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    反应体系pH对化学液相还原制备铂粉分散性的影响

    Effect of pH Value of Reaction System on Dispersibility of Pt Powder by Chemical Liquid Phase Reduction

    • 摘要: 将等体积的铂质量浓度为10 g·L−1的Na2PtCl6前驱体溶液滴加入质量分数1%的N2H4·H2O溶液中,通过NaOH溶液和HCl溶液控制反应体系pH(2.5~10),采用化学液相还原法制备铂粉,研究了铂粉的微观形貌、粒径分布和分散性随pH的变化规律。结果表明:控制反应体系pH为10时,铂粉颗粒粒径小,颗粒团聚呈絮状,粒径分布宽,累积分布占比90%的粒径D90与累积分布占比10%的粒径D10之差为4.48 μm;随着pH降低,铂粉粒径变大,颗粒分散性提高,粒径分布变窄;当pH为6~7时,铂粉粒径基本不变,分散性良好,粒径分布变宽;随着pH的继续降低,粒径变小,颗粒分散性降低,小颗粒团聚程度加剧,粒径分布变宽。当反应体系pH为8时,铂颗粒的分散性最佳,D90D10之差仅为2.29 μm。随着pH的降低,铂粉的衍射峰强度明显减弱,半高宽变大,在碱性体系中制备的铂粉晶粒尺寸较大,而在酸性体系中晶粒尺寸较小。

       

      Abstract: Na2PtCl6 solution with platinum mass concentration of 10 g·L−1 was dropped into N2H4·H2O solution with 1% mass fraction with an equal volume. The pH value of the reaction system (2.5–10) was controlled by NaOH solution and HCl solution. Pt powder was prepared by the chemical liquid phase reduction method. The variation laws of the micromorphology, particle size distribution and dispersibility of Pt powder with pH value were studied. The results show that when the pH value of the reaction system was controlled at 10, the Pt powder particles were small and aggregated in a flocculent form, and had wide particle size distribution; the difference between the particle size with a cumulative distribution ratio of 90% (D90) and that with a cumulative distribution ratio of 10% (D10) was 4.48 μm. With increasing pH value, the particle size of Pt powder increased, the dispersibility of the particles was improved, and the particle size distribution was narrated. When the pH value was 6 to 7, the particle size of Pt powder remained basically unchanged, the particle dispersibility was good, and the particle size distribution became wider. As the pH value continued to decrease, the particle size and the dispersibility of the particles decreased, the degree of agglomeration of small particles was intensified, and the particle size distribution was broadened. When the pH value of the reaction system was 8, the dispersibility of Pt particles was the best, with D90D10 being only 2.29 μm. With decreasing pH value, the diffraction peak intensity of the prepared Pt powder was significantly weakened, and the half-peak width increased. The grain size of the Pt powder prepared in the alkaline system was relatively large, while that prepared in the acidic system was relatively small.

       

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