微波水热法制备单分散球形Fe-Tb共掺杂Y_(2)Zr_(2)O_(7)橘红色料

Preparation of Monodisperse Spherical Fe-Tb Co-doped Y_(2)Zr_(2)O_(7) Orange-red Pigment by Microwave Hydrothermal Method

采用微波水热法制备了一种Fe-Tb共掺杂Y_(2)Zr_(2)O_(7)橘红色料,研究了水热条件对Y_(2)Zr_(1.85)Fe_(0.15)O_(7)产物形貌的影响,以及引入Tb后对Fe在Y_(2)Zr_(2)O_(7)中掺杂上限的影响。结果表明:以尿素作为沉淀剂有利于提高Y_(2)Zr_(1.85)Fe_(0.15)O_(7)产物的分散性,且在正丙醇和水以3:1体积比为混合溶剂的条件下,得到了粒径1μm~2μm的单分散球形产物。此外,在尿素与阳离子摩尔比达到100时,产物粒径减小至1μm以下,异形产物不再生成。非晶态水热产物在1100℃下经3小时热处理后高度晶化,产物的单分散球状形貌仍能保持。Fe在Y_(2)Zr_(2-x)Fe_(x)O_(7)产物中的掺杂上限为0.15,Tb的引入能够提高掺杂上限。当Tb的引入量为0.25时,掺杂上限提升至0.35,对应的产物化学式为Y_(1.75)Tb_(0.25)Zr_(1.65)Fe_(0.35)O_(7)。该产物与无色透明熔剂混合经热处理后表现出橘红色调,L^(*)值、a^(*)值及b^(*)值分别为61、31及29。

Fe-Tb co-doped Y_(2)Zr_(2)O_(7) orange-red pigment was prepared by using a microwave hydrothermal method.The effects of hydrothermal circumstance on morphology of the Y_(2)Zr_(1.85)Fe_(0.15)O_(7) powders and the effects of Tb on the upper doping limit of Fe in Y_(2)Zr_(2)O_(7) were studied.It is found that the introduction of urea as precipitating agent had a positive effect on dispersibility of the Y_(2)Zr_(1.85)Fe_(0.15)O_(7) powders.Monodisperse spherical samples with particle sizes of 1~2μm were synthesized in the mixed solvent of n-propanol and water with a volume ratio of 3:1.In addition,when the molar ratio of urea to cation reached 100,the particle size decreased to less than 1μm and the samples with irregular morphology were no longer generated.The amorphous hydrothermal samples were highly crystallized after heat treatment at 1100℃ for 3 h and the monodisperse spherical morphology could be well retained.The upper limit of Fe in Y_(2)Zr_(2-x)Fe_(x)O_(7) is 0.15,which increased with the introduction of Tb.It is further increased to 0.35 when the content of Tb is increased to 0.25,corresponding to Y_(1.75)Tb_(0.25)Zr_(1.65)Fe_(0.35)_(O7).The Y_(1.75)Tb_(0.25)Zr_(1.65)Fe_(0.35)O_(7) was then mixed with a colorless transparent flux,which showed orange-red tone after heat treatment,with L^(*),a^(*) and b^(*) values to be 61,31 and 29,respectively.