氧化锌及铁酸镍三维光子晶体的制备及性能研究

发布时间：2018-04-08 21:18

本文选题：蛋白石结构　切入点：反蛋白石结构　出处：《陕西科技大学》2017年硕士论文

【摘要】：光子晶体本质上是一种有序结构,由不同介质在空间周期性排列得到。结构特殊性赋予光子晶体材料许多特性,比如光子带隙、光子局域效应等。其中,光子带隙是其最基本的特性,类似于半导体能带结构中的带隙对电子的作用,光子带隙也可以对光子起到调制作用。本文分别介绍了聚甲基丙烯酸甲酯(PMMA)、ZnO蛋白石光子晶体材料及ZnO、NiFe_2O_4反蛋白石光子晶体材料的制备,通过对PMMA、ZnO蛋白石形成的结构色、ZnO反蛋白石的光催化性能及NiFe_2O_4反蛋白石的微波吸收性能的表征,研究这种特殊微结构对材料各种性能的影响,以便未来可以扩展出光子晶体更多潜在应用。(1)采用无皂乳液聚合法,制备了单分散性良好且粒径均一可控的胶体聚甲基丙烯酸甲酯(PMMA)微球,采用XRD,SEM,FT-IR,UV-Vis反射光谱等对微球及微球自组装后得到的光子晶体结构色进行了表征。结果表明,所制备的微球为非晶体,球面较为光滑,粒径较为均一,介于150~300nm;粒径受单体浓度、引发剂加入量、反应温度和搅拌速度影响。微球粒径随单体含量增加而变大;随引发剂添加量和搅拌速度的增加呈现出先增大后减小的趋势;反应最佳温度为75 oC。组装成膜的结构色与微球粒径之间呈正比关系,可随微球粒径的增大发生红移;光子晶体中存在的缺陷及过度受热会使光子晶体的有效折射率减小,结构色亮度降低。(2)采用溶胶凝胶两步法制备了单分散性良好、粒径均一可控的ZnO胶体微球,采用XRD,SEM,TEM,FT-IR,TG-DSC及UV-Vis反射光谱等对影响微球粒径的因素及微球自组装后得到的光子晶体结构色进行表征。分析结果表明,制备的ZnO微球为纯净的纤锌矿结构,由ZnO颗粒团聚而成,球面较为粗糙,粒径介于150~500 nm之间。微球粒径随着前驱液加入量增加而逐渐变小。微球内含有约30%的有机物残留,煅烧后微球会发生轻微收缩。采用重力沉积法组装得到ZnO光子晶体结构色层,乳液浓度越大,得到的结构色层越厚;相比于PMMA结构色,ZnO结构色层更耐温。(3)采用自制的PMMA光子晶体为模板,金属离子硝酸盐混合液为前驱液,通过模板法成功制备了具有反蛋白石结构的ZnO材料,采用XRD,SEM,TEM,TG,DRS等对材料的形貌及光催化性能进行分析。研究发现,制备的ZnO反蛋白石为纤锌矿结构,其结构受到填充前驱液的浓度、浸渍次数及模板移除温度的影响,尤其模板移除温度过高会导致结构变形坍塌。光催化性能分析发现,反蛋白石具有的有序连通孔结构和慢光效应,有效提高了光利用率和有机染料转移效率,使其光催化性能优于同反应条件下制备的ZnO材料。(4)采用模板法制备了NiFe_2O_4反蛋白石材料,采用XRD,SEM,TEM,VNA等对样品的物相、形貌及性能进行了表征。研究发现,制备的NiFe_2O_4为纯相的尖晶石结构,结晶性良好;NiFe_2O_4反蛋白石具有完整的三维有序孔结构,孔形成于有机模板的煅烧移除,光滑的孔壁由铁酸盐纳米颗粒组成,颗粒尺寸均小于27 nm,孔径介于70~200 nm之间。与普通无序的铁酸盐纳米颗粒材料的吸波性能进行对比可以发现:其反射损耗最大可达27.5 dB,高于无序NiFe_2O_4颗粒的17.4 d B,使其吸波性能有了很大提高。
[Abstract]:Photonic crystal is essentially a kind of ordered structure by different media periodically arranged in space. The special structure of photonic crystal materials gives many characteristics, such as photonic band gap photonic localization effect. The photonic band gap is the most basic feature, similar to the effect of band gap semiconductor energy band structure of electronic, photonic band gap can also modulate the photon. This paper introduces the polymethylmethacrylate (PMMA), ZnO opal photonic crystal materials and ZnO, NiFe_2O_4 inverse opal materials preparation, based on the PMMA structure, ZnO color opal formation, characterization of absorption properties of ZnO inverse opal and photocatalytic properties NiFe_2O_4 inverse opal microwave, study the special micro structure of various properties of materials, so that the future can be extended to more potential applications of photonic crystal. (1) using soap free emulsion polymerization Legitimate, good monodispersity and uniform particle size controllable colloid was prepared by polymethyl methacrylate (PMMA) microspheres, using XRD, SEM, FT-IR, color of the photonic crystal structure and self-assembly of microspheres microspheres obtained were characterized by UV-Vis spectroscopy. The results indicated that the prepared microspheres for non spherical crystal, more smooth, uniform sizes, ranging from 150~300nm; particle size by monomer concentration, initiator dosage, reaction temperature and stirring speed. The size of microspheres with monomer content increases; with the initiator dosage and