用SBA-15合成介孔氮化碳及浸渍法问题？文献出处: Adv Mater, 2009, 21, 4270.Young-Si Jun, Won Hi Hong, Markus Antonietti, and Arne Thomas, Mesoporous, 2D Hexagonal Carbon Nitride and Titanium Nitride/Carbon Composites隶属材料学牛人马普所Markus Antonietti的文章。实验部分有如下步骤：Synthesis of 2D Hexagonal C3N4: In a typical synthesis, 1.0 g of SBA-15 was impregnated in 1.0 g of a water solution containing 0.29 g (7 mmol) of cyanamide (Aldrich) and stirred for 1 h. The resultant mixture was then centrifuged, dried in air, and finally calcined under nitrogen for 4 h at a heating rate of 2.3 °C min-1.In order to remove the silica template, the resulting bright-yellow powder was treated with 4 M NH4HF2 (Aldrich) for 24 h, followed by filtration, washing with water and ethanol several times, and drying at 50 °C.其中的SBA-15晶化温度为80-100 °C。问题来了，当这1g的 氰胺 水溶液滴到1gSBA-15上，部分SBA-15压根没有润湿，还是蓬松的固体。有点像拿了一点点水倒在很多沙子上一样。结果可好，人家将这 混合物 还经过离心，离心的目的就是分离固液啊，这SBA-15和氰胺水溶液的composite纵然放个半天还是比较干燥的 白色粉 末，咋离心啊？最后，人家使用这一步得到了p6m反相的的介孔氮化碳，居然小角XRD和HR-TEM都不错。在Angew 2010, 49, 9706上该课题组，使用介孔KIT-6做模板，又是将这1g的氰胺水溶液滴到1gKIT-6上，经过搅拌、离心...最后得到Ia-3d反向的介孔氮化碳。朋友愚笨，请各位高手指点下，这种干燥的粉末如何个搅拌，离心？我们做了好几次，SBA-15压根没有形成流质，最后脱模板后，得到的小角XRD和HR-TEM一塌糊涂。查看更多7个回答 . 10人已关注
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