光子晶体结构色釉的制备与表征

发布时间：2018-05-05 00:22

本文选题：SiO2 + Ti　；参考：《陕西科技大学》2015年硕士论文

【摘要】：结构色是一种由物质微观结构引起光的折射、干涉、衍射、散射等作用而产生的颜色。目前,结构色在一些领域的应用研究已非常活跃,但在陶瓷釉方面的研究却鲜有涉及。本文通过制备Si O2、Ti O2及Si O2@Ti O2三种光子晶体结构色用单分散微球,以垂直沉积法分别在玻璃和瓷胎表面自组装,制得了颜色艳丽的结构色釉,通过对结构色釉的各种影响因素进行深入地探讨和分析,以期为光子晶体仿生结构色在玻璃及瓷胎上的应用提供一定的实验基础与理论指导。(1)采用溶胶凝胶法制备了不同粒径的单分散Si O2胶体微球,并以垂直沉积自组装法将其在玻璃及瓷胎表面制备了颜色艳丽的结构色釉。研究了微球粒径的工艺控制方法及微球尺寸、热处理温度、膜层厚度、不同基底以及微球后处理对结构色的影响。SEM、XRD、红外光谱等分析表明:在Si O2微球制备过程中,随着反应过程中氨水和正硅酸乙酯浓度的增大,微球粒径逐渐增大;水解、缩聚反应温度升高,微球尺寸会逐渐减小;体系水含量增大,Si O2微球尺寸先增大后减小,存在一个峰值。薄膜分析表明:具有良好三维有序密堆积结构的薄膜,其颜色随着自组装用微球粒径的增大发生红移;热处理过程可使微球收缩,粒径减小,晶面间距缩短,结构色釉颜色发生微弱蓝移。研究发现:胶体粒子浓度过大,将导致膜层过厚,结构色釉颜色饱和度降低;瓷胎与玻璃基相比,所得结构色膜层缺陷少、制备周期短、颜色更为均一艳丽,且不易出现肉眼可见的横向“条纹”;直接采用反应后悬浮液中的微球,比之热处理后的微球进行自组装,所得结构色的颜色红移且色彩更为鲜亮。(2)采用溶胶凝胶法制备了不同粒径的单分散Ti O2胶体微球,并以垂直沉积自组装法将其在玻璃及瓷胎表面制备了颜色艳丽的结构色釉。研究了微球粒径的工艺控制方法、不同基底以及微球尺寸对结构色的影响。SEM、XRD分析表明:在Ti O2微球制备过程中,随着钛源浓度增大,微球粒径逐渐增大;随着氨水、乙腈含量及反应温度逐渐增加,微球粒径逐渐减小;温度越低,微球表面越光滑;乙腈含量超过一定值,小的薄层碎片会从Ti O2微球表面脱落,使微球性质变差。薄膜分析表明:相同条件下,在瓷胎上制得的结构色层近乎白色,颜色不如玻璃基呈色效果好;与Si O2微球相似,Ti O2光子晶体结构颜色也会随着自组装用的Ti O2微球颗粒的增大而发生红移,但Ti O2光子晶体结构色层所显现的颜色并不如Si O2的鲜亮,且相同颜色下,Ti O2结构颜色所用的微球粒径要比Si O2硅结构颜色所用的微球粒径小;根据实验推算结果可知合成的Ti O2微球的折射率约为1.806,与水合非晶氧化钛的理论值刚好相符。(3)通过向氧化硅球种子溶液中加入钛前驱液后,合成了单分散Si O2@Ti O2核壳结构胶体微球,以垂直沉积自组装法将其在玻璃表面制备了结构色釉。研究了包覆前后结构色釉层颜色、物相的变化。SEM、EDS及XRD分析表明:合成的Si O2@Ti O2核壳结构微球同Si O2微球相似,均为无定型态,至600℃出现微弱的锐钛矿相,900℃开始转变为金红石相;与包覆前的Si O2结构色釉的显色相比,包覆后的Si O2@Ti O2结构色发生红移,显示微弱的红色,同时饱和度及明度都有很大程度的降低。
[Abstract]:Structural color is a color produced by the refraction, interference, diffraction and scattering of light, which is caused by the microscopic structure of the material. At present, the application of structural color in some fields is very active, but the research on the ceramic glaze is rarely involved. In this paper, three kinds of photonic crystal structures of Si O2, Ti O2 and Si O2@Ti O2 are prepared by monodisperse microdispersion Ball, with vertical deposition on the surface of glass and enamel, self-assembled on the surface of glass and porcelain, the color glaze of colorful structure was made. The influence factors of the structure color glaze were deeply discussed and analyzed in order to provide the experimental basis and theoretical guidance for the application of the photonic crystal biomimetic structure color on the glass and porcelain. (1) the sol-gel method was used. The monodisperse Si O2 colloid microspheres with different particle sizes were prepared by the gel method, and the colourful colored glazes were prepared on the surface of glass and porcelain by the vertical deposition self assembly method. The process control method of the particle size and the size of the microspheres, the heat treatment temperature, the thickness of the film layer, the different substrate and the effect of the post treatment on the structure color of the microspheres were studied.SEM. XRD, IR spectra and other analysis showed that the size of microspheres increased gradually with the increase of the concentration of ammonia and ethyl orthosilicate during the preparation of Si O2 microspheres, and the size of microspheres decreased gradually, and the water content of the system increased, and the size of Si O2 microspheres increased first and then decreased, and there was a peak. Thin film analysis was found. It is shown that the color of the thin