Letter to the Editor
Synthesis and characterization of carbon fiber/silica
aerogel nanocomposites
Ślosarczyk Agnieszka
a,
⁎, Strauchmann Wojciech
a
, Ziółkowski Piotr
a
, Jakubowska Paulina
b
a
Poznan University of Technology, Institute of Structural Engineering, Poland
b
Poznan University of Technology, Institute of Chemical Technology, Poland
abstract article info
Article history:
Received 5 January 2015
Received in revised form 13 February 2015
Accepted 15 February 2015
Available online xxxx
Keywords:
Silica aerogel;
Sol–gel synthesis;
Carbon fibers;
Chemical modification
Nanoporous silica aerogel–carbon fiber composites were prepared via a sol–gel process by surface modification at
ambient pressure. Oxidizing modification of the carbon microfibers improved the adhesion between hydrophilic
silica gel and the carbon material surface. Suggested solution contributed to the blocking of hydroxide bonds of silica
gel via reaction with the oxidized carbon material surface, which lowered the contraction of gel volume during its
drying in atmospheric pressure and led to the more stable structure.
© 2015 Elsevier B.V. All rights reserved.
1. Introduction
Receiving good structural parameters of aerogel does not improve
the main drawback of silica aerogels, which is their brittleness. One of
the ways to improve the aerogel brittleness is the use of fibers. Never-
theless, there are very few articles on the synthesis of nanocomposites
as silica aerogel-fibers. First research on this subject was conducted in
1990's [1]. Paramenter and Milstein modified silica aerogel with silica
fibers, alumina fibers and aluminaborosilicate fibers. Those fibers are
characterized by a relatively high mass density, which significantly
changes the density of the created nanocomposites. Research proved
that applied fibers considerably limited the contraction of silica aerogel,
but they lowered its mechanical parameters, such as compressive
strength and elastic modulus. Much better parameters were achieved
by Meador and co-workers while modifying silica aerogel with much
lighter carbon nanofibers and di-isocyanate [2]. In the case of this solu-
tion an improvement of compressive strength by 5% was achieved.
However, Zhang and co-workers were the first to apply polypropylene
fibers as silica aerogel component [3]. They used polypropylene fibers
12 mm long obtaining good structural properties of silica aerogel with-
out significant changes in its density. A drawback of hitherto solutions
for this type of modification was the lack of fiber surface modification
and lack of chemical bonding between fibers and silica gel.
The main aim of presented studies was to form the silica aerogel–
carbon fiber nanocomposites with more durable structure. The syn-
thesis of aerogel and its composites with carbon fibers was performed
in two-step sol–gel process using the drying in atmospheric pressure.
The chemical modification of carbon fibers in nitric acid was carried
out to enhance the adhesion between carbon fibers and silica aerogel
skeleton. In addition, the chemical modification of aerogel nanocom-
posites in TMCS/n-hexane mixture was performed. The structure and
temperature stability of silica aerogel–carbon fiber composites were
tested through the following methods: BET analysis, thermogravimetric
measurements TGA and Fourier Transform Infrared Spectroscopy FTIR.
2. Materials and methods
As the precursor of silica aerogel synthesis the tetramethylsilane
TMOS (Sigma-Aldrich) in methanol solution (CHEMPUR) was used.
The catalyst of reaction was the aqueous solution of ammonium with
the concentration of 29–30% (Sigma-Aldrich). The chemical modi-
fication of silica aerogel was performed using the trimethylchlorosilane
TMCS (Sigma-Aldrich) and n-hexane (CHEMPUR). As component of
silica aerogel–carbon fiber composites, low-modulus carbon fibers from
coal-tar pitch with density of 1.64 g/cm
3
were used (OsakaGas Corp.).
Carbon fibers have the diameter of 13 μm and length of 700 μm, and are
characterized by shape factor of L/d = 50. They have a low graphitization
level and small specific surface area 0.96 m
2
/g (according the BET meth-
od) with very small micropore content (0.0009 cm
3
/g).
The physical and chemical characterization of synthesized nano-
materials was performed by the using of BET and thermo-gravimetric
analysis. Surface area and pore volume of aerogel composites were esti-
mated based on adsorption isotherms in low-temperature nitrogen sorp-
tion in the temperature of 77 K using the equation of BET isotherm and
analyzer ASAP 2010 (Micrometrics). Thermo-gravimetric analysis of
Journal of Non-Crystalline Solids 416 (2015) 1–3
⁎ Corresponding author at: Piotrowo 5 str., 60–965 Poznan, Poland.
E-mail address: agnieszka.slosarczyk@put.poznan.pl (Ś. Agnieszka).
http://dx.doi.org/10.1016/j.jnoncrysol.2015.02.013
0022-3093/© 2015 Elsevier B.V. All rights reserved.
Contents lists available at ScienceDirect
Journal of Non-Crystalline Solids
journal homepage: www.elsevier.com/ locate/ jnoncrysol
LETTER TO THE EDITOR