Thick silica foam films through combined catalytic decomposition of
H
2
O
2
and sol–gel processes
Martin Timusk
a,b,
⁎, Agnes Kuus
b
, Kathriin Utt
b
, Triin Kangur
b
, Andris Šutka
b,c
,
Martin Järvekülg
b,d
, Maris Knite
a
a
Institute of Technical Physics, Faculty of Materials Science and Applied Chemistry, Riga Technical University, Paula Valdena 3/7, Riga, LV 1048, Latvia
b
Institute of Physics, University of Tartu, W. Ostwaldi Str. 1, 50411 Tartu, Estonia
c
Institute of Silicate Materials, Faculty of Materials Science and Applied Chemistry, Riga Technical University, Paula Valdena 3/7, Riga, LV 1048, Latvia
d
Biomaterials Research Laboratory, Riga Technical University, Paula Valdena 3/7, Riga, LV 1048, Latvia
HIGHLIGHTS
• Low-density silica foams with a previ-
ously unreported closed-cell morpholo-
gy were prepared in a novel fashion.
• H
2
O
2
-containing silica sol was spray-
coated onto MnO
2
-coated substrates,
leading to foam formation.
• Gelation of the sol occurs concurrently
with the foam formation, “freezing”
the formed structure.
• This work is a step towards a simple
route to aerogel-like silica materials
without the supercritical drying of wet
gels.
GRAPHICAL ABSTRACT
abstract article info
Article history:
Received 21 April 2016
Received in revised form 30 August 2016
Accepted 31 August 2016
Available online 1 September 2016
A novel method for the preparation of thick silica foam films is reported that combines an alkoxide-based hydro-
lytic sol–gel process and in situ catalytic decomposition of hydrogen peroxide on a catalyst-coated support. A hy-
drogen peroxide/nitric acid aqueous solution was used to carry out acid-catalysed hydrolysis of
tetramethoxysilane. Complete stability of H
2
O
2
in the resulting silica sols over extended periods (N 120 min)
was demonstrated by in situ Raman spectroscopy. The H
2
O
2
-loaded sols were sprayed on MnO
2
-coated sub-
strates, resulting in heterogeneous catalytic decomposition of H
2
O
2
and effective foaming and simultaneous
gel formation due to oxygen gas and water formation. Silica foam films with a well-defined closed-cell porosity
were annealed at 600 °C without any damage to the closed-cell porous film morphology. Up to 530 μm thick films
were prepared with macropore sizes in the range of 29–47 μm, exceptionally thin macropore wall thicknesses of
16–50 nm and a bulk density as low as 64 kg/m
3
, comparable to that of the aerogels. The lowest measured ther-
mal conductivity of the prepared foams was 0.018 ± 0.001 W/(m* K), which is also similar to silica aerogels, en-
abling the prepared foams to be used as efficient thermal insulation materials.
© 2016 Elsevier Ltd. All rights reserved.
Keywords:
Silica foam
Low-density material
Closed-cell porosity
Sol–gel
Hydrogen peroxide
Manganese dioxide
1. Introduction
Sol–gel chemistry is one of the cornerstones of material science and
nanotechnology, enabling the preparation of materials with a wide
Materials and Design 111 (2016) 80–87
⁎ Corresponding author at: Institute of Technical Physics, Faculty of Materials Science
and Applied Chemistry, Riga Technical University, Paula Valdena 3/7, Riga, LV 1048, Latvia.
E-mail address: martin.timusk@ut.ee (M. Timusk).
http://dx.doi.org/10.1016/j.matdes.2016.08.092
0264-1275/© 2016 Elsevier Ltd. All rights reserved.
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