Christopher Ingold Laboratories, Department of Chemistry, University College London, 20 Gordon Street, London WC1H 0AJ, UK.
Philos Trans A Math Phys Eng Sci. 2010 Sep 28;368(1927):4331-49. doi: 10.1098/rsta.2010.0135.
High-throughput continuous hydrothermal flow synthesis has been used as a rapid and efficient synthetic route to produce a range of crystalline nanopowders in the Ce-Zn oxide binary system. High-resolution powder X-ray diffraction data were obtained for both as-prepared and heat-treated (850 degrees C for 10 h in air) samples using the new robotic beamline I11, located at Diamond Light Source. The influence of the sample composition on the crystal structure and on the optical and physical properties was studied. All the nanomaterials were characterized using Raman spectroscopy, UV-visible spectrophotometry, Brunauer-Emmett-Teller surface area and elemental analysis (via energy-dispersive X-ray spectroscopy). Initially, for 'as-prepared' Ce(1-x)Zn(x)O(y), a phase-pure cerium oxide (fluorite) structure was obtained for nominal values of x=0.1 and 0.2. Biphasic mixtures were obtained for nominal values of x in the range of 0.3-0.9 (inclusive). High-resolution transmission electron microscopy images revealed that the phase-pure nano-CeO(2) (x=0) consisted of ca 3.7 nm well-defined nanoparticles. The nanomaterials produced herein generally had high surface areas (greater than 150 m(2) g(-1)) and possessed combinations of particle properties (e.g. bandgap, crystallinity, size, etc.) that were unobtainable or difficult to achieve by other more conventional synthetic methods.
高通量连续水热流合成已被用作一种快速有效的合成方法，用于在 Ce-Zn 氧化物二元体系中产生一系列晶态纳米粉末。使用位于英国钻石光源的新机器人光束线 I11，对未经处理和热处理（在空气中 850°C 下处理 10 小时）的样品进行了高分辨率粉末 X 射线衍射数据采集。研究了样品组成对晶体结构以及光学和物理性质的影响。所有纳米材料均采用拉曼光谱、紫外-可见分光光度法、Brunauer-Emmett-Teller 比表面积和元素分析（通过能量色散 X 射线光谱法）进行了表征。最初，对于“未经处理”的 Ce(1-x)Zn(x)O(y)，对于名义值 x=0.1 和 0.2 的 CeO2（萤石）结构获得了单相混合物。对于名义值 x 在 0.3-0.9（包括）范围内的混合物，获得了两相混合物。高分辨率透射电子显微镜图像显示，单相纳米 CeO2（x=0）由约 3.7nm 定义明确的纳米颗粒组成。本文所制备的纳米材料通常具有高比表面积（大于 150m2g-1），并具有难以通过其他更常规的合成方法获得或难以实现的颗粒性质（例如带隙、结晶度、尺寸等）的组合。
