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Chapter - 5

Physico-chemical properties of ambiently


dried sodium silicate based aerogels
catalyzed with various acids

Physico-chemical properties of

81

Chapter - 5

Chapter - 5
Physico-chemical properties of ambiently dried sodium
silicate based aerogels catalyzed with various acids
5.1 Introduction
Generally silica aergels are produced by hydrolysis and condensation
of silicon alkoxides like TMOS or TEOS in the presence of an acidic or basic
catalyst followed by supercritical drying in an autoclave. Since, various
research groups have prepared monolithic and transparent silica aerogels
applying the same method [1-5]. However, this method of preparation of
aerogels in an autoclave is very risky and expensive. Because the drying
occurs at high temperature and pressure with evacuation of highly
flammable gases and the chemicals used are hazardous for health and
costly. Hence, for commercialization, it is necessary to produce silica
aerogels using low cost inorganic precursor and drying the gels at ambient
pressure. Therefore, for easy availability we prepared the silica aerogels
using sodium silicate precursor and dried the gels at ambient pressure. So,
in this chapter we studied the effect of various acid catalysts for the
preparation and characterization of silica aerogels.
5.2 Experimental
The schematic presentation of the silica aerogels catalyzed with
various acids is shown in fig. 5.1. Wet gels were prepared from commercial
sodium silicate precursor of specific gravity 1.05 diluted from specific gravity
of 1.39 (Na2SiO3, s-d fine chemicals, India, Na2SiO3 content 36 wt%,
Na2O:SiO2=1:3.33) using various strong and weak acids as catalysts
keeping molar ratio of Na2SiO3:H2O constant at 1:146.67. The sols were
prepared by adding acid dropwise in sodium silicate solution while stirring
and were kept for gelation at 50oC in a temperature controlled oven to form a
gel. The formed gels were aged for 3 h at 50oC to give strength to the gel
network. To study the effect of various acids, the monolithic gels were first
cut into very small pieces then exchanged with 50 ml water four times so that
the sodium salt trapped in the pores of gel will come out and once with

Physico-chemical properties of

82

Chapter - 5

methanol in 24 h respectively. The subsequent surface chemical


modification was carried out using a mixture of methanol (MeOH), hexane
(Merck, India) and trimethylchlorosilane (TMCS, Fluka, Pursis grade,
Switzerland) in volume ratio of 1:1:1 over a period of 24 h. After completion
of surface modification, the gels were exposed to ambient air for 24 h. Dry
gels obtained by ambient drying were heated at 50oC and 200oC for 1 h
each, and were taken out for characterization after cooling of oven to room
temperature as hydrophobic silica aerogels.
To obtain hydrophobic and low density silica aerogels, we prepared
the gels varying the acid catalysts like strong acids namely hydrochloric
(HCl), nitric (HNO3), sulfuric (H2SO4) acids and weak acids namely
hydrofluoric (HF), acetic (CH3COOH), formic (HCOOH), propionic (C3H6O2),
orthophosphric (H3PO4), tartaric (C4H6O6), citric (C6H8O7.H2O) acids along
with their concentrations.
20 ml of 1.05 specific gravity of
Sodium silicate + 2 ml of acid
o

Gelation at 50 C

Hydrogel
Aging for 3 h at 500C

Aged Gel
Washed with water for
0
4 times in 24 h at 50 C

Hydrogel
Exchanged with methanol
once in 24 h at 50 0C

Alcogel
Silylated with 1:1:1 volume
ratio of methanol, hexane
o
and TMCS for 24 h at 50 C

Silylated alcogel
Dried at room temperature
0
0
for 24 h and 50 C & 200 C
for 1 h each

