Effect of additives on microstructure of coal-based graphite
YU Zhaoyi;XIE Weining;QIU Tian;LU Qichang;JIANG Haidi;HE Yaqun
以太西无烟煤为原料,分别加入不同质量的二氧化硅、二氧化钛、氧化铁为添加剂,采用高温石墨化处理制备煤基石墨。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、激光共焦拉曼光谱仪(RAMAN)、全自动比表面积和孔径分析仪(BET)等手段表征煤基石墨微观结构。研究表明经2800 ℃高温热处理后,所得煤基石墨的石墨化度均超过89%,显著改善了无烟煤无序的微晶结构,实现了煤中sp2杂化碳原子有序化重排;在相同的添加剂混入水平下,以二氧化钛为添加剂的煤基石墨的石墨化程度、堆砌高度相对较高,层间距与理想石墨层间距差异最小,碳材料有序度越高;拉曼光谱显示不同添加剂作用下煤基石墨的有序度差异明显,并同步受添加剂用量影响,各添加剂中TXSC3、TXTC2和TXIC3煤基石墨的有序度最高;扫描电镜下发现在3种添加剂条件下,可分别制备出鳞片状,球形以及2种形貌兼具的煤基石墨;各煤基石墨的比表面积和孔径分布数据显示具有相似的低温氮气吸附−脱附等温线。
The Taixi anthracite was used as the raw materials, and mixed with different masses of additives, namely silicon oxide, titanium oxide, and iron oxide, to prepare the coal-based graphite by high temperature graphitization. The microstructure of coal-based graphite was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser confocal Raman spectroscopy (Raman) and Specific surface area and porosity analyzer.The results show that the graphitization degree of the coal-based graphite can reach over 89% after high temperature heat treatment at 2800 °C , which significantly improves the microcrystalline structure of anthracite and achieves orderly rearrangement of sp2 hybrid carbon atoms in the coal. Under the same additive mixing level, the graphitization degree and stacking height of coal-based graphite with titanium dioxide as additive are relatively high, the difference between the layer spacing and the ideal graphite layer spacing is the smallest, and the degree of ordering of carbon materials is the highest. The Raman spectroscopy results showed that the order degree of coal -based graphite prepared under different additives was significantly different, and the order degree of TXSC3, TXTC2 and TXIC3 coal-based graphite was the highest among the additives. Under the electron microscope, it is found that under the conditions of three additives, the scales, spherical and two shapes of coal-based graphite can be prepared separately. It can be seen from the specific surface area and pore size distribution data of coal-based graphite that they have similar low-temperature nitrogen adsorption-desorption isotherms.
Taixi anthracite;high temperature graphitization;silica oxide;titanium oxide;iron oxide;coal-based graphite
主办单位:煤炭科学研究总院有限公司 中国煤炭学会学术期刊工作委员会