J. of Supercritical Fluids 89 (2014) 28–32
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The Journal of Supercritical Fluids
j o ur na l ho me page: www.elsevier.com/locate/supflu
Hexafluoroisopropyl alcohol as a new solvent for aerogels preparation
Sergey Lermontov
a,∗
, Alena Malkova
a
, Lyudmila Yurkova
a
, Elena Straumal
a
,
Nadezhda Gubanova
b
, Alexander Baranchikov
c
, Mikhail Smirnov
d
,
Viktor Tarasov
d
, Vyacheslav Buznik
e
, Vladimir Ivanov
c,f
a
Institute of Physiologically Active Compounds of the Russian Academy of Sciences, 1 Severnij Pr., Chernogolovka, 142432, Russia
b
National Research Centre “Kurchatov Institute”, B. P. Konstantinov Petersburg Nuclear Physics Institute, Gatchina, Leningrad District, 188300, Russia
c
Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences, 31 Leninsky Av., Moscow, 119991, Russia
d
Institute of Problems of Chemical Physics of the Russian Academy of Sciences, 1 Prospect Akademika Semenova, Chernogolovka, Moscow Reg., 142432,
Russia
e
“All-Russian Scientific Research Institute of Aviation Materials”, Federal State Unitary Enterprise, State Research Center of the Russian federation, 17 Radio
Street, Moscow, 105005, Russia
f
Tomsk State University, Faculty of Chemistry, 36 Lenin Av., Tomsk, 634050, Russia
a r t i c l e i n f o
Article history:
Received 10 December 2013
Received in revised form 14 February 2014
Accepted 14 February 2014
Keywords:
Aerogels
Hexafluoroisopropyl alcohol
Supercritical drying
Silica
Alumina
Zirconia
a b s t r a c t
Fluorinated alcohols are claimed to be promising solvents for supercritical drying. A number of metal
oxide aerogels (both monoliths and powders) including silica, alumina and zirconia were prepared using
hexafluoroisopropyl alcohol. It is shown that the specific surface area of all the aerogels dried in hexaflu-
oroisopropyl alcohol is twice that of the aerogels prepared in ethanol. Surface modification of aerogels
with fluorinated organic species is shown to take place upon supercritical drying.
© 2014 Published by Elsevier B.V.
1. Introduction
Aerogels are mesoporous solid materials possessing unique
properties including very low bulk density (up to 98% of their
volume is air), large specific surface area and high thermal sta-
bility among others [1]. Since their discovery in 1931 [2], great
efforts were made to develop industrial and domestic applications
of aerogels. Nowadays they are used as reusable oil spills adsor-
bents [3], CO
2
scavengers [4,5] and water desalination materials
[6]. A very large specific surface area makes aerogels promising
catalysts and catalyst supports [7–10], energy storage materials
[11–14] and hydrogen accumulators for fuel cells [15]. Prepa-
ration of graphene–aerogels electroconducting nanocomposites
[14,16–18] presents a very promising recent area of application.
The most interesting feature of aerogels is their extremely
low thermoconductivity up to 0.004 W m
-1
K
-1
[10]. For instance,
organic aerogels are used as thermoinsulators in space explo-
ration technologies and in special clothing including sportswear
∗
Corresponding author. Tel.: +7 4965249508; fax: +7 4965249508.
E-mail addresses: lermontov52@yandex.ru, lermon@ipac.ac.ru (S. Lermontov).
[10]. Great efforts were made to develop the use of aerogels
as thermoinsulating windows since high transparency and low
thermoconductivity makes aerogels an ideal material for this appli-
cation.
Aerogels are usually prepared by a sol–gel technique using
supercritical drying (SCD) [1]. A solvent removal at a temperature
exceeding its critical temperature is a necessary stage of this proce-
dure. Thus the critical temperature of the solvent is a key parameter
which determines the overall energy consumption in course of SCD
as well as the resultant aerogels’ properties. Alcohols and carbon
dioxide (CO
2
) are the most conventional types of SCD fluids for
aerogels’ preparation [19]. SCD with CO
2
is widely used since this
compound is non-flammable and has a low critical temperature
(31
◦
C). However, SCD with CO
2
requires expensive equipment. On
the contrary, SCD in alcohol media is performed using compara-
tively low cost equipment, but alcohols are flammable substances,
having a higher critical temperature.
Little is known about the influence of the nature of supercritical
solvent on composition and structural characteristics of aerogels,
including specific surface area and porosity. Only a few publica-
tions were found concerning the comparative study of the influence
of the solvent used for supercritical drying on aerogels’ properties
http://dx.doi.org/10.1016/j.supflu.2014.02.011
0896-8446/© 2014 Published by Elsevier B.V.