原位晶体生长及化学反应的湿环境扫描电子显微分析

    In-situ Crystal Growth and Chemical Reaction in Wet Environment Scanning Electron Microscopy

    • 摘要: 采用环境扫描电镜(ESEM)及微操纵/微注入系统(MMI/MIS),动态观察NaCl晶体的原位溶解和结晶过程以及BiVO4晶体的原位反应.实测MMI系统的针尖在线性进退(Z-轴)、水平(X-轴)转动和垂直(Y-轴)转动3个方向的位移精度分别达到5、5和0.5 nm.MIS系统的液滴尺寸为200~300μm.通过改变样品室压力(420~850 Pa)和样品温度(-1~50℃),控制水的蒸发和凝结状态,研究水湿环境对晶体的溶解、生长及生长速率的影响.采用2个MMI/MIS系统,通过液体微注入方式,在700 Pa和4℃下分别注入NH4VO3和Bi (NO3)3液滴,得到原位反应产物BiVO4八面体.

       

      Abstract: Dynamic observation of dissolving-crystallization process of NaCl crystal and in-situ reaction of BiVO4 crystal were carried out by using an environmental scanning electron microscope(ESEM) and the micro-manipulator/micro-injector system(MMI/MIS).The step precision of MMI system in three directions,retreat-forward linearity(Z-axis),clock-unclockwise rotation(X-axis) and up-down rotation(Y-axis) are 5,5 and 0.5 nm,respectively.The size of the liquid droplet of MIS system was about 200 μm-300 μm.The influences of the water wetting environment on dissolving,growth and growing rate of crystals were studied by changing pressures(450-850 Pa) in chamber and sample temperatures(0-50 ℃),as well as by controlling states of water evaporation and condensation.Reactive products of BiVO4!octahedron were obtained at 700 Pa and 4 ℃ via liquid micro-injection approach by using two MMI/MIS systems,i.e.,one for NH4VO3 and one for Bi(NO3)3 injection.

       

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