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從含鈦電爐熔分渣制備納米結構六鈦酸鉀晶須

Preparation of potassium titanate nanowhiskers from electric furnace molten slag with titanium

  • 摘要: 研究了一種通過水熱堿法-酸液回流-煅燒,從含鈦電爐熔分渣中分離提取、制備納米結構六鈦酸鉀晶須材料的新方法.采用掃描電子顯微鏡、透射電子顯微鏡、X射線衍射、X射線熒光光譜等表征手段,詳細探討了煅燒過程中鈦鉀摩爾比、煅燒溫度、保溫時間和水浸對最終產物物相和微觀形貌的影響.含鈦電爐熔分渣在水熱溫度為200℃,水熱反應時間為24 h,堿液濃度達12 mol·L-1時,經酸液回流后所得偏鈦酸呈一維單晶納米棒狀結構.隨著鈦鉀摩爾比從1.50增加至1.75,煅燒溫度從800℃升高到1100℃,保溫時間從0.5h延長至7h,制備得到的六鈦酸鉀晶須的純度、結晶性及長徑比逐漸提高.當鈦鉀摩爾比為1.75,煅燒溫度為1100℃,保溫5 h,水浸2 h后可制備得到尺寸均一的六鈦酸鉀納米晶須.

     

    Abstract: Potassium titanate (K2Ti6O13) nanowhiskers were successfully prepared from electric furnace molten slag with titanium by a hydrothermal method with alkaline solution, then refluxing in an acid medium and finally calcination. The effects of titanium-to-potassium mole ratio, calcination temperature, reaction time and water immersion on the crystal phase and morphology of as-prepared products during the calcination process were investigated in detail by scanning electron microscopy, transmission electron microscopy, X-ray diffraction and X-ray fluorescence. It is found that one-dimensional single crystalline metatitanic acid nanorods with uniform size are obtained when the hydrothermal reaction is controlled at about 200℃ for 24 h in a 12 mol·L-1 potassium hydroxide solution. The purity, the crystallinity degree and the aspect ratio of formed potassium titanate whiskers are improved with increasing titanium-to-potassium mole ratio from 1.50 to 1.75, calcination temperature from 800 to 1100℃, and reaction time from 0.5 to 7 h. The optimum conditions for preparing potassium titanate nanowhiskers are the titanium-to-potassium mole ratio of 1.75, the calcination temperature of 1100℃, the reaction time of 5 h, and the water immersion time of 2 h.

     

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