大比表面积钛黑颜料的制备和表征

本文首次通过pH值控制沉淀法制备前驱物丁二酸钛肼复盐,并进一步热分解制备大比表面积钛黑颜料-黑色钛氧化物。通过比表面积(BET)、电子能谱(EDS)、X射线光电子能谱分析(XPS)、X射线粉末衍射(XRD)、场发射扫描电子显微镜(HRSEM)、物理吸附仪、激光粒度仪和Color i5型台式分光测色仪对黑色钛氧化物进行了表征,确定了黑色钛氧化物的组成为2TiO2·Ti2O3,其表面积为53.854 4 m2·g-1。并考察了酸源、水合肼用量、酸钛比、反应时间、pH、NaOH浓度和煅烧温度等各种反应参数对黑色钛氧化物的颗粒尺寸、分布均匀性和黑色度的影响。用元素分析仪和等离子体光谱仪测定了前驱物组成,确定其组成为[Ti(C4H4O4)2]0.85·2Ti2O3·6N2H4·3H2O,并探讨了黑色钛氧化物形成机理,为新型混合价材料黑色钛氧化物的制备提供重要参考依据。

Preparation and Characterization of Black Titanium Oxides with Large Surface Area

In this paper, the precursor hydrazine titanium succinic acid was first prepared by pH value controlled precipitation method, after that, the titanium black pigment, namely, black titanium suboxides with large surface area were prepared by thermal decomposing the precursor. The black titanium suboxides were characterized by Brunauer-Emmett-Teller (BET) surface area, Energy dispersive x-ray spectrometry (EDS), X-ray Photoelectron Spectroscopy(XPS),X-ray diffraction patterns (XRD), high resolution scanning electron microscopy (HRSEM), nitrogen sorption analysis, laser particle size analyzer, and color i5 colorimeter spectrophotometer. The composition of black titanium suboxides was determined as 2TiO₂·Ti₂O₃, and its surface area is 53.854 4 m²·g^-1. The influences of acid source, the amount of hydrazine hydrate, acid/TiCl₃ ratio, reaction time, pH, NaOH concentration, the calcination temperature and various reaction parameters on the particle size, the distribution uniformity and blackness of black titanium suboxides were discussed. The composition of the precursor with its molecular formula as [Ti(C₄H₄O₄)₂]_0.85·2Ti₂O₃·6N₂H₄·3H₂O was analyzed by Elemental analyzer and plasma spectrometer. From these data, the formation mechanism of the black titanium suboxides was deduced. These provide an important basis for the preparation of novel mixed-valence material black titanium suboxides.