结果表明，三种稀土离子取代都改善了产物的静磁性能，并随着稀土离子半径的增大呈规律性变化，其饱和磁化强度Ms增大的顺序为：SmBF
3．合成了不同聚苯胺含量的聚苯胺-La掺杂W型铁氧体复合材料PANI/Ba0.85La0.15Co2Fe16O27。振动样品磁强计的测试结果发现，复合产物的饱和磁化强度随着聚苯胺含量的增加而逐渐减小；复合产物的复介电常数随着聚苯胺含量在增加而有规律的增加，当PANI:Ba0.85La0.15Co2Fe16O27的质量比为7:5时，复合产物在~9.3GHz处的反射损耗RL达到最大-14.95dB，比单相铁氧体Ba0.85La0.15Co2Fe16O27的反射损耗(RL=-7.1dB)增高近2.1倍。对其性能主要影响机制的研究发现，聚苯胺加强了复合材料的取向极化和界面极化作用，使复合材料的介电损耗部分得到加强，从而使复合材料反射损耗RL提高，微波吸收性能加强。
4．采用溶胶-凝胶自蔓延燃烧法制备不同重稀土离子取代Ba2+的W型铁氧体Ba0.85RE0.15Co2Fe16O27(RE=Gd3+，Tb3+，Ho3+)。根据Gd3+, Tb3+和Ho3+之间的离子半径和离子磁矩的差异，对产物的微观结构参数的和静磁性能的研究发现，产物的晶胞参数a、c和晶胞体积Vcell随稀土离子半径的减小而逐渐增大，饱和磁化强度随稀土离子半径的减小而逐渐增大。将三种稀土离子取代产物分别与等量的聚苯胺复合，制备了PANI/Ba0.85RE0.15Co2Fe16O27复合材料。用微波矢量网络分析仪测试复合产物的复介电常数和复磁导率，结果发现，聚苯胺复合产物的取向极化、界面极化作用和阻抗匹配都有所加强，从而使复介电常数提高，介电损耗加强，改善了复合材料的微波吸收性能。比较三种稀土离子取代铁氧体的聚苯胺复合产物，稀土离子Ho3+掺杂的复合产物PANI/Ba0.85Ho0.15Co2Fe16O27在~9GHz处的反射损耗RL为-15.1dB，反射损耗RL最高，微波吸收性能最佳。
W-type hexaferrite is a kind of magnetic material with high saturationmagnetization, which is usually used as high-frequency microwave absorbingmaterial due to its large reflection loss at high frequency. However, the application ofthe hexaferrite microwave absorber was restricted by some disadvantages such asheavy weight, low absorption and narrow absorb bandwidth. In order to enlarge theapplication field of the W-type hexaferrite microwave absorber, it is necessary toadjust and optimize the performance of the hexaferrite. This paper prepared a varietyof rare earth ions substituted W-type hexaferrites, then, take the conductivepolyaniline as shell and the substituted hexaferrite as core, synthesized a series ofpolyaniline-W-type hexaferrite composites. In hope that the strong spin-orbitcoupling effect of the rare earth ions and the excellent dielectric properties of theconductive polyaniline can improve the static magnetic and electromagneticproperties and microwave absorption performance. Based on the internal interactionbetween the microstructure and electromagnetic properties, the general influence ofthe rare earth ions on W-type hexaferrite was discussed in detail. Thecharacterization and performance of the prepared samples were investigated byX-ray diffraction spectrometer, vibrating sample magnetometer, X-ray photoelectronspectroscopy and microwave vector network analyzer etc. The main conclusions areas following:
1．The light rare earth ions substituted W-type hexaferriteBa0.9RE0.1Co2Fe16O27(RE=La3+，Nd3+，Sm3+) were synthesized via solid statereaction method. The research results of XRD patterns and microstructureparameters show that the replacement of Ba2+by light rare earth ions reduces the crystal cell parameters. And the crystal cell parameter a, c and crystal cell volumeVcellof the substituted hexaferrite decrease regularly with the decrease of ionicradius of rare earth, the porosity of the substituted hexaferrite increases with thedecrease of ionic radius of rare earth. The static magnetic properties investigationsshow that the light rare earth ions substitution can improve the magnetic propertiesof W-type hexaferrite, and the saturation magnetization Msshows a change regularlywith the increase of rare earth ionic radius: SmBF
3．The polyaniline/hexaferrite composite PANI/Ba0.85La0.15Co2Fe16O27wassynthesized with different polyaniline content. The measurement result of vibratingsample magnetometer show that the saturation magnetization of the compositesdecreases with the increasing of polyaniline content. The complex permittivity of thecomposites increase regularly with the increasing of polyaniline content. Themaximum reflection loss of the composite was-14.95dB at the frequency about9.7GHz, when the PANI:Ba0.85La0.15Co2Fe16O27mass ratio of is7:5, which was morethan double that of pure hexaferrite Ba0.85La0.15Co2Fe16O27(-7.1dB). The discussionon the mechanism shows that the orientation polarization and interface polarizationof the composite were enhanced by the coating of polyaniline effectively, and thedielectric loss part of the composite was improved, consequently, the microwaveabsorbing performance of the composite was enhanced.
4．The W-type hexaferrite Ba0.85RE0.15Co2Fe16O27(RE=Gd3+, Tb3+, Ho3+)with different heavy rare earth ions substituted were synthesized via sol-gelself-propagating combustion method. The microstructure parameters and staticmagnetic properties of the synthesized sample was investigated based on thedifference of ionic radius and ionic magnetic moment of rare earth ions. The resultsshows that the crystal cell parameter a, c and crystal cell volume Vcellincrease withthe decreasing of ionic radius of rare earth, and the saturation magnetizationincreases with the decreasing of ionic radius of rare earth. Furthermore, the Gd3+,Tb3+and Ho3+substituted hexaferrites Ba0.85RE0.15Co2Fe16O27were combined withconductive polyaniline under the equal mass ratio to prepared thePANI/Ba0.85RE0.15Co2Fe16O27composite material. The complex permittivity andpermeability of the composite were investigated by microwave vector networkanalyzer. And the results showed that the orientation polarization, interfacepolarization and the impedance matching of the composite were improved by thecoating of polyaniline, which was better for strengthening the dielectric loss part of the composite. Consequently, the microwave absorbing performance of thecomposite was enhanced. The maximum reflection loss ofPANI/Ba0.85Ho0.15Co2Fe16O27composite at about9GHz was-15.1dB, which wasexcellent in the three composite materials.
引文
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