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The structure of the powder was examined under an argon-gas atmosphere at room temperature via X-ray diffractometry (XRD) (Model D5000, Siemens, Karlsruhe, Germany), using CuKa radiation. The mean crystallite size of the powder was estimated from the diffraction-peak width, using the Scherrer equation.39 The microstructure of the powder was studied via transmission electron microscopy (TEM) (Model 430, Philips, Eindhoven, the Netherlands and Model 2000 FXII, JEOL, Tokyo, Japan, the latter of which was equipped with a energy-dispersive spectroscopy (EDS) system (Link Systems, High Wycombe, Buckinghamshire, U.K.)). For the TEM studies, the washed powder was dispersed in methanol using an ultrasonic bath and a drop of solution was placed on a copper grid that had been coated with holey carbon film. Simultaneous differential thermal analysis (DTA) and thermogravimetric analysis (TGA) were conducted using a thermal analysis system (Model Thermoflex, Rigaku, Tokyo, Japan) under a constant air flow of 2 cm3/min with a heating rate of 20°C/min. The specific surface area was measured via a Brunauer–Emmett- Teller (BET) nitrogen-gas absorption method at a temperature of 77 K (Model Gemini 2360, Micromeritics, Norcross, GA). The particle size was also measured via a laser light scattering (LLS) method (Model Mastersizer Microplus, Malvern Instruments, Malvern, U.K.). For the LLS measurements, powders were dispersed in deionized water with a (NaPO3)6 dispersant, using an ultrasonic probe for .15 min. A density of 7.135 g/cm3 and real and imaginary parts of the refractive index—2.3 and 0.1, respectively— were used for the LLS measurements. Inductively coupled plasma–atomic emission spectroscopy (ICP–AES) analysis was conducted at the Chemistry Centre at the University of Western Australia, to analyze the CeO2 nanopowder for traces of elementaliron, sodium, and chlorine. |
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木虫 (著名写手)
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【答案】应助回帖
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在室温并且氩气的保护下通过XRD分析粉末的结构，使用CuKa辐射的SiemensD5005X射线衍射仪。使用谢乐公式计算通过衍射峰的宽度估算粉末的平均微晶尺寸。粉末的微观结构通过配备了能谱系统的透射电子显微镜观察。为了TEM研究，洗过的粉末被使用超声浴的方法分散在甲醇中，滴一滴溶液在已经涂敷一层多孔的碳膜的铜格上。同时还进行示差热分析和热重分析，这两种分析都在一个加热速率为20℃/min，恒流速为2cm3/min的热分析系统进行。比表面积在温度77K下通过一个BET氮气吸收方法测量。通过激光散射方法来测量颗粒大小。对于激光散射测量，粉末被分散在含有(NaPO3)6去离子剂的去离子水中，使用超声探测15min。密度为7.135g/cm3，用在激光散射测量的折射率实部和虚部分别为2.3和0.1。电感耦合等离子体-原子发射光谱分析在澳大利亚西部大学的化学中心进行，分析纳米粉CeO2中的铁、钠和氯元素。 大致翻译了一下，希望有所帮助！ |
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3楼2010-05-07 18:57:18