Hydrophobic Silica Aerogel


Fig. 5.1 Preparation of silica aerogels

Physico-chemical properties of

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Chapter - 5

5.3 Method of characterizations


The density of as prepared aerogels was calculated by ratio of mass
of aerogel to its volume where mass is measured by microbalance (Dhona
100 DS, 10-5 accuracy) and volume is measured by filling the aerogel beads
in a cylinder of known volume. The volume shrinkage (%), porosity (%) and
pore volume were calculated from the formulae, which have been reported
elsewhere [6]. Thermal conductivity of aerogel was measured using C-T
meter, USA. The hydrophobicity of aerogel was tested by measuring the
contact angle using contact angle meter, rame-hart, USA. Further, it was
confirmed by observing the Fourier Transform Infrared Spectra (FTIR) of the
aerogels. The microstructural studies were carried out using Transmission
Electron Microscopy (TEM), Philips TECNAI F20 FEI. The quantity of the
sodium present in the pores of aerogels is estimated by the Atomic
Absorption spectroscopy (AA), Perkin Elmer, USA. The thermal stability of
aerogel was checked by Thermo Gravimetric-Differential Thermal analyses
(TGA-DTA). Lastly the surface area, pore volume and average pore
diameter were measured using a N2 adsorption-desorption BET surface
analyzer, Micromeritics Tristar 3000.
5.4 Results and discussion
Acid or base catalyst can influence both the hydrolysis and
condensation rates and the structure of condensed product. Hydrolysis goes
to completion when sufficient water is added. Acids serve to protonate
negatively charged groups, enhancing the reaction kinetics by producing
good leaving groups, and eliminating the requirement for proton transfer
within the transition state. Acid catalyzed condensation is directed
preferentially towards the end rather than the middles of chains, resulting in
more extended, less highly branched polymers.
A Bronsted acid is a compound that produces H+ ions in the solution.
The strength and concentration of acids play an important role in the
chemical reactions. According to Bronsted-Lowry, the strengths of acids are
given by the equilibrium constant (KA) as given below.

Physico-chemical properties of

KA =

84

[B][H+]
[A]

Chapter - 5

--- (5.1)

where [B] is the concentration of base, [H+] is the concentration of protons


and [A] is the acid concentration. Further, it is evidenced that the degree of
dissociation or hydrolysis increases with increasing the dilution means
decreasing the concentration of acid as given in the formula [7].
2
KA = cx
1-x

--- (5.2)

where x is the degree of dissociation or hydrolysis and c is the concentration


of acid. Aelion et. al observed that the rate and extent of hydrolysis reaction
was most influenced by the strength and concentration of the acid or base
catalyst [8, 9]. They found that all strong acids behaved similarly, whereas
weaker acids required longer reaction times to achieve the same extent of
reaction. Therefore, in the present chapter, we studied the physico-chemical
properties of ambiently dried sodium silicate based aerogels catalyzed with
various acids.
The reaction mechanism of acid clarifies at what extent the acid
replaces the various groups from the precursor to form the silanols. From the
following acid reaction mechanism, it is very clear that the branched
structure of sodium silicate is transferred to the silicic acid. As an example,
weak acid (HF) has been considered (Equation 5.3). Initially, the attack of
H2O on sodium silicate involves the displacement of two NaO groups via a
bimolecular nucleophilic (SN2-Si) mechanism forming the NaOH as
byproduct. In the next step, F- attacks the Si atom from back side resulting in
a pentavalent intermediate, which on further nucleophilic attack of H2O
displaces the first O atom of O-Si-O chain producing HF as byproduct. In the
third step, again F- attacks the Si atom from front side which follows the
second step to replace the second O atom of the O-Si-O chain giving the
final product as silicic acid. The byproducts NaOH formed in the beginning of
reaction get neutralized with HF regenerated during the reaction to produce
the sodium fluoride salt as final byproduct.

