Carbon 40 (2002) 2413–2422 Preparation, characterization and pyrolysis of poly(furfuryl alcohol) / porous silica glass nanocomposites: novel route to carbon template * Aldo J.G. Zarbin , Roberto Bertholdo, Maria A.F.C. Oliveira ´ ´ Departamento de Quımica, Universidade Federal do Parana ( UFPR), C.P . 19081, CEP 81531-990 Curitiba PR, Brazil Received 18 January 2002; accepted 8 April 2002 Abstract In this paper we report the preparation of glassy carbon through the pyrolysis of poly(furfuryl alcohol) inside the pores of Vycor glass, which was used as a template. Different routes to the in situ polymerization of furfuryl alcohol inside the pores of Vycor glass were developed. The nanocomposites glass/polymer obtained were characterized by several techniques. Carbonization of these nanocomposites produces new silica glass / carbon nanocomposites, which were characterized and treated with HF to remove the silica fraction. It was found that the resulting carbon presents low crystallinity when compared to graphite. However, it presents more order than the glassy carbon resulting from the pyrolysis of the free poly(furfuryl alcohol) resin. 2002 Elsevier Science Ltd. All rights reserved. Keywords: A. Carbon composites; Pyrolitic carbon; Carbon precursor; B. Pyrolysis 1. Introduction Kyotani and co-workers have developed a template technique for synthesizing novel carbon materials based on In the last decade, several efforts have been made by the carbonization of an organic polymer in several inor- chemists to obtain materials in nanometric dimensions. ganic host materials [17–23]. The general procedure There are numerous chemical methods to prepare nanoma- consists of introducing a monomer (such as acrylonitrile or terials. One of them is the so-called ‘template synthesis’, furfuryl alcohol) into the inorganic matrix, followed by its which entails the synthesis of the desired materials within polymerization and subsequent carbonization. The re- the channels, layers or cavity spaces of nanoporous host sulting matrix / carbon nanocomposite is washed with HF structures [1,2]. Martin et al. have used the template solution to dissolve the inorganic matrix and the carbon method to prepare electronically conductive polymers [3], template is obtained as the insoluble fraction. At the metals [4] and semiconductors [5], using ‘track-etch’ moment, the template technique for novel carbon materials membranes as host matrix. A large class of nanomaterials has been carried out using a combination of different have been prepared by several research groups, using precursors and inorganic hosts [17–26]. different nanoporous host matrices as templates, including Many different organic polymers have been used as layered materials [6,7], zeolites [8–10] and porous glasses carbonaceous precursor, including poly(acrylonitrile) [27], [11–13]. The utilization of inorganic host matrices to poly( p-phenylene vinylene) [28], polyimides [29], poly- obtain nanomaterials produces new unique nanocomposites vinyl acetate [23], poly(furfuryl alcohol) (PFA) [27], etc. [14–16], which present potentially interesting properties of Among then, PFA is a common typical thermosetting resin their own, not possible from each individual component that forms carbon with a fairly high yield on carbonization separately [14–16]. [31–33]. PFA can easily be formed from its monomer liquid (furfuryl alcohol, FA) in which acid is added as a catalyst for polymerization. The carbonization reactions of *Corresponding author. Tel.: 155-41-361-3297; fax: 155-41- PFA and the properties of the carbon materials derived 361-3186. E-mail address: aldo@quimica.ufpr.br (A.J.G. Zarbin). from it have been investigated a great deal for several 0008-6223 / 02 / $ – see front matter 2002 Elsevier Science Ltd. All rights reserved. PII: S0008-6223(02)00130-6