稀土替代锶铁氧体及其复合材料的制备和吸波性能研究
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摘要
现代微电子技术的飞速发展给人们的生活带来便利,但是电磁波辐射对环境的影响日益增大,因此,具有吸收电磁波功能的材料成为研究和应用的热点。理想的吸波涂层材料应该具有强吸收、宽频段、厚度薄、质量轻的特点。但迄今为止,还没有发现任何一种材料能够完全满足这些要求。因此,对现有材料进行适当改性和设计就成为了研究的重点。六角晶锶铁氧体由于具有高的各向异性场、高饱和磁化强度、高磁损耗、强耐酸碱性以及性能稳定等优点,被广泛应用于微波吸收材料中,但是单一的锶铁氧体仍具有吸收不够强、吸收频段比较窄的缺点。本论文旨在研制一种制备工艺简单、吸收频带更宽和吸收能力更强的新型锶铁氧体基复合材料,并研究相关的制备科学问题和吸波机理,为吸波材料的生产和应用提供技术和理论支撑。
论文首先用稀土离子替代的方法,显著改善了锶铁氧体的吸波性能,特别是提高了吸收强度。本文采用了溶胶-凝胶技术和自蔓延燃烧法相结合的方法制备镧、铈、钕三种离子替代的锶铁氧体。研究结果表明,稀土离子在锶铁氧体中的替代量取决于其离子化合价与离子半径。正四价的铈离子几乎不能进入锶铁氧体晶格,而轻稀土元素镧和钕的正三价离子替代量分别为0.15和0.1。与氧离子半径差别较小的镧离子替代量较高。离子替代使锶铁氧体的晶粒尺寸变小,颗粒团聚程度减弱;在饱和磁化强度不太降低的情况下,使矫顽力增加;吸波性能大大提高,特别是对镧离子,当替代量为0.15时,匹配厚度从2.6mm减小到2.3mm,反射损耗从-24dB降低到-37.7dB, 10dB带宽从2.7GHz(6.4-9.1GHz)拓展到4GHz(6-10GHz)。穆斯堡尔谱研究结果表明:虽然稀土离子替代的是锶铁氧体中锶位,但是对铁离子的超精细场,周围的电子云密度、以及电子轨道都有影响,当三价的镧离子替代锶铁氧体中的二价锶离子以后,为了化合价的平衡,在4 f 1和2a位,有少部分的铁离子从三价变为二价。替代锶铁氧体吸波性能提高的原因是:晶粒尺寸减小增加了界面损耗;矫顽力增大使磁滞损耗增加;离子替代引起的铁离子化合价的改变使介电损耗增加。
为了进一步拓展锶铁氧体的吸收带宽,采用了两步包覆法和一步复合法制备锌铁氧体与锶铁氧体复合粉末。结果表明,一步复合法可以有效扩展其带宽,两步法制备的复合粉末有少量的α? Fe2 O 3生成。当锌铁氧体的质量含量为15%时,两种复合方法都可以提高吸波性能,但当质量比增加到30%,吸波性能下降,这是因为锌铁氧体在所研究的频率范围内本身不具有吸波性能,过多的锌铁氧体使整体复合材料的性能下降。一步法制备的复合材料性能更加优越,在2.3mm的匹配厚度下,最低反射损耗达到-35dB,10dB带宽超过4GHz,这是由于此种方法制备的复合材料颗粒比较小,成分更加均匀,相互作用界面更多,并且没有α? Fe2 O 3存在。与纯锶铁氧体以及替代锶铁氧体不同的是,复合粉末除了存在一个随厚度变化的反射损耗峰;另外,在16GHz左右,还存在一位置不随样品厚度发生改变的反射损耗峰,这是由于两种铁氧体相互作用引起的。
最后,为了研制出一种吸波性能优越并且可以在实际中应用的吸波材料,在前面研究的基础上,选择性能最好的替代铁氧体以及比较好的复合方式,制备镧替代锶铁氧体与锌铁氧体的复合粉末。并且用以上制备的复合粉末为吸波剂,选择实际应用比较多的环氧树脂作为基体,制备吸波剂与基体质量比分别为1、1.25、1.5的复合材料。研究结果表明,当吸波介质与基体质量比为1.25时,所得复合材料的吸波性能最好,相对纯锶铁氧体有很大提高,匹配厚度从2.6mm减小到2.2mm,最小反射频率从-24dB降低到-41dB,下降了70%,10dB带宽从2.7GHz拓宽到5.7GHz,拓宽了一倍以上,展示出该材料的应用前景。特别是当样品厚度为1.5mm时,也得到了比较好的吸波性能,这在实际应用中有非常重要意义,满足了吸波涂层材料要求的吸收强,频带宽,厚度薄,质量轻的特点。
通过对镧替代锶铁氧体与锌铁氧体复合粉末的晶体结构、磁性能和穆斯堡尔谱进行研究,结果表明,镧替代锶铁氧体与锌铁氧体复合材料兼具了替代和复合两种优势。由于两种铁氧体的复合,使正尖晶石型的锌铁氧体向复合尖晶石类型转变,并且锌离子在镧离子存在的情况下,进入到锶铁氧体晶格中,替换了4 f 1位置的铁离子,从而使镧替代锶铁氧体的晶格常数变大,锌铁氧体晶格常数变小。两种铁氧体的这种相互作用使饱和磁化强度增加,从而增加了磁损耗。这些理论推断对今后复合铁氧体新型吸波材料的开发以及吸波机理的研究具有一定的参考意义。
The electromagnetic absorption material has become a hot research topic and development focus as a consequence of the booming research and widely application of GHz electromagnetic waves in modern society. As a solution of electromagnetic pollution and some special usage in military and aerospace field, electromagnetic absorption material is required to have strong absorption, wide bandwidth and proper mechanical properties. The hexagonal strontium ferrite is a good candidate material due to its high magnetic anisotropy, high saturation magnetization and excellent chemical stability. However, disadvantages like relatively weaker absorption performance and narrower frequency bandwidth constrains its application. The purpose of this work is to fabricate a Sr ferrite material with better absorption performance and wider bandwidth, as well as studying the absorption mechanism and material preparation process.
Firstly, absorption performance was remarkably improved by introducing rare-earth ion substitution into Sr ferrite. La/Ce/Nd ion substituted strontium ferrites were prepared by sol-gel technique and self-propagating combustion method. XRD analysis shows that the maximum substitute amount of La/Ce/Nd ion is 0.15, 0.1 and 0 under the process condition of 1000℃, 1.5h. Ce can’t enter the lattice due to its stable +4 valence. The substitute amount of rare-earth ions depends on their valence and ion radius. Compare to pure strontium ferrite, the lattice