溶胶—共沉淀法合成硅酸锆包裹硫硒化镉色料的研究

发布时间：2018-03-25 06:02

本文选题：硅酸锆包裹硫硒化镉　切入点：溶胶-共沉淀法　出处：《华南理工大学》2015年硕士论文

【摘要】：硅酸锆包裹硫硒化镉色料经过近半世纪的应用,一直都是作为其他红色色料发色的参照标准。虽然应用时间长,但仍然存在不少需要改进的问题,尤其是在今天这样一个科技大变革的时代,对传统色料提出了新要求,如粒度、耐温性等。本课题主要研究对象就是该色料,旨在目前水平基础上探讨一些改进方案和益尝试。本课题采用了X射线衍射仪、扫面电子显微镜分析、色度分析仪、偏光显微镜分析、空气动力学粒径谱仪、激光粒度仪、傅里叶红外变换分析仪等手段对其进行分析表征。课题主要研究了溶胶-共沉淀法制备硅酸锆包裹硫硒化镉色料在传统水溶液体系和有机体系中的合成工艺。在水溶液体系中主要探讨的问题主要是两种加料工艺、更换硫源和硅源、固相合成温度、气氛剂等工艺因素的影响。实验表明:改进的硫源后置法对控制前驱体的团聚有较好效果,色料中具有4.2%小于2μm的小颗粒,但对整个色料的呈色效果改进并不明显;以硫脲为硫源取代硫化钠为能进一步控制前驱体的团聚,与硫化钠为硫源之间的色度差为△L=-0.76,△a=0.72,△b=0.34,硫脲有利于色料包裹率的提升;以HL365型白炭黑取代五水硅酸钠为硅源能大幅减少色料孔洞,与五水硅酸钠为硅源之间的色度差,在1100℃釉中为△L=0.66,△a=-0.16,△b=0.15,1100℃下合成色料的包裹量为6.1%,在1250℃釉中为△L=0.33,△a=1.13,△b=0.71,在高温釉中具有明显优势。在乙醇胺体系中主要探讨了乙醇胺体系对色料各性能的影响。实验表明:在适宜浓度的乙醇胺体系中,前驱体的分散性优于水溶液体系,粒度在20~100 nm;色料颗粒的酸洗孔随着乙醇胺的浓度升高而减少,浓度为100%时,孔洞基本消失,当乙醇胺浓度为50%时,色料的呈色效果最佳,色度值坐标为L=41.67,a=48.64,b=30.32,色剂包裹量为6.37%,且优于水溶液体系,乙醇胺浓度过高时,有机质的残留是影响色料呈色的主要原因,乙醇胺浓度高于75%时,呈色效果迅速变差;适宜的乙醇胺体系中色料粒度分布比水溶液体系稍微宽,但粒度分布于0.1~1μm之间的细颗粒有14.96%,小于2μm的颗粒有25.89%,这部分细颗粒的存在使此色料应用于陶瓷喷墨打印成为可能。
[Abstract]:Zirconium silicate inclusions of cd-s-se pigment after application for half a century, has been used as other red color standard. Although the application of a long time, but there are still many problems need to be improved, especially in such a technology era of great change, the traditional color put forward new requirements, such as granularity, temperature resistance and so on. The main topic of the research object is the pigment, to the current level on the basis of the improved scheme and beneficial attempt. This thesis adopts X ray diffraction, scanning electron microscopy analysis, colorimetric analyzer, polarizing microscope analysis, aerodynamic particle size analyzer, laser particle analyzer, analysis and characterization the Fourier transform infrared analyzer. Studying the sol coprecipitation synthesis process of preparation of zirconium silicate enwrapped cd-s-se pigment in the traditional aqueous and organic system. In aqueous solution, the main problems are mainly two kinds of charging process, the replacement of sulfur and silicon source, solid phase synthesis temperature, influence of atmosphere agent process factors. The experimental results show that the improved method of post sulfur source has good effect on controlling the precursor reunion, with 4.2% small particles of pigment is less than 2 m but on the whole, the pigment color effect of the improvement is not obvious; with thiourea as sulfur source to replace sodium sulfide to further control the agglomeration of precursors, and sodium sulfide for Delta L=-0.76, Delta a=0.72, Delta b=0.34 as sulfur source between chroma, thiourea can enhance the rate of pigment coated with silica instead of type HL365; five water sodium silicate as silicon source can greatly reduce the pigment and water holes, five sodium silicate as silicon source chromaticity difference between 1100 degrees in the glaze for Delta L=0.66, Delta a=-0.16, Delta b=0.151100 the amount of synthetic pigment is 6.1% degrees, 1250 degrees in the glaze for Delta L=0.33 , Delta a=1.13, Delta b=0.71, has obvious advantages in high temperature glaze. In ethanol amine system mainly discussed the influence of ethanolamine system on the properties of the pigment. Experiment results show that the suitable concentration of ethanol amine system, dispersion is better than water solution precursor, 20~100 in size nm; pickling hole of pigment particles decreased with the concentration of ethanolamine increased, the concentration is 100%, the hole disappeared, when the ethanol concentration is 50%, the pigment color is best, chroma coordinates L=41.67, a=48.64, b=30.32, color agent amount is 6.37%, which is better than the aqueous solution, ethanol concentration is too high, the residual organic matter is the main reason for the influence of pigment color, ethanolamine concentration was higher than 75%, the color effect of rapid variation; ethanol amine system color material distribution with suitable size slightly wider than the aqueous solution system, fine particle size distribution but between 0.1 ~1 m 14. 96%, the particles less than 2 mu m have 25.89%. The presence of this part of fine particles makes it possible to apply this color to ceramic ink-jet printing.

【学位授予单位】：华南理工大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ174.45

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