Hollow porous carbon microspheres obtained by the pyrolysis of TiO2/poly(furfuryl alcohol) composite precursors

Hollow porous carbon microspheres obtained by the pyrolysis of TiO2/poly(furfuryl alcohol) composite precursors
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DOI:
10.1016/j.carbon.2006.06.002
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发表时间:
2006-11
期刊:
影响因子:
10.9
通讯作者:
Cláudio de Almeida Filho;A. Zarbin
Cláudio de Almeida Filho;A. Zarbin
中科院分区:
材料科学2区
文献类型:
--
作者:
Cláudio de Almeida Filho;A. Zarbin

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以溶胶-凝胶法制备的TiO 2/聚糠醇复合材料为原料,通过热解制备了高孔隙率的无序碳材料。以四异丙氧基钛(TTIP)和糠醇(FA)为前驱体制备了复合材料。我们的复合材料进行了两种不同的合成程序,基于添加糠醇(FA)之前或之后的二氧化钛纳米粒子形成。此外,还测试了不同的TTIP/FA比率。通过两种合成路线获得的杂化材料在氩气流下在900°C下热解,产生新型TiO 2/碳复合材料。采用XRD、FT-IR、DR-FTIR、拉曼光谱和TEM对样品进行了表征。结果表明,FA在TiO 2纳米粒子上发生了有效的聚合,聚合物在热解后转化为无序碳,同时发生了TiO 2锐钛矿-金红石相转变。将所得的TiO 2/碳复合材料用HF溶液处理,目的是溶解氧化物,产生作为不溶性部分的极其多孔的碳材料。这些多孔碳材料的形态在很大程度上取决于复合材料前体所采用的合成路线,从碳泡沫到高度有序的中空微球。
Disordered carbon materials with high porosity were prepared through the pyrolysis of TiO2/poly(furfuryl alcohol) composites, obtained by the sol–gel method. The composites were prepared starting from titanium tetra-isopropoxide (TTIP) and furfuryl alcohol (FA) as precursors. Two different synthetic procedures for our composites were carried out, based on the addition of furfuryl alcohol (FA) before or after the TiO2nanoparticles formation. Also, different TTIP/FA ratio was tested. The hybrid materials obtained by both synthetic routes were pyrolyzed, under argon flow, at 900°C producing novel TiO2/carbon composites. All samples were characterized by XRD, FT-IR, DR-FTIR, Raman spectroscopy and TEM. Results indicated the effective FA polymerization on TiO2(anatase) nanoparticles, and polymer conversion to disordered carbon after the pyrolysis, simultaneously with TiO2anatase–rutile phase transition. The resulting TiO2/carbon composites were treated with HF solution aiming the oxide dissolution, yielding an extremely porous carbon material as insoluble fraction. The morphology of these porous carbon materials is strongly dependent on the synthetic route adopted for the composite precursor, varying from carbon foam to highly ordered hollow microspheres.