dimension and particle size of the ion substituted ferrite are smaller, that can remarkably improve the electromagnetic absorption performance by increasing the coercivity without causing any significant deterioration in specific saturation magnetization. Especially for La-substituted ferrite, when the substitute amount is 0.15, compared with pure strontium ferrite, the matching thickness can be reduced from 2.6mm to 2.3mm, the minimum reflection loss decreases from -24dB to -37.7dB. and 10db bandwidth can be expanded from 2.7GHz (6.4-9.1GHz) to 4GHz (6-10GHz). The M?ssbauer spectroscopy showed that when the La3+ substituted the Sr2+ in the ferrite, there will be some Fe3+ turns into Fe2+ for the valence balance at 4 f1 and 2a site. That means although its Sr2+ is substituted by the rare-earth ions, but the hyperfine field electron cloud density and electron orbit of the Fe ions are also influenced. The reason why the ion substituted strontium ferrite gets better absorption performance is: smaller lattice dimension brought bigger boundary loss, increasing of coercivity enlarged the hysteretic attenation and lattice distortion induced by ion substitution increased the dielectric loss.
Secondly, to achieve a further improvement of absorption bandwidth, composite powder of strontium and zinc ferrite was prepared using coating and one-step method respectively. Experimental result showed that 15% zinc ferrite can improve the absorption performance but too much zinc ferrite (over 30%) will do the other way because zinc ferrite is not an originally electromagnetic absorption material. it can reach -35dB reflecting loss and over 4GHz 10dB bandwidth at 2.3mm matching thickness. Because Sr ferrite material is very liable to congregate as cluster, it’s hard to achieve a complete coating on the un-uniform particles even with grinding, ultrasonic dispersing and mechanical stirring. That compromised the final performance of coating prepared ferrites. Different with pure Sr ferrite and ion-substituted ferrite, the composite powder has two reflecting loss peak. As a result of the interaction of two kinds of ferrites, the location of the peak at around 15GHz is independent with the sample thickness.
Finally, based on the research above, to prepare the La substituted ferrite and zinc ferrite composite powder using one-step method. Using this composite powder as absorption material and epoxy-resin as matrix, composite sample can be prepared with different powder vs. matrix ratio. Test result showed that when powder/matrix ratio at 1.25, good absorption performance can be obtained with 2.2mm matching thickness, -41dB minimum reflection loss and 5.7GHz 10dB bandwidth. For practical application, this composite material’s absorption performance is much better than pure Sr ferrite even at very low thickness (<2mm), well meet the requirements of real application: strong absorption, wide bandwidth, being thinner and lighter. Results showed that this composite possess both of good absorption ability and wide absorption bandwidth. M?ssbauer spectroscopy analysis showed that the composite process of the two kind of ferrite can make positive zinc ferrite turns into mixed spinal ferrite type, and when La ion exists, Zn ion can enter the Sr ferrite lattice and substitute the Fe ion at 4 f1 site. That process can enhance the specific saturation magnetization and improve the electromagnetic absorption performance.
