College of Material Sciences and Engineering, Northeast Forestry University, Harbin 150040, China.
Carbohydr Res. 2011 Jun 1;346(8):999-1004. doi: 10.1016/j.carres.2011.03.020. Epub 2011 Mar 16.
Carbon spheres (CSs) with controllable sizes and rich in oxygen-containing groups were fabricated using a simple hydrothermal treatment of glucose. The effects of the hydrothermal parameters, including the concentration of glucose, reaction temperature, duration, and the second hydrothermal treatment were investigated. The obtained CSs were then activated using KOH for the eventual preparation of porous carbon spheres. A scanning electron microscope was used to characterize the morphology and size of the CSs. Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy were used to analyze the functional surface groups. N(2) adsorption–desorption isotherms were used to analyze the porous structure of the CS. The results revealed that the morphologies and size distribution of the CSs can be controlled by adjusting the experimental parameters. A hydrothermal temperature between 180 and 190°C over 4-5h was suitable for CS formation. Under these conditions, the size of the CS increased with the concentration of glucose. Mono-dispersed CSs with good morphologies and large numbers of oxygen-containing functional groups (primarily -OH and C=O) can be obtained using a 0.3mol/L glucose solution that is hydrothermally treated at 190°C for 4h. The resulting CSs sizes were about 350nm in diameter. After a second hydrothermal treatment, the sizes of CSs grew nearly 250nm without damage to its morphology or broadening of their size distribution. Porous CSs with perfectly spherical shapes and fully developed structures (S(BET)=1282.8m(2)/g, V(micro)=0.44cm(3)/g) could then be obtained via KOH activation.
采用简单的水热法，以葡萄糖为原料制备了具有可控尺寸且富含含氧基团的碳球。考察了水热参数（包括葡萄糖浓度、反应温度、时间以及二次水热处理）对产物的影响。然后，用 KOH 对所得碳球进行活化，以制备多孔碳球。利用扫描电子显微镜对碳球的形貌和尺寸进行了表征。利用傅里叶变换红外光谱和 X 射线光电子能谱对其表面官能团进行了分析。利用 N2 吸附-脱附等温线对碳球的多孔结构进行了分析。结果表明，通过调节实验参数可以控制碳球的形貌和尺寸分布。在 180-190°C 下水热 4-5h 有利于碳球的形成。在此条件下，碳球的尺寸随葡萄糖浓度的增加而增大。在 190°C 下以 0.3mol/L 葡萄糖溶液水热处理 4h 可得到形貌良好、含氧官能团（主要为-OH 和 C=O）数量较多的单分散碳球。所得碳球的直径约为 350nm。经二次水热处理后，碳球的尺寸几乎增大了 250nm，而其形貌或尺寸分布并未受到破坏。通过 KOH 活化可得到具有完美球形形貌和完全发达结构的多孔碳球（比表面积为 1282.8m2/g，微孔体积为 0.44cm3/g）。
