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~20nm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Fe2O3的形式存在,热处理温度升高(900℃)后Fe2O3被还原为单质铁,且金属颗粒团聚长大,在高温(1300℃)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300℃~500℃热处理范围内,随温度的升高铁被还原为单质铁.
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