85

Physico-chemical properties of

Chapter - 5

Acid reaction mechanism


H+
O Na

NaO

H .OH

Si
O

O- Na

NaO

(-)

HO

Si

HO
O

H+
+

(-)

NaO-

NaO
H .OH

Si

Si

+ NaOH
O

Pentavalent inetrmediate

Sodium silicate

HO

NaO

HO

Si

OH

HO

Si

OH
O

+ NaOH
O
(-)

OH

HO

F-

Si
O

OH

(-)

F-

OH

HO
Si
H2O

Si

(-)

F-

Si
O

(-)
H2O

OH

OH

HO
Si
HO

OH

HO

OH

F
OH

OH

OH

+ HF
OH

HO

Si

OH
Si

OH

HO

HO

OH2

H2O
Si

Si

Si

OH

HO
F

F-

HO
F-

OH

HO

+ HF
OH

---(5.3)

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Physico-chemical properties of

Chapter - 5

Therefore, the general sol-gel reactions (hydrolysis and condensation)


for various acids are as follows:
Hydrolysis
Na2SiO3

H2O

Acid

Sodium silicate

Si (OH)4

---(5.4)

Sodium salt

Silicic acid

Condensation
OH

Si OH

OH

n HO Si OH + HO Si OH
OH

Si

OH

+ 2n H2O ---(5.5)

O
OH

Silica gel
Since, the formed silica gels contain the hygroscopic OH groups on their
surface which are modified with TMCS as in the following reaction.
Surface chemical modification
Si OH
O
Si

Cl Si (CH3)3
+

OH

Si O Si (CH3)3
O

Cl Si (CH3)3

Silica surface Trimethylchlorosilane

Si

+ 2HCl ---(5.6)
O Si (CH3)3

Modified silica surface

Hence, the hydrophobic silica aerogels were obtained by the replacement of


H from the surface OH groups with the inert CH3 groups.
5.4.1 Effect of strong acids
The effect of strong acids HCl, HNO3, H2SO4 and their concentration
on the physico-chemical properties of the silica aerogels have been studied
as shown in table 5.1. While preparing the sols using all the acids, the molar
ratio of Na2SiO3:H2O was kept constant at 1:146.67. An interesting fact
noted is that the gelation time of sols strongly depends on the concentration
of acid. From table 5.1 it is observed that all strong acids show same
behavior in gelation means as their concentration increased to 5M, the
gelation time decreased to 5 minutes. This may be because of the rates of
hydrolysis and condensation reactions taking place during gel formation. In

Physico-chemical properties of

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Chapter - 5

general, for a condensation process (i.e. gelation) a maximum amount of


OH- groups and minimum amount of protons are needed [5]. At low acid
concentration (<2M) both the protons and OH- groups are present in less
amount leading to very slow gelation of the sol. At higher acid concentration
(>3M), the gelation was faster due to presence of equal amount of protons
and OH- groups. The gelation of sol takes place at isoelectric point of silica.
At this point the surface charge is zero and the rate of condensation is least.
The isoelectric point of silica depends on the acid used to make gel [10].
Table 5.1 Effect of strong acids on physico-chemical properties of
the silica aerogels
Concen-

Gelation

Volume

Poro

Pore

Thermal

Contact

tration of

time

shrin-

-sity

volume

conductivity

angle

acid (M)

(min.)

kage (%)

(%)

(cc/g)

(W/m.K)

(deg.)

(a) Hydrochloric acid (HCl)


1

19,920

95

95

10.0

0.100

<90

1,470

91

85

2.9

0.150

<90

10

86

84

2.8

0.151

135

77

87

3.6

0.137

138

73

89

4.4

0.118

145

(b) Nitric acid (HNO3)


1

30,420

86

95

9.7

0.101

140

2,940

89

86

3.3

0.145

<90

90

86

88

3.8

0.146

137

81

86

3.1

0.147

134

77

88

3.9

0.125

147

(c) Sulfuric acid (H2SO4)


1

33,480

95

92

6.1

0.112

140

2,700

80

91

5.7

0.114

140

1,800

84

85

3.1

0.147

100

86

78

1.8

0.170

100

84

79

2.0

0.165

110

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Physico-chemical properties of

Chapter - 5

As the strength and concentration of acids affect the gelation, in the


same way it influences the density of the silica aerogels. All strong acids
produced only dense aerogels. Fig. 5.2 shows the effect of concentration of
acids on the density of silica aerogels. It was observed that as the
concentration of acid increased (>1M), the density of aerogel increased,
which further decreased with an increase in concentration. At lower
concentration (~1M), low density aerogels were obtained. The reason for this
may be the turbid nature of the gels due to formation of silica clusters
instead of a three dimensional network. At concentration greater than 2M,
dense aerogels were obtained because of very fast hydrolysis and
condensation reactions. Among all these three acids, H2SO4 produced low
density silica aerogels (0.160 g/cc).