论文首先用稀土离子替代的方法,显著改善了锶铁氧体的吸波性能,特别是提高了吸收强度。本文采用了溶胶-凝胶技术和自蔓延燃烧法相结合的方法制备镧、铈、钕三种离子替代的锶铁氧体。研究结果表明,稀土离子在锶铁氧体中的替代量取决于其离子化合价与离子半径。正四价的铈离子几乎不能进入锶铁氧体晶格,而轻稀土元素镧和钕的正三价离子替代量分别为0.15和0.1。与氧离子半径差别较小的镧离子替代量较高。离子替代使锶铁氧体的晶粒尺寸变小,颗粒团聚程度减弱;在饱和磁化强度不太降低的情况下,使矫顽力增加;吸波性能大大提高,特别是对镧离子,当替代量为0.15时,匹配厚度从2.6mm减小到2.3mm,反射损耗从-24dB降低到-37.7dB, 10dB带宽从2.7GHz(6.4-9.1GHz)拓展到4GHz(6-10GHz)。穆斯堡尔谱研究结果表明:虽然稀土离子替代的是锶铁氧体中锶位,但是对铁离子的超精细场,周围的电子云密度、以及电子轨道都有影响,当三价的镧离子替代锶铁氧体中的二价锶离子以后,为了化合价的平衡,在4 f 1和2a位,有少部分的铁离子从三价变为二价。替代锶铁氧体吸波性能提高的原因是:晶粒尺寸减小增加了界面损耗;矫顽力增大使磁滞损耗增加;离子替代引起的铁离子化合价的改变使介电损耗增加。
为了进一步拓展锶铁氧体的吸收带宽,采用了两步包覆法和一步复合法制备锌铁氧体与锶铁氧体复合粉末。结果表明,一步复合法可以有效扩展其带宽,两步法制备的复合粉末有少量的α? Fe2 O 3生成。当锌铁氧体的质量含量为15%时,两种复合方法都可以提高吸波性能,但当质量比增加到30%,吸波性能下降,这是因为锌铁氧体在所研究的频率范围内本身不具有吸波性能,过多的锌铁氧体使整体复合材料的性能下降。一步法制备的复合材料性能更加优越,在2.3mm的匹配厚度下,最低反射损耗达到-35dB,10dB带宽超过4GHz,这是由于此种方法制备的复合材料颗粒比较小,成分更加均匀,相互作用界面更多,并且没有α? Fe2 O 3存在。与纯锶铁氧体以及替代锶铁氧体不同的是,复合粉末除了存在一个随厚度变化的反射损耗峰;另外,在16GHz左右,还存在一位置不随样品厚度发生改变的反射损耗峰,这是由于两种铁氧体相互作用引起的。
最后,为了研制出一种吸波性能优越并且可以在实际中应用的吸波材料,在前面研究的基础上,选择性能最好的替代铁氧体以及比较好的复合方式,制备镧替代锶铁氧体与锌铁氧体的复合粉末。并且用以上制备的复合粉末为吸波剂,选择实际应用比较多的环氧树脂作为基体,制备吸波剂与基体质量比分别为1、1.25、1.5的复合材料。研究结果表明,当吸波介质与基体质量比为1.25时,所得复合材料的吸波性能最好,相对纯锶铁氧体有很大提高,匹配厚度从2.6mm减小到2.2mm,最小反射频率从-24dB降低到-41dB,下降了70%,10dB带宽从2.7GHz拓宽到5.7GHz,拓宽了一倍以上,展示出该材料的应用前景。特别是当样品厚度为1.5mm时,也得到了比较好的吸波性能,这在实际应用中有非常重要意义,满足了吸波涂层材料要求的吸收强,频带宽,厚度薄,质量轻的特点。
通过对镧替代锶铁氧体与锌铁氧体复合粉末的晶体结构、磁性能和穆斯堡尔谱进行研究,结果表明,镧替代锶铁氧体与锌铁氧体复合材料兼具了替代和复合两种优势。由于两种铁氧体的复合,使正尖晶石型的锌铁氧体向复合尖晶石类型转变,并且锌离子在镧离子存在的情况下,进入到锶铁氧体晶格中,替换了4 f 1位置的铁离子,从而使镧替代锶铁氧体的晶格常数变大,锌铁氧体晶格常数变小。两种铁氧体的这种相互作用使饱和磁化强度增加,从而增加了磁损耗。这些理论推断对今后复合铁氧体新型吸波材料的开发以及吸波机理的研究具有一定的参考意义。
The electromagnetic absorption material has become a hot research topic and development focus as a consequence of the booming research and widely application of GHz electromagnetic waves in modern society. As a solution of electromagnetic pollution and some special usage in military and aerospace field, electromagnetic absorption material is required to have strong absorption, wide bandwidth and proper mechanical properties. The hexagonal strontium ferrite is a good candidate material due to its high magnetic anisotropy, high saturation magnetization and excellent chemical stability. However, disadvantages like relatively weaker absorption performance and narrower frequency bandwidth constrains its application. The purpose of this work is to fabricate a Sr ferrite material with better absorption performance and wider bandwidth, as well as studying the absorption mechanism and material preparation process.
