正硅酸乙酯为碳源制备C@ZrSiO_4色料的研究  

Study on Preparation of C@ZrSiO_4 Pigment from Tetraethoxysilane as a Colorant

作　　者：张筱君[1] 陈婷[1,2] 江伟辉[1,2] 刘健敏 查剑锐 

机构地区：[1]景德镇陶瓷学院材料科学与工程学院,景德镇333001 [2]国家日用及建筑陶瓷工程技术研究中心,景德镇333001

出　　处：《人工晶体学报》2016年第4期1029-1034,1040,共7页Journal of Synthetic Crystals

基　　金：国家自然科学基金(51402135;51362014);江西省科技厅青年科学基金(20142BAB216006);江西省优秀科技创新团队建设计划项目(20133BCB24010);江西省教育厅基金(GJJ150887;GJJ150919)

摘　　要：采用正硅酸乙酯为碳源和硅源,四氯化锆为锆源,Li F为矿化剂,通过非水解溶胶-凝胶法(NHSG)制备了硅酸锆包裹炭黑(C@ZrSiO_4)色料。通过XRD和SEM研究了前驱体和矿化剂浓度对硅酸锆合成及显微形貌的影响,同时采用CIE-L~*a~*b~*色度仪考察了该色料的色度。实验结果表明,正硅酸乙酯中的乙氧基原位炭化成细小的碳粒作为发色基团,同时与氯化锆通过非水解溶胶-凝胶反应生成硅酸锆均匀包裹于炭黑颗粒表面。随着前驱体浓度的增大原位碳含量增加,C@ZrSiO_4色料黑度提高;前驱体浓度高于3 mol·L^(-1)时样品颗粒团聚严重,同时过厚的包裹层不利于色料发色。经氮气气氛900℃热处理2 h,空气气氛800℃热处理2 h后制备出的C@ZrSiO_4黑色包裹色料具有良好的色度值,L~*=44.54,a~*=0.82,b~*=2.84,施于透明基础釉中经1200℃煅烧仍能保持优异的呈色能力。Zirconium silicate coated carbon black pigment（ C@ZrSiO4） was prepared by non-hydrolytic sol-gel method（ NHSG）,using ZrCl4 as zirconium source,tetraethoxysilane（ TEOS） as colorant and silicon source,LiF as mineralizer, respectively. The effects of the concentration of precursor and mineralizer on the synthesis and morphology of samples were studied by using X-ray diffraction（ XRD）and scanning electron microscope（ SEM）,while the chromatic value of the pigments was characterized by CIE-L＊a＊b＊color system. The results show that the carbon particles can be transformed from oxethyl of TEOS,which react with zirconium chloride via NHSG process to form zircon coated on carbon simultaneously. The black deep hue of C @ZrSiO4 pigment was improved with increasing the precursor concentration due to the increase of in-situ carbon content. However,too higher to 3 mol·L^-1 caused the particles aggregation and the ZrSiO4 layer thickening,resulting in the poor chromatic performance.After calcining under nitrogen atmosphere at 900 ℃ for 2 h and then flowing air atmosphere at 800 ℃ for2 h,the as-prepared C@ZrSiO4 inclusion pigment exhibits excellent chromatic value（ L＊= 44. 54,a＊=0. 82,b＊= 2. 84）,and possesses strong tinting strength in transparent glaze at 1200 ℃.

关 键 词：黑色色料 非水解溶胶-凝胶法 硅酸锆 正硅酸乙酯 

分 类 号：TQ174[化学工程—陶瓷工业]