玻璃微珠基复合吸波材料的制备及其性能研究
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摘要
玻璃微珠具有密度低、比表面积大、热稳定性好、化学稳定性好、机械强度高、流动性好等优点,其主要的化学组成为SiO2和Al2O3。玻璃微珠虽然本身并不具有吸波性能,但却是制备吸波材料的良好基材。以玻璃微珠为核,通过化学镀在其表面镀覆一层具有良好软磁性能的铁镍合金或铁纳米粒子,既可以有效的降低吸波剂的密度,还可以获得不俗的吸波性能。本文在前人研究的基础上设计出以玻璃微珠为载体,采用化学镀法分别制备出了表面包覆铁镍合金和铁纳米粒子的玻璃微珠基核壳复合粒子,并对其表面形貌、组成成分及静磁性能进行了表征,研究了其电磁参数及电磁特性,得到以下结论：
(1)通过置换金属离子法和氨基化改性法对玻璃微珠表面进行活化处理,采用化学镀法分别得到了球形结构和准膜状结构的铁镍合金包玻璃微珠核壳复合粒子,具有球形结构的铁镍合金包覆玻璃微珠核壳复合粒子的饱和磁化强度Ms为34.54emu/g,高于准膜状结构的铁镍合金包覆玻璃微珠核壳复合粒子的饱和磁化强度(24.9emu/g)。在化学镀铁镍的最佳工艺条件为：温度为50℃,pH值为10,粉体装载量为8 g／L。
(2)采用化学镀法和溶胶凝胶法在玻璃微珠表面分别包覆了铁纳米粒子及SiO2层,并研究了SiO2层形成的机理。通过SEM和XRD分析表明玻璃微珠表面上分别地包覆了一层铁和SiO2层,磁滞回线分析得包覆SiO2前粉末的矫顽力Hc为94.86kOe,饱和磁化强度Ms为14.98emu/g,而包覆SiO2后粉末的矫顽力Hc为100.55kOe,饱和磁化强度Ms为23.01emu／g。
(3)矢量网络分析仪对玻璃微珠／铁镍合金、玻璃微珠／铁复合材料的电磁参数分析表明：当填充比玻璃微珠／铁镍：石蜡=1：4,厚度d=2.5mm时,球形结构的玻璃微珠／铁镍复合材料的最大反射损耗值R=-49.28dB,且R<-10dB的频宽约为9GHz,而膜状的玻璃微珠／铁镍复合材料的最大反射损耗值R=-33.8dB,且R<-10dB的频宽约为4GHz。包覆二氧化硅后的玻璃微珠／铁核壳复合粒子的最大反射损耗值为-15.45dB,而未包覆二氧化硅的玻璃微珠／铁核壳复合粒子的最大反射损耗值为-11.17dB。
Hollow glass microspheres is a good base material for synthesizing the wave absorption materials due to the characteristics of low density, huge surface area, excellent thermal and chemical stability, high mechanical strength and fine fluidity. Microwave absorptive materials such as iron-nickel alloy and iron nano-particles coated on hollow glass microspheres via electroless plating can effectively reduce the density of absorbing agents. In this paper, the iron-nickel alloy and iron coated core-shell particles are prepared by using hollow glass microspheres as the base core through electroless plating. The morphology and structure of the hollow glass microspheres-based core-shell particles are characterized; the magnetic properties and the microwave absorption properties are also discussed. The conclusions are followed:
replacement of metal ions method and the amino-modified method are used to improved the activity of hollow glass microspheres, and the obtained iron-nickel alloy coated hollow glass microspheres have two different morphologies. The spherical structure of the iron-nickel alloy coated hollow glass microspheres core-shell particles of the saturation magnetization Ms is 34.54emu/g, higher than the membranous structure of the iron-nickel alloy coated hollow glass microspheres core-shell particles of the saturation magnetization(24.9emu/g). The optimal conditions of electroless plating iron-nickel alloy coated hollow glass microspheres is temperature 50℃, pH= 10, powder loading was 8 g/L.
Electroless plating and sol-gel method are used to coated iron nanoparticles and the SiO2 layer on the surface of hollow glass microspheres respectively, and mechanism of the formation of SiO2 layer is also studied. SEM and XRD analysis show that the surface of hollow glass microspherescoated with the iron and SiO2 layers, respectively. Magnetic hysteresis curve analysis are pre-coated SiO2 powder coercivity He is 94.86kOe, saturation magnetization Ms is 14.98emu/g, while the post-coated SiO2 powder coercivity He as 100.55kOe, saturation magnetization Ms is 23.01emu/g.
vector network analyzer on the glass microspheres/iron-nickel alloy, glass microspheres/Fe Composite Materials Characterization analysis shows that:when the filling ratio of glass microspheres/Fe-Ni:wax=1:4, thickness d= 2.5mm, the spherical structure of glass microspheres/iron-nickel composites the maximum reflection loss value of R=-49.28dB, and R<-10dB bandwidth is about 9GHz, while the membranous glass microspheres/iron-nickel composites the maximum reflection loss value of R=-33.8dB, and R<-10dB bandwidth is about 4GHz. the maximum reflection loss value of glass microspheres/iron composites is-11.17dB, while after coat a layer of SiO2, the maximum reflection loss value increase to-14.56dB.