Firstly, absorption performance was remarkably improved by introducing rare-earth ion substitution into Sr ferrite. La/Ce/Nd ion substituted strontium ferrites were prepared by sol-gel technique and self-propagating combustion method. XRD analysis shows that the maximum substitute amount of La/Ce/Nd ion is 0.15, 0.1 and 0 under the process condition of 1000℃, 1.5h. Ce can’t enter the lattice due to its stable +4 valence. The substitute amount of rare-earth ions depends on their valence and ion radius. Compare to pure strontium ferrite, the lattice dimension and particle size of the ion substituted ferrite are smaller, that can remarkably improve the electromagnetic absorption performance by increasing the coercivity without causing any significant deterioration in specific saturation magnetization. Especially for La-substituted ferrite, when the substitute amount is 0.15, compared with pure strontium ferrite, the matching thickness can be reduced from 2.6mm to 2.3mm, the minimum reflection loss decreases from -24dB to -37.7dB. and 10db bandwidth can be expanded from 2.7GHz (6.4-9.1GHz) to 4GHz (6-10GHz). The M?ssbauer spectroscopy showed that when the La3+ substituted the Sr2+ in the ferrite, there will be some Fe3+ turns into Fe2+ for the valence balance at 4 f1 and 2a site. That means although its Sr2+ is substituted by the rare-earth ions, but the hyperfine field electron cloud density and electron orbit of the Fe ions are also influenced. The reason why the ion substituted strontium ferrite gets better absorption performance is: smaller lattice dimension brought bigger boundary loss, increasing of coercivity enlarged the hysteretic attenation and lattice distortion induced by ion substitution increased the dielectric loss.
Secondly, to achieve a further improvement of absorption bandwidth, composite powder of strontium and zinc ferrite was prepared using coating and one-step method respectively. Experimental result showed that 15% zinc ferrite can improve the absorption performance but too much zinc ferrite (over 30%) will do the other way because zinc ferrite is not an originally electromagnetic absorption material. it can reach -35dB reflecting loss and over 4GHz 10dB bandwidth at 2.3mm matching thickness. Because Sr ferrite material is very liable to congregate as cluster, it’s hard to achieve a complete coating on the un-uniform particles even with grinding, ultrasonic dispersing and mechanical stirring. That compromised the final performance of coating prepared ferrites. Different with pure Sr ferrite and ion-substituted ferrite, the composite powder has two reflecting loss peak. As a result of the interaction of two kinds of ferrites, the location of the peak at around 15GHz is independent with the sample thickness.
Finally, based on the research above, to prepare the La substituted ferrite and zinc ferrite composite powder using one-step method. Using this composite powder as absorption material and epoxy-resin as matrix, composite sample can be prepared with different powder vs. matrix ratio. Test result showed that when powder/matrix ratio at 1.25, good absorption performance can be obtained with 2.2mm matching thickness, -41dB minimum reflection loss and 5.7GHz 10dB bandwidth. For practical application, this composite material’s absorption performance is much better than pure Sr ferrite even at very low thickness (<2mm), well meet the requirements of real application: strong absorption, wide bandwidth, being thinner and lighter. Results showed that this composite possess both of good absorption ability and wide absorption bandwidth. M?ssbauer spectroscopy analysis showed that the composite process of the two kind of ferrite can make positive zinc ferrite turns into mixed spinal ferrite type, and when La ion exists, Zn ion can enter the Sr ferrite lattice and substitute the Fe ion at 4 f1 site. That process can enhance the specific saturation magnetization and improve the electromagnetic absorption performance.
引文
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