本文選題：硅酸鋯包裹硫硒化鎘　切入點：溶膠-共沉淀法　出處：《華南理工大學》2015年碩士論文

【摘要】：硅酸鋯包裹硫硒化鎘色料經(jīng)過近半世紀的應用,一直都是作為其他紅色色料發(fā)色的參照標準。雖然應用時間長,但仍然存在不少需要改進的問題,尤其是在今天這樣一個科技大變革的時代,對傳統(tǒng)色料提出了新要求,如粒度、耐溫性等。本課題主要研究對象就是該色料,旨在目前水平基礎上探討一些改進方案和益嘗試。本課題采用了X射線衍射儀、掃面電子顯微鏡分析、色度分析儀、偏光顯微鏡分析、空氣動力學粒徑譜儀、激光粒度儀、傅里葉紅外變換分析儀等手段對其進行分析表征。課題主要研究了溶膠-共沉淀法制備硅酸鋯包裹硫硒化鎘色料在傳統(tǒng)水溶液體系和有機體系中的合成工藝。在水溶液體系中主要探討的問題主要是兩種加料工藝、更換硫源和硅源、固相合成溫度、氣氛劑等工藝因素的影響。實驗表明:改進的硫源后置法對控制前驅(qū)體的團聚有較好效果,色料中具有4.2%小于2μm的小顆粒,但對整個色料的呈色效果改進并不明顯;以硫脲為硫源取代硫化鈉為能進一步控制前驅(qū)體的團聚,與硫化鈉為硫源之間的色度差為△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鈉為硅源能大幅減少色料孔洞,與五水硅酸鈉為硅源之間的色度差,在1100℃釉中為△L=0.66,△a=-0.16,△b=0.15,1100℃下合成色料的包裹量為6.1%,在1250℃釉中為△L=0.33,△a=1.13,△b=0.71,在高溫釉中具有明顯優(yōu)勢。在乙醇胺體系中主要探討了乙醇胺體系對色料各性能的影響。實驗表明:在適宜濃度的乙醇胺體系中,前驅(qū)體的分散性優(yōu)于水溶液體系,粒度在20~100 nm;色料顆粒的酸洗孔隨著乙醇胺的濃度升高而減少,濃度為100%時,孔洞基本消失,當乙醇胺濃度為50%時,色料的呈色效果最佳,色度值坐標為L=41.67,a=48.64,b=30.32,色劑包裹量為6.37%,且優(yōu)于水溶液體系,乙醇胺濃度過高時,有機質(zhì)的殘留是影響色料呈色的主要原因,乙醇胺濃度高于75%時,呈色效果迅速變差;適宜的乙醇胺體系中色料粒度分布比水溶液體系稍微寬,但粒度分布于0.1~1μm之間的細顆粒有14.96%,小于2μm的顆粒有25.89%,這部分細顆粒的存在使此色料應用于陶瓷噴墨打印成為可能。
[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.

【學位授予單位】：華南理工大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TQ174.45

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