采用稻壳和酚醛树脂作为复合碳源,无水四氯化锆和正硅酸乙酯为原料,氟化锂为矿化剂,通过非水解溶胶-凝胶法制备了C@ZrSiO4黑色包裹色料。分别利用X射线衍射( XRD)和透射电子显微镜( TEM)分析了色料的晶体结构和显微形貌,同时采用CIE-L? a? b?色度仪表征了样品的色度值。实验结果表明,酚醛树脂可以同时作为碳源和稻壳的分散剂,并且酚醛树脂和稻壳作为复合碳源制备的包裹黑色色料的发色效果优于使用单一碳源(稻壳或者酚醛树脂)制备的色料。当复合碳源添加量为硅酸锆2.50wt%时(其中酚醛树脂添加量为稻壳的15wt%),经1000℃氮气气氛热处理1 h后,可以制备出呈色良好的C@ZrSiO4黑色色料,色度值L?=39.02,a?=1.14,b?=2.68。
C@ ZrSiO4 black encapsulation pigment was prepared by a nonhydrolytic sol-gel ( NHSG ) method, using the composite of rice husk and phenolic resin ( PF ) as carbon source, zirconium tetrachloride ( ZrCl4 ) and tetraethoxysilane ( TEOS ) as raw materials, lithium fluoride ( LiF ) as mineralizer, respectively. The phase composition and the morphology of the pigment were studied by means of X-ray diffraction patterns ( XRD) and transmission electron microscope ( TEM) , respectively, and the chromatic value of the pigment was investigated by CIE-L?a?b?color system. The experiment results indicate that the phenolic resin can be used as carbon resource and the dispersant for rice husk. The chromatic value of the pigment from carbon composite is lower than that of the single carbon resource, i. e. rice husk and PF. When the addition amount of PF is 15wt% and the compound colorants amount is 2. 50wt%, the C@ ZrSiO4 black pigment exhibited excellent chromatic performance after calcining under nitrogen atmosphere at 1000 ℃ for 1 h, as L?=39. 02, a?=1. 14, b?=2. 68.
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