Density (g/cc)

0.434
0.372
0.310
0.248
0.186

H2SO4

0.270
0.225
0.180
0.135
0.090

HNO3

0.288
0.240
0.192
0.144
0.096

HCl

Acid concentration (M)


Fig. 5.2 Effect of strong acid concentration on the density of the aerogel

Physico-chemical properties of

89

Chapter - 5

TEM micrographs of the aerogels prepared using H2SO4 are shown in


fig. 5.3. For the aerogels prepared using 5M H2SO4, the structure is denser
than that of aerogels prepared using 2M H2SO4. The weight ratio of Na/Si
estimated using AA spectroscopy in 2M H2SO4 catalyzed silica aerogel is
4.4310-3.

(a)

50 nm

(b)

50 nm

Fig. 5.3 TEM micrographs of the aerogels prepared using strong acid
(a) H2SO4 - 2M (b) H2SO4 - 5M
FTIR spectra of the silica aerogels prepared using strong acids (2M)
catalyst are shown in fig. 5.4. It is evident from fig. 5.4 that the intensity of
the peaks around 3400 and 1630 cm-1 correspond to O-H absorption band

Physico-chemical properties of

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Chapter - 5

[11] decreased in the manner HCl> HNO3> H2SO4. And the intensity of
absorption peaks at 2923 and 1450 cm-1 correspond to terminal CH3 and
peak at 845 cm-1 correspond to Si-C groups [12], increased in the manner
HCl< HNO3< H2SO4. The presence of absorption peak at 1096 cm-1
correspond to Si-O-Si is expected for the silica materials [13].

% of transmission (arbitrary unit)

c
b
a
-OH

Si-C

C-H

C-H
-OH

Si-O-Si

4000

3000

2000
1500
Wavenumber (cm-1)

1000

500

Fig. 5.4 FTIR spectra of aerogels prepared using strong acids (2M)
a) HCl, b) HNO3, c) H2SO4
5.4.2 Effect of weak acids
The effect of weak acids and their concentration on the physicochemical properties of silica aerogels have been studied as given in the table
5.2. From table 5.2 it is observed that for the acids HF, CH3COOH, HCOOH
and H3PO4, the gelation time decreased with increase in concentration
(<4M) and then remained constant. And for the acids C3H6O2, C4H6O6,
C6H8O7.H2O the gelation time first decreased with an increase in
concentration and then increased. The increase in gelation time at higher
concentration may be because of the presence of large amount of protons
and less amount of OH- groups. The lower gelation times for the weak acids
are due to the fact that the anions of weak acids are basic [5].

Physico-chemical properties of

91

Chapter - 5

Table 5.2 Effect of weak acids on physico-chemical properties of


the silica aerogels
Concen-

Gelation

Volume

Poro

Pore

Thermal

Contact

tration of

time

shrinka-

-sity

volume

conductivity

angle

acid (M)

(min.)

ge (%)

(%)

(cc/g)

(W/m.K)

(deg.)