film with good three-dimensional and ordered dense packing structure is red shift with the increase of the particle size of the self assembled microspheres. The heat treatment process can make the microspheres shrink, the particle size decreases, the spacing of the crystal surface is shortened, and the color of the structural color glaze is weak blue shift. Compared with the glass base, the ceramic tire has less defects, short preparation period, more uniform color, and not easy to appear horizontal "stripes", and the microspheres in the suspension after reaction are self-assembled, the color of the structure color is red shift and the color is brighter. (2) the monodisperse Ti O2 colloid microspheres with different particle sizes were prepared by the sol-gel method, and the colourful colored glazes were prepared on the surface of glass and porcelain by the vertical deposition self assembly method. The process control method of the particle size of the microspheres was studied. The effects of different substrates and microspheres size on the structure color were.SEM. The XRD analysis showed that in Ti O2 microsphere In the process of ball preparation, with the increase of the concentration of titanium, the particle size of the microspheres increases gradually. With the ammonia water, the content of acetonitrile and the reaction temperature gradually increase, the particle size decreases gradually, the lower the temperature, the smooth surface of the microspheres, the content of acetonitrile more than a certain value, the small thin layer fragments will fall off the surface of Ti microspheres and make the properties of microspheres worse. Thin film analysis shows that: Under the same condition, the structural color layer made on the ceramic tire is almost white, and the color is not better than the glass based color. Similar to the Si O2 microspheres, the Ti O2 photonic crystal structure color will be red shift with the increase of Ti O2 microspheres, but the color of the Ti O2 photonic crystal structure is not as bright as Si O2, and the phase is not bright. Under the same color, the size of the microspheres used in the Ti O2 structure color is smaller than that of the Si O2 silicon microspheres. According to the experimental results, the refractive index of the synthesized Ti O2 microspheres is about 1.806, which coincide with the theoretical value of the hydrated amorphous titanium oxide. (3) the monomer was synthesized by adding the titanium precursor to the seed solution of the silicon oxide ball. The Si O2@Ti O2 core shell colloid microspheres were dispersed and the structure color glaze was prepared on the glass surface by the vertical deposition self assembly method. The color glaze layer before and after coating and the phase change.SEM, EDS and XRD analysis showed that the synthesized Si O2@Ti O2 core shell microspheres were similar to Si O2 microsphere, all were amorphous, and were weak at 600 degrees C. Anatase phase begins to change to rutile phase at 900 C. Compared with the color display of Si O2 structure color glaze before coating, the Si O2@Ti O2 structure color after coating is red shift, showing a weak red, and the saturation and lightness are greatly reduced.

【学位授予单位】：陕西科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ174.43

【参考文献】