stirring speed increase increases first and then decreases; the optimal reaction temperature 75 oC. assembly is proportional to the membrane structure color and particle size, particle size increases with redshift; defects in photonic crystals and excessive heating will make the effective refractive index of the photonic crystals decreases, structural color brightness Reduced. (2) preparation of monodispersed sol gel by two - step method, colloidal ZnO microspheres, uniform particle size controllable by XRD, SEM, TEM, FT-IR, TG-DSC and UV-Vis photonic crystal structure color reflection spectrum effect on particle size factors and microspheres self-assembly obtained were characterized. The results show that the ZnO microspheres for the wurtzite structure of pure, by the agglomeration of ZnO particles into the spherical surface is rough, the particle size is 150~500 nm. The particle size of precursor solution with addition of organic matter decreased. Microspheres containing about 30% residues, the calcined microspheres will happen slight shrinkage. Assembly of ZnO photonic crystal layer by gravity deposition method, emulsion concentration and the structure of the layer is thicker than the PMMA structure; ZnO structure layer color, more resistant to temperature. (3) the PMMA photonic crystal made of metal ion as template, nitrate mixture As the liquid precursor solution, the template method was successfully prepared with inverse opal structure of ZnO material, using XRD, SEM, TEM, TG, DRS etc. Analysis of morphology and light on the catalytic performance of materials. The study found that the preparation of ZnO inverse opal is of wurtzite structure. Its structure is filled with precursor concentration liquid, effect of impregnation times and template removal temperature, especially the template removal too high temperature will cause the deformation of structure collapse. Analysis showed that the photocatalytic properties of inverse opal is orderly connected pore structure and slow light effect, effectively improves the light utilization rate and organic dye transfer efficiency, the preparation of ZnO photocatalytic material to make it the performance is better than the same reaction conditions. (4) NiFe_2O_4 inverse opal materials was prepared by template method using XRD, SEM, TEM, VNA of the sample phase, morphology and properties were investigated. The study found that the prepared NiFe_2O_4 is pure phase spinel. The good crystallinity; NiFe_2O_4 inverse opal with 3D ordered pore structure, calcination to remove the hole formed in the organic template, smooth hole wall is composed of ferrite nano particles, the particle size was less than 27 nm, pore size between 70~200 and nm. Can be found between the absorbing properties of ferrite nanoparticles of common salt random: the maximum reflection loss of up to 27.5 dB, 17.4 d higher than the disordered NiFe_2O_4 particles B, the absorbing performance has been greatly improved.

【学位授予单位】：陕西科技大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O734

【参考文献】