1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
1
2
3
4

(a) Hydrofluoric acid (HF)


450
84
89
4.5
0.117
5
81
85
3.0
0.149
3
81
82
2.5
0.156
2
81
83
2.6
0.153
2
77
89
4.4
0.118
(b) Acetic acid (CH3COOH)
20,220
96
95
10.1
0.100
540
89
84
2.8
0.152
15
86
86
3.3
0.147
5
84
85
2.9
0.150
5
80
88
3.9
0.125
(c) Formic acid (HCOOH)
24,360
98
93
6.7
0.110
1,980
84
90
4.9
0.117
35
89
85
3.0
0.149
5
84
86
3.1
0.147
5
77
89
4.2
0.120
(d) Propionic acid (C3H6O2)
4,140
97
96
12
0.090
135
84
88
4.0
0.122
5
82
89
4.1
0.121
2
77
89
4.2
0.121
7
55
94
7.8
0.107
(e) Orthophosphoric acid (H3PO4)
17,460
96
95
10.1
0.100
2,220
86
92
6.1
0.115
630
82
90
4.6
0.119
247
82
91
5.1
0.116
5
84
95
3.6
0.127
(f) Tartaric acid (C4H6O6)
734
77
93
7.0
0.112
2
82
95
3.7
0.127
30
50
94
8.0
0.105
85
59
92
6.3
0.115
(g) Citric acid (C6H8O7.H2O)
315
82
89
4.2
0.121
2
77
87
3.6
0.127
20
34
95
11
0.092
45
39
95
9.9
0.100

130
133
100
100
140
146
148
144
147
140
147
143
144
145
146
145
135
147
147
148
145
137
145
147
145
147
144
136
147
145
143
148
148

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Physico-chemical properties of

Chapter - 5

Figs. 5.5 and 5.6 show the effect of weak acid concentration on the
density of the silica aerogels. From fig. 5.5 it clears that for the silica
aerogels prepared using the acids HF, CH3COOH, HCOOH and C3H6O2, the
variation in the density is same as that of strong acids. But for the aerogels
prepared using the acids H3PO4, C4H6O6 and C6H8O7.H2O, the density
increased with increase in concentration, then decreased, and further
increased with concentration of acid as seen from the fig. 5.6.

Density (g/cc)

0.210
0.175
0.140
0.105
0.070

C3H6O2

0.280
0.245
0.210
0.175
0.140

HCOOH

0.312
0.260
0.208
0.156
0.104
0.350
0.315
0.280
0.245
0.210

CH3COOH

HF

Acid concentration (M)


Fig. 5.5 Effect of weak acid concentration on the density of the aerogel
Weak acids produce low density aerogels because of the systematic
formation of the network during gelation. The growth of silica particles occur
more slowly than with strong acids, forming a well connected network.
Among all the weak acids, the citric acid (3M) catalyzed silica aerogels have

Physico-chemical properties of

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Chapter - 5

low density (0.086 g/cc). These aerogels were obtained for the molar ratio of
Na2SiO3:H2O:Citric acid:TMCS at 1:146.67:0.72:9.46.

Density (g/cc)

0.252
0.210
0.168
0.126
0.084

C6H8O7.H2O

0.245
0.210
0.175
0.140
0.105

C4H6O6

0.238
0.204
0.170
0.136
0.102

H3PO4

Acid concentration (M)


Fig. 5.6 Effect of weak acid concentration on the density of the aerogel

TEM images clarify the differences between the silica aerogels


prepared using 2M and 3M citric acid as shown in fig. 5.7. The aerogels
prepared using citric acid 2M shows the dense and compact texture (fig.
5.7a) while using citric acid 3M shows the loosely connected particles to a
well tailored three dimensional network of silica. Na/Si weight ratio quantified
using AAS in the silica aerogels catalyzed with 3M citric acid is 2.2310-3.

Physico-chemical properties of

94

Chapter - 5

(a)

50 nm

(b)

50 nm

Fig. 5.7 TEM micrographs of the silica aerogels prepared using weak acid
(a) Citric-2M (b) Citric-3M
Fig. 5.8 shows the FTIR spectra of silica aerogels catalyzed with
weak acid (3M). It is observed that there is not much noticeable difference in
the intensity of the peaks around 3400 and 1630 cm-1 which correspond to
O-H absorption band [11]. But the intensity of absorption peaks at 2923 and
1450 cm-1 correspond to terminal CH3 and peak at 845 cm-1 correspond to
Si-C groups [13], increased in the manner CH3COOH<HCOOH< C3H6O2<
H3PO4<C4H6O6<C6H8O7.H2O. This indicates that the silica aerogels
catalyzed with citric acid (3M) are hydrophobic in character.

