Fe/C复合纳米材料的制备研究  

A STUDY OF PREPARATION OF IRON-CONTAINING CARBON NANOMATERIALS

作　　者：吴卫泽[1] 朱珍平[1] 刘振宇[1] 

机构地区：[1]中国科学院山西煤炭化学研究所煤转化国家重点实验室,山西太原030001

出　　处：《新型炭材料》2002年第1期4-9,共6页New Carbon Materials

基　　金：国家自然科学基金资助项目 (5 9872 0 47)~~

摘　　要：以强酸为絮凝剂 ,将碱性溶液中的水性中间相沥青絮凝 ,从而使水性中间相沥青在酸性介质中形成炭基溶胶和凝胶。将此炭基溶胶和硝酸铁溶液混合形成复合溶胶、凝胶 ,进而采用醇水交换和超临界干燥制备出粒度为 5nm～ 2 0nm的Fe C复合纳米材料。考察了硝酸铁和水性中间相沥青的比例 ,以及热处理条件对Fe C复合纳米材料织构和结构的影响。利用透射电镜、物理吸附、ICP AES、X 射线衍射、热重等表征手段对Fe C复合纳米材料特性和热处理的变化规律进行了研究。结果表明 :通过改变炭基溶胶中硝酸铁的加入量可以制备不同铁含量的Fe C复合纳米材料 ;在惰性气氛下 ,于较低温度热处理时 ,Fe C复合纳米粉中铁是以Fe2 O3的形式存在 ,热处理温度升高 (90 0℃ )后Fe2 O3被还原为单质铁 ,且金属颗粒团聚长大 ,在高温 (130 0℃ )时 ,铁以Fe3C的形式存在 ,颗粒进一步长大且有部分炭石墨化。在还原性气氛下 ,在 30 0℃～ 5 0 0℃热处理范围内 。A carbonaceous gel in acidic media was formed from the oxidation of coal tar pitch, dissolution in alkaline solution and flocculation with HCl. Iron containing carbon nanomaterials were prepared through the carbonaceous sol gel containing iron salt association with supercritical drying. The effects of the ratio of aqua mesophase pitch to iron nitrate and heat treatment on the structures of the iron containing carbon nanomaterials were investigated using FTIR, TEM, physical adsorption, ICP AES, X ray diffraction and TG. The results indicate that Fe/C nanomaterials with different Fe contents can be prepared using this method. After HTT at 500?℃, iron in Fe/C nanomaterial exists as Fe 2O 3, after HTT at 900?℃ it is reduced to elemental iron, and after HTT at 1?300?℃, it reacts with carbon to form Fe 3C and graphitization of the carbon is observed. Under H 2 flow, Fe 2O 3 is reduced to elemental iron when the heat treatment temperature is increased to the range of 300?℃～?500?℃.

关 键 词：铁/碳复合纳米材料 制备 表征 溶胶-凝胶 水性中间相沥青 

分 类 号：TB333[一般工业技术—材料科学与工程] TB383