以无水四氯化锆、正硅酸乙酯为前驱体,氟化锂为矿化剂,氯化钠(NaCl)为分散剂,采用非水解溶胶一凝胶法制备硅酸锆纳米粉体。借助XRD和TEM研究分散剂NaCl对硅酸锆纳米粉体合成及分散的影响。结果表明:周态NaCl与530℃预烧后的硅酸锆干凝胶混合,控制NaCl与四氯化锆的摩尔比为3,经700℃低温热处理可获得分散性好的硅酸锆纳米粉体;Nacl用量过少不利于粉体的分散,而用量过大则影响硅酸锆的合成;提高热处理温度有助于硅酸锆的合成,并且所形成的熔融NaCl对抑制粉体颗粒的长大与团聚有明显的效果。
Zircon nanopowder has been synthesized via a non-hydrolytic sol-gel route using ZrCl4 and Si (OC2H5)4 as precursors, lithium fluoride as a mineralizer and sodium chloride (NaCI) as a dispersing agent. The effects of NaCI on the synthesis and dispersion of zircon nanopowder were investigated by means of XRD and TEM. The results show that the zircon nanopowder with good dispersibility can be obtained by calcining the mixture of solid NaCl with xerogel at 750℃ with the precalcination temperature of the xerogel being 530℃, and the molar ratio of NaCI/ZrCl4 being 3. The excessive NaCI restrains the synthesis of zircon while the insufficient NaCI is not beneficial to the dispersion of powder. Besides, raising the heat treatment temperature is beneficial to the synthesis of zircon, and the formation of molten NaCl contributes to inhibiting the growth and agglomeration of the zircon powder.