95

% of transmission (arbitrary unit)

Physico-chemical properties of

Chapter - 5

g
f
e
d
c

C-H

Si-C

-OH
C-H

a
-OH

Si-O-Si

4000

3000

2000

1500

1000

500

-1

Wavenumber (cm )
Fig. 5.8 FTIR spectra of the aerogels prepared using weak acids (3M)
a) HF, b) CH3COOH, c)HCOOH, d)C3H6O2, e)H3PO4, f)C4H6O6, g)C6H8O7.H2O
Further, the hydrophobicity is confirmed by measuring the contact
angle of water on the surface of aerogel. Fig. 5.9 illustrates the drop of water
on a hydrophobic aerogel surface catalyzed with citric acid (3M) showing
148o contact angle.

Fig. 5.9 Water drop on the aerogel surface catalyzed with citric acid (3M); =148o

96

Physico-chemical properties of

Chapter - 5

The as prepared silica aerogels have the thermal stability up to


around 420 oC as measured by the TGA-DTA as seen from the fig. 5.10.
Three major weight losses were observed in thermal analysis plot. The first
weight loss was attributed to the removal of moisture and adsorbed water
from the system. This resulted in endothermic peak in the DTA plot, centered
at the temperature of 100oC. The second weight loss was observed as an
exothermic peak at 420oC. This was attributed to the oxidation of organic
groups. The third weight loss was observed in the temperature range
between 420oC and 1000oC. This gradual and continuous weight loss was
attributed to the condensation of silanol groups. It increased rapidly between
420oC and 700oC and to a small extent above 700oC.
0.6

100

Weight (%)

420oC
98

0.4

96

0.2

94

92

- 0.2

90
0

200

400

600

800

Temperature Difference (oC/mg)

TGA
DTA

- 0.4
1000

Temperature (oC)
Fig. 5.10 TG-DT analyses of the aerogel prepared using citric acid (3M)
5.4.3 N2 adsorption-desorption of silica aerogels
Fig. 5.11 shows the N2 adsorption-desorption isotherms of the
aerogels prepared using H2SO4-2M (fig. a), 5M (fig. b) and citric acid-2M (fig.
c), 3M (fig. d). From the shape of the isotherms it can be observed that the
materials exhibited the type IV isotherms for all the four samples, which is

Physico-chemical properties of

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Chapter - 5

associated with capillary condensation taking place in mesopores, and a


limiting uptake over a range of high p/po. From figs. (a) and (c), it can be
seen that the hysteresis loop is of type H1 consisting of agglomerates of
approximately uniform spheres in fairly regular array. Also, figs. (b) and (d)
indicate the H2 type hysteresis loop consisting of pores with narrow necks
and wide bodies (ink-bottle pores) [14]. The maximum amount of the N2 gas
adsorbed by a porous solid depends on the volume of the pores present in
that material. From fig. (a), it seems that the aerogels prepared with H2SO42M adsorbed maximum amount of gas saturated at 900 cc/g corresponding
to a pressure of 750 mmHg. And the aerogels prepared with H2SO4-5M
adsorbed 750 cc/g gas at the same pressure (fig. b). As shown in figs. (c)
and (d), it can be seen that the citric acid 2M and 3M catalyzed aerogels
adsorbed almost same volume of N2 gas (1450 cc/g).

