氩气压力对二茂铁催化CaC_2-CHCl_3体系制备碳球的影响  

Effects of argon pressure on carbon spheres by ferrocene catalyzed CaC_2-CHCl_3 system

作　　者：尹彩流[1,2] 黄启忠[2] 王秀飞[1] 文国富[1] 刘宝容[3] 蒙洁丽[1] 潘申明[1] 黄学宁[1] 

机构地区：[1]广西民族大学物理与电子工程学院,广西南宁530006 [2]中南大学粉末冶金国家重点实验室,湖南长沙410083 [3]广西大学物理科学与工程技术学院,广西南宁530004

出　　处：《中南大学学报（自然科学版）》2010年第2期489-494,共6页Journal of Central South University:Science and Technology

基　　金：国家重点基础研究发展计划("973"计划)项目(2006CB600901);广西科学基金资助项目(桂青科0991015);广西教育厅项目(200808MS083);广西民族大学科研基金资助项目

摘　　要：以电石和氯仿为碳源和反应物，以二茂铁为催化剂，研究不同压力对CaC2-CHCl3体系制备碳球的形貌和结构的影响。反应设备是100mL的不锈钢高压釜，充入的氩气压力为0．5～1．5MPa，在350℃进行化学反应并保温3h，制备不同类型的碳球。采用X线衍射仪、扫描电子显微镜、透射电子显微镜和激光拉曼光谱仪等手段分析碳球的物相、形貌和结构。探讨空心碳结构的CHCl3雾化小液滴生长机理。研究结果表明：CaC2-CHCl3体系制备的碳球主要由无定形炭组成，随着压力增加，结晶程度增大。空心碳球的形成与体系压力相关，当充入压力为0．5MPa时，合成直径为100～260nm的实心无定形碳球，具有向菜花结构转变的趋势；当充入的氩气压力为1．0MPa时，合成4种不同空心碳结构，即空心毛绒碳球、角状空心碳棒、空心光滑碳球或碳棒和多边形化的空心碳球；当充入的氩气压力为1．5MPa时，合成3种不同直径范围的碳球，相同直径的碳球团聚在一起。With calcium carbide and chloroform as carbon sourses, and ferrocene as catalyst, the effect of different argon pressures on morphology and microstructure of carbon spheres was studied. The reaction setup is 100 mL autoclave, and 0.5-1.5 MPa of argon pressure was filled into the autoclave, respectively. Chemical reaction of CaC2-CHCl3 system was carried out at 350 ℃ for 3 h, and different types of carbon spheres were fabricated. The phase, morphology and microstructure of carbon spheres were analyzed by XRD, SEM, TEM and Raman spectrum. At last, CHCl3 atomizating small droplet growth mechanism of hollow carbon structures was supposed. The results show that carbon spheres are mainly composed of amorphous carbon, and with the increase of the argon gas pressure, the crystallization degree enhances. The formation of hollow spherical carbon depends on the system pressure. Solid and amorphous carbon spheres form under 0.5 MPa of argon pressure, and the mierostructure is cauliflower-like. Under 1.0 MPa of argon pressure, four hollow carbon structures are fabricated; including hollow fluffy carbon spheres, horn hollow carbon spheres, smooth hollow carbon spheres and polygon-like and hollow carbon spheres with internal filament structure. Carbon spheres with three different diameters are synthesized under 1.5 MPa of argon pressure, and carbon spheres with the same diameter are prone to agglomerate.

关 键 词：碳球 氩气 透射电镜 显微结构 

分 类 号：TB383[一般工业技术—材料科学与工程]