(1)通过置换金属离子法和氨基化改性法对玻璃微珠表面进行活化处理,采用化学镀法分别得到了球形结构和准膜状结构的铁镍合金包玻璃微珠核壳复合粒子,具有球形结构的铁镍合金包覆玻璃微珠核壳复合粒子的饱和磁化强度Ms为34.54emu/g,高于准膜状结构的铁镍合金包覆玻璃微珠核壳复合粒子的饱和磁化强度(24.9emu/g)。在化学镀铁镍的最佳工艺条件为：温度为50℃,pH值为10,粉体装载量为8 g／L。
(2)采用化学镀法和溶胶凝胶法在玻璃微珠表面分别包覆了铁纳米粒子及SiO2层,并研究了SiO2层形成的机理。通过SEM和XRD分析表明玻璃微珠表面上分别地包覆了一层铁和SiO2层,磁滞回线分析得包覆SiO2前粉末的矫顽力Hc为94.86kOe,饱和磁化强度Ms为14.98emu/g,而包覆SiO2后粉末的矫顽力Hc为100.55kOe,饱和磁化强度Ms为23.01emu／g。
(3)矢量网络分析仪对玻璃微珠／铁镍合金、玻璃微珠／铁复合材料的电磁参数分析表明：当填充比玻璃微珠／铁镍：石蜡=1：4,厚度d=2.5mm时,球形结构的玻璃微珠／铁镍复合材料的最大反射损耗值R=-49.28dB,且R<-10dB的频宽约为9GHz,而膜状的玻璃微珠／铁镍复合材料的最大反射损耗值R=-33.8dB,且R<-10dB的频宽约为4GHz。包覆二氧化硅后的玻璃微珠／铁核壳复合粒子的最大反射损耗值为-15.45dB,而未包覆二氧化硅的玻璃微珠／铁核壳复合粒子的最大反射损耗值为-11.17dB。
Hollow glass microspheres is a good base material for synthesizing the wave absorption materials due to the characteristics of low density, huge surface area, excellent thermal and chemical stability, high mechanical strength and fine fluidity. Microwave absorptive materials such as iron-nickel alloy and iron nano-particles coated on hollow glass microspheres via electroless plating can effectively reduce the density of absorbing agents. In this paper, the iron-nickel alloy and iron coated core-shell particles are prepared by using hollow glass microspheres as the base core through electroless plating. The morphology and structure of the hollow glass microspheres-based core-shell particles are characterized; the magnetic properties and the microwave absorption properties are also discussed. The conclusions are followed:
replacement of metal ions method and the amino-modified method are used to improved the activity of hollow glass microspheres, and the obtained iron-nickel alloy coated hollow glass microspheres have two different morphologies. The spherical structure of the iron-nickel alloy coated hollow glass microspheres core-shell particles of the saturation magnetization Ms is 34.54emu/g, higher than the membranous structure of the iron-nickel alloy coated hollow glass microspheres core-shell particles of the saturation magnetization(24.9emu/g). The optimal conditions of electroless plating iron-nickel alloy coated hollow glass microspheres is temperature 50℃, pH= 10, powder loading was 8 g/L.
Electroless plating and sol-gel method are used to coated iron nanoparticles and the SiO2 layer on the surface of hollow glass microspheres respectively, and mechanism of the formation of SiO2 layer is also studied. SEM and XRD analysis show that the surface of hollow glass microspherescoated with the iron and SiO2 layers, respectively. Magnetic hysteresis curve analysis are pre-coated SiO2 powder coercivity He is 94.86kOe, saturation magnetization Ms is 14.98emu/g, while the post-coated SiO2 powder coercivity He as 100.55kOe, saturation magnetization Ms is 23.01emu/g.
vector network analyzer on the glass microspheres/iron-nickel alloy, glass microspheres/Fe Composite Materials Characterization analysis shows that:when the filling ratio of glass microspheres/Fe-Ni:wax=1:4, thickness d= 2.5mm, the spherical structure of glass microspheres/iron-nickel composites the maximum reflection loss value of R=-49.28dB, and R<-10dB bandwidth is about 9GHz, while the membranous glass microspheres/iron-nickel composites the maximum reflection loss value of R=-33.8dB, and R<-10dB bandwidth is about 4GHz. the maximum reflection loss value of glass microspheres/iron composites is-11.17dB, while after coat a layer of SiO2, the maximum reflection loss value increase to-14.56dB.
引文
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