(c)

Pressure (mmHg)

(b)

Volume adsorbed (cc/g)

Volume adsorbed (cc/g)

(a)

(d)

Pressure (mmHg)

Fig. 5.11 N2 adsorption-desorption isotherms of the aerogels prepared


using H2SO4-2M (a), 5M (b) and Citric acid-2M (c), 3M (d)

Physico-chemical properties of

98

Chapter - 5

The results of fig. 5.11 are illustrated in table 5.3. It is observed that
for the silica aerogels prepared using H2SO4, the increase in the
concentration shifts the BET surface area towards maximum (458 m2/g) due
to decrease in the particle size. Further, for the aerogels prepared using
citric acid, the BET surface area increased from 448 to 719 m2/g when the
concentration of citric acid increased from 2 to 3M. The increase in the BET
surface area with decrease in the particle size can be explained on the
model proposed by Zarzycki et al. [15]. According to this model, the specific
surface area of a dry gel is related to particle and pore sizes. Assuming that
the particles are spheres having uniform size, the specific surface area has
been related to the inverse of the particle radius. Among all the strong and
weak acids, the weak acid, citric acid-3M produced low density (0.086 g/cc)
silica aerogels with large specific surface area (719 m2/g).
Table 5.3 BET surface area, pore volume and average pore diameter of
the aerogels catalyzed using H2SO4 and citric acids.
Physical Properties
BET surface area (m2/g)

H2SO4

H2SO4

2M

5M

H2O 2M

3M

458

283

448

719

C6H8O7. C6H8O7.H2O

5.5 Conclusions
Silica aerogels were obtained by catalyzing the hydrolysis and
condensation of sodium silicate with different acid catalysts varying their
concentration

followed

by

simultaneous

solvent

exchange,

surface

modification and ambient pressure drying. Strong acids requires a longer


gelation time than the weak acids. In particular, the citric acid produced low
density (0.086 g/cc) silica aerogels. These aerogels are obtained for the
molar

ratio

of

Na2SiO3:H2O:Citric

acid:TMCS

at

1:146.67:0.72:9.46

repectively. They have low thermal conductivity (0.09 W/m.K) with good
hydrophobicity (148o). TEM spectra expressed the well connected network of
silica particles with high porosity. These aerogels exhibited large specific
surface area (719 m2/g) with mesopores in their network. And these aerogels
are thermally stable up to a temperature of around 420oC.

Physico-chemical properties of

99

Chapter - 5

References
[1] S. Henning and L. Svensson, Phys. Scr., 23 (1981) 697
[2] G. Poelz and R. Riethmuller, Nucl. Instrum. Methods, 195 (1982) 491
[3] M. Prassas, J. Phalippou, and J. Zarzycki, J. Mater. Sci., 19 (1984) 1665
[4] G. M. Pajonk, A. Venkateswara Rao, P. B. Wagh, and D. Haranath,
J. Mater. Synt. and Processing, 5 (1997) 6
[5] A. Venkateswara Rao, G. M. Pajonk, N. N. Parvathy, J. Mater. Sci.,
29 (1994) 1807
[6] A. Parvathy Rao, G. M. Pajonk, A. Venkateswara Rao, J. Mater. Sci., 40
(2005) 3481
[7] R. P. Bell F. R. S., Acids and Base: Their Quantitative Behavior, Ch. 2,
p. 17
[8] R. Aelion, A. Loebel, and F. Eirich, J. Am. Chem. Soc., 72 (1950) 5705
[9] R. Aelion, A. Loebel, F. Eirich, Recueil Travaux Chimiques, 69 (1950) 61
[10] Z. Z. Vysotskii and D. N. Strazhesko, Wiley, New York, (1973)
[11] C. J. Lee, G. S. Kim, and S. H. Hyun, J. Mater. Sci., 37 [11] (2002) 2237
[12] S. S. Prakash, C. J. Brinker, and A. J. Hurd, J. Non-Cryst. Solids, 190[3]
(1995) 264
[13] F. Shi. L. J. Wang, J. X. Liu, S. H. Li, New Building Materials, 6 (2004) 9
(in Chinese)
[14] K. S. W. Sing, D. H. Everett, R. A. W. Haw, L. Moscow, R. A. Pierotti,
J. Rouquerol, T. Siemieniewska, Pure Appl. Chem., 57(4) (1985) 603
[15] J. Zarzycki, M. Prassas and J. Phalippou, J. Mater. Sci. 17 (1982) 3371

Physico-chemical properties of

100

Chapter - 5

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