Comparative Study of the Synthesis of a Red Ceramic Pigment Using Microwave Heat Treatment

Colorants Pub Date : 2023-08-08 DOI:10.3390/colorants2030025
Eva Miguel, Guillermo Paulo-Redondo, J. B. Carda Castelló, I. Nebot-Díaz
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Abstract

In this study, a new red ceramic pigment has been developed within a perovskite structure, and microwave heat treatments have been applied. Those red ceramic pigments within the YAlO3 system doped with chromium with the nominal composition Y0.98Al0.98Cr0.04O3 were synthesized by traditional routes and alternative methods like coprecipitation. Also, heat treatment has been studied comparing a traditional electric and microwave kiln. Different flux agents have been incorporated to improve the synthesis reaction. Prepared pigments have been characterized by X-ray diffraction (XRD) as having a predominant phase of perovskite structure, which is responsible for the red shade, and a minority garnet phase that causes more brown colorations. Studies by Ultraviolet-Visible spectroscopy gave rise to a series of absorption bands that indicate the presence of Cr(III) in the octahedral position corresponding to perovskite and Cr(IV) corresponding to garnet in both the octahedral and tetrahedral positions. The perovskite phase is favored with the use of flux mix, corroborating the UV-visible results and being more pronounced in traditional high temperature thermal treatments. The coprecipitation route has been studied to increase the reactivity of the particles given their nanometric size; however, this reactivity favors a greater appearance of undesirable garnet phases with both types of flux. Scanning Electron Microscopy (SEM) micrographs offer information obtained from the secondary electrons of predominantly cubic crystalline phases with sizes between 1 µm and 2 µm in pigments synthesized via the traditional method and sizes less than 1µm together with the glassy phase in pigments synthesized via coprecipitation. Microwave thermal treatments have been studied, obtaining pigments with a majority structure of perovskite and garnet at lower temperatures and relatively short synthesis times. The feasibility of use in porous single-fired ceramic glazes has been studied, whose chromatic coordinates have been collected using an Ultraviolet-Visible Spectrophotometer based on the CIEL*a*b* system.
微波热处理合成红色陶瓷颜料的比较研究
在本研究中,开发了一种新的钙钛矿结构的红色陶瓷颜料,并应用了微波热处理。采用传统方法和共沉淀法合成了掺杂铬的YAlO3体系内的红色陶瓷颜料,其标称成分为Y0.98Al0.98Cr0.04O3。并对传统电窑和微波窑的热处理进行了对比研究。加入了不同的助熔剂以改善合成反应。制备的颜料经x射线衍射(XRD)表征,其主要相为钙钛矿结构,这是导致红色的原因,而少数石榴石相则导致更多的棕色。紫外-可见光谱研究显示,在钙钛矿的八面体位置上存在Cr(III),在钙钛矿的八面体位置上存在Cr(IV),在石榴石的八面体位置和四面体位置上都存在Cr(IV)。使用助熔剂混合物有利于钙钛矿相,证实了紫外可见结果,并且在传统的高温热处理中更为明显。研究了共沉淀法以提高纳米级颗粒的反应性;然而,这种反应性有利于在两种类型的助熔剂中出现更多不需要的石榴石相。扫描电子显微镜(SEM)显微照片提供了通过传统方法合成的颜料中尺寸在1µm到2µm之间的主要立方晶相的二次电子信息,以及通过共沉淀合成的颜料中尺寸小于1µm的玻璃相。研究了微波热处理方法,在较低的温度和较短的合成时间内获得了以钙钛矿和石榴石为主要结构的颜料。采用基于CIEL*a*b*体系的紫外-可见分光光度计对多孔单烧陶瓷釉的色坐标进行了采集,研究了其在多孔单烧陶瓷釉中的应用可行性。
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