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摘要
利用阳离子取代法制备阳离子掺杂的石墨相氮化碳样品,将共晶熔盐[m(KCl)∶m(NaCl)∶m(LiCl)=1∶1∶1]和三聚氰胺按照质量比10∶1的比例悬蒸干燥,同时加入氯化锰溶液使得锰元素的掺杂质量分数分别为0%、0.3%、0.5%、0.7%和1%,在温度520℃锻烧4 h后得到多种元素掺杂的纳米管材料,之后将样品酸处理3 h,去掉Na+、K+、Li+离子,最后将样品放入马弗炉中400℃煅烧2 h,可以去除Cl+和H+得到只有锰掺杂的氮化碳材料。该制备方法解决了传统离子掺杂氮化碳材料比表面积小、形貌不可控的问题。同时利用SEM、XRD、BET、UV-Vis、FT-IR和PL对阳离子取代法制备的锰离子掺杂的氮化碳纳米管的形貌和尺寸、孔结构、吸光范围和载流子分离效率等进行表征,并在可见光下对样品进行光催化产氢性能测试。
Abstract
A sequential cation-exchanging method is developed at the first time to synthesize cation doped g-C3N4.The eutectic molten salt (LiCl:KCl:NaCl=1:1:1 in weight) and melamine are firstly mixed in the ratio of 10:1 and then dissolved in the distilled water.Then different amounts of MnCl2 solution is added as a doping precursor,with concentration of manganese being 0%,0.3%,0.5% and 0.7%,respectively.After water in the solution is entirely evaporated out by a rotary evaporator,the remaining powder is put into an alumina crucible with a cover,and then heated at 520℃ for 4 h to get multi-elements doped nanotubes.The obtained nanotubes are treated with 1 M HCl solution for 3 h,which removing Na+,K+ and Li+.The powder sample is finally calcined at 400℃ for 2 h again,removing Cl+ and H+ and finally get a Mn doped g-C3N4 sample.This preparation method solves the problem that the conventional ion doped carbon nitride material has a small specific surface area and uncontrollable morphology.The morphology,phase structure,pore structure,light absorption and carrier separation efficiency of the obtained samples are detected by SEM,XRD,BET,UV-Vis,FT-IR and PL.The photocatalytic hydrogen production performances of samples are evaluated under visible light.
关键词
石墨相氮化碳
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光催化产氢
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共晶熔融盐
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质子化
Key words
g-C3N4
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photocatalytic hydrogen production
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eutectic molten salt
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protonation
Author summay
闫潇潇(1993-),女,硕士研究生,主要从事光电功能材料的研究,yxx1234321@163.com
阳离子取代法制备锰离子掺杂的石墨相氮化碳材料[J].
, 2018, 38(12): 82-85,87 DOI:10.16606/j.cnki.issn0253-4320.2018.12.018