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以煤焦油沥青为碳源、纳米Fe(OH)_3为模板制备了一种三维石墨烯类多孔碳材料.通过测试氧还原性能,确定了最佳制备工艺:反应物煤沥青、纳米Fe(OH)_3、KOH的质量配比为6:8:4,热解温度为800oC.扫描电镜测试结果表明,制得的产品具有明显的孔结构且分布均匀.透射电镜测试结果进一步表明,产品具有泡沫状的多孔结构,高分辨透射电子显微镜照片表明,该产品具有多层的三维石墨烯结构.X射线衍射数据表明,在29o位置出现的衍射峰是多层石墨烯结构,42o位置的衍射峰说明产品具有一定程度的石墨化.由拉曼光谱结果计算I_G与I_(2D)的比值表明产品为多层石墨烯结构.X射线光电子能谱分析检测到的C元素含量约为88.7%,主要包含C—C键,图谱中未发现铁元素的存在,证明纳米Fe(OH)3模板已被洗净.根据比表面积测定可知,多孔碳的比表面积为2040m~2·g~(-1),孔径集中分布在10~400 nm,这与TEM测试得到的结果一致.在0.1 mol·L~(-1)KOH中进行催化氧还原性能测试,起始还原电位为0 V(vs.Hg/Hg O),电子转移数为3.58.测试结果表明,制得的三维石墨烯类多孔碳具有良好的催化氧还原性能.
A kind of three-dimensional graphene porous carbon material was prepared by using coal tar pitch as carbon source and nano-Fe (OH) 3 as template.The best preparation technology was determined by measuring the oxygen reduction performance: coal tar pitch, nano Fe (OH) ) _3, KOH mass ratio of 6: 8: 4, pyrolysis temperature of 800oC. SEM results show that the product has a clear pore structure and uniform distribution. Transmission electron microscopy test results further show that the product has a foam Shaped porous structure and high resolution transmission electron micrographs show that the product has a multilayer three-dimensional graphene structure.The X-ray diffraction data show that the diffraction peak at 29o is a multi-graphene structure, and the diffraction peak at the position of 42o shows that The product has a certain degree of graphitization. The ratio of I_G to I_ (2D) calculated by Raman spectroscopy indicates that the product is a multi-graphene structure. The content of C element detected by X-ray photoelectron spectroscopy is about 88.7% C-C bond, no iron was found in the spectrum, which proves that nano-Fe (OH) 3 template has been washed.According to the determination of specific surface area, the specific surface area of porous carbon is 2040m 2 · g -1, Aperture concentrated in the 10 ~ 400 nm, which TE M were measured.The results showed that the initial reduction potential was 0 V (vs.Hg / Hg O) and the electron transfer number was 3.58 in 0.1 mol·L -1 KOH.The results of the test It shows that the obtained three-dimensional graphene porous carbon has good catalytic oxygen reduction performance.