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Effects of Solvents on Synthesis and Dispersion of Zircon Powder via Non-hydrolytic Sol-gel Route

机译:溶剂对非水解溶胶-凝胶法合成和分散锆石粉的影响

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Zircon nano-powder has been synthesized via the non-hydrolytic sol-gel route, using industral zirconium tetrachloride (ZrCl_4) and tetraethoxysilane (TEOS) as precursors, lithium fluoride (LiF) as mineralizer, PEG 1000 as dispersant. The effects of solvents on the synthesis and dispersion of zircon nano-powder were investigated by means of XRD and TEM. The results indicate that the aprotic solvent N, N-dimethyl formamide (DMF) is not conducive to the nucleophilic substitution reaction, which directly affect the zircon synthesis, and the particles are easy to agglomerate due to the large surface tension; the powder with size of 30nm and good dispersion can be obtained using dichloromethane (CH_2Cl_2) as solvent; different anhydrous alcohols as solvents influence zircon synthesis, the order of the yield is listed as EtOH>propanol (PrOH)>isopropanol (Pr~iOH). Powder particles are larger than 50nm with wide distribution and serious agglomeration when taking PrOH and Pr'OH as solvents. Nano-zircon with good dispersion and yield up to 94.5% can be obtained via using ethanol as solvent.
机译:锆石纳米粉已通过非水解溶胶-凝胶路线合成,使用工业四氯化锆(ZrCl_4)和四乙氧基硅烷(TEOS)作为前体,氟化锂(LiF)作为矿化剂,PEG 1000作为分散剂。通过XRD和TEM研究了溶剂对锆石纳米粉体合成和分散的影响。结果表明,非质子传递溶剂N,N-二甲基甲酰胺(DMF)不利于亲核取代反应,直接影响锆石的合成,且由于表面张力大而易于团聚。以二氯甲烷(CH_2Cl_2)为溶剂,可制得粒径为30nm,分散性好的粉末。不同的无水醇作为溶剂影响锆石的合成,其收率顺序为:EtOH>丙醇(PrOH)>异丙醇(Pr〜iOH)。当以PrOH和Pr'OH为溶剂时,粉末颗粒大于50nm,分布宽,结块严重。以乙醇为溶剂,可以得到分散性好,产率高达94.5%的纳米锆石。

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