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研究了一种通过水热碱法—酸液回流—煅烧,从含钛电炉熔分渣中分离提取、制备纳米结构六钛酸钾晶须材料的新方法.采用扫描电子显微镜、透射电子显微镜、X射线衍射、X射线荧光光谱等表征手段,详细探讨了煅烧过程中钛钾摩尔比、煅烧温度、保温时间和水浸对最终产物物相和微观形貌的影响.含钛电炉熔分渣在水热温度为200℃,水热反应时间为24 h,碱液浓度达12 mol·L-1时,经酸液回流后所得偏钛酸呈一维单晶纳米棒状结构.随着钛钾摩尔比从1.50增加至1.75,煅烧温度从800℃升高到1100℃,保温时间从0.5h延长至7h,制备得到的六钛酸钾晶须的纯度、结晶性及长径比逐渐提高.当钛钾摩尔比为1.75,煅烧温度为1100℃,保温5 h,水浸2 h后可制备得到尺寸均一的六钛酸钾纳米晶须.
A new method for preparing nanostructured potassium hexatitanate whisker by hydrothermal alkali-acid reflux-calcination was studied by separating and extracting the slag from titanium-containing electric furnace. The scanning electron microscopy, transmission electron microscopy, X-ray diffraction and X-ray fluorescence spectroscopy, the effects of molar ratio of Ti and K, calcination temperature, holding time and water immersion on the phase and microstructure of the final product during calcination were discussed in detail. Hydrothermal temperature of 200 ℃, hydrothermal reaction time of 24 h, alkali concentration of 12 mol·L-1, the acid refluxed the resulting titanic acid was one-dimensional single crystal nanorods structure with the molar ratio of titanium potassium The purity, crystallinity and aspect ratio of the prepared potassium hexatitanate whisker increased gradually from 1.50 to 1.75, the calcination temperature increased from 800 ℃ to 1100 ℃, and the holding time increased from 0.5h to 7h. Potassium molar ratio of 1.75, the calcination temperature of 1100 ℃, holding 5 h, 2 h after flooding can be prepared uniform size of potassium hexatitanate nanowhiskers.