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Summary
Aerogel has gained the interest of the researchers and industrialists in past 20 years.
Aerogels are light in weight, having very low thermal conductivity, high surface area and
high porosity. The production procedure involves gel-formation, solvent exchange and
drying. The properties of the aerogels are affected by any changes in these steps.
However, this procedure is very time-consuming and condition specific which greatly
affects the production of aerogels on a large scale. Aerogels are mostly used as thermal
insulating materials in buildings, bridges and in capacitors. However, the main
resistance for the aerogels is its high cost. They are 10 times more costly than other
insulating materials of its category. Proper safety precautions must be taken while
installing aerogels or it may cause skin and throat diseases.
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Index
Summary.....................................................................................................2
1 Introduction..........................................................................................5
2 History of Aerogels..............................................................................5
3 Characteristics and types of Aerogel.................................................7
4 Production of Aerogels........................................................................8
4.1 Gel Formation.......................................................................................................8
4.2 Solvent Exchange/ Aging Method........................................................................9
4.3 Drying.................................................................................................................10
4.3.1 Supercritical Drying......................................................................................10
4.3.2 Ambient Pressure Drying.............................................................................12
5 Experimental Procedure for Preparation for Aerogels...................12
6 Absorption and desorption properties of Aerogels:.......................13
6.1 Thermal properties of aerogel:...........................................................................13
7 Applications of Aerogels...................................................................14
7.1 Aerogels in Building Applications.......................................................................14
7.1.1 Aerogel In windows, and Roofs...................................................................14
7.2 Aerogels as Catalyst:.........................................................................................16
7.3 Fire Retardation..................................................................................................16
7.4 Aerogels as Sensors..........................................................................................17
7.5 Other Applications..............................................................................................17
8 Safety and Hazards of Aerogels.......................................................17
9 Economic Analysis and Future aspects of Aerogels......................18
Conclusion................................................................................................19
Reference Images …………………………………..…………………………
20
References................................................................................................21
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List of Figures
Figure 1 Number of Publishing per Year on aerogels (Du, Zhou, Zhang, & Shen, 2013) 6
Figure 2 The Density of different states of matter vs The Enthalpy of system (Du et al.,
2013)..................................................................................................................................7
Figure 3 The synthesis paths of Silica Aerogels by direct and two step methods (Koebel,
Rigacci, & Achard, 2012)...................................................................................................9
Figure 4 Schematic of supercritical drying autoclave (Gurav et al., 2010)....................11
Figure 5 Images of Ambient pressure Dried MTMS Based aerogels prepared at various
MeOH/MTMS molar Ratios (S): (a) S= 21, (b) S=28 and (c) S = 35...............................13
Figure 6 High Performance thermal insulation for daylighting using Aerogels (Kalwall,
2010)................................................................................................................................15
Figure 7 (a) Aerogel with a mass of only 2 grams supports a 2.5 Kg brick, (b) Flower is
protected from the fame via the superior insulating property of aerogel (Riffat & Qiu,
2013)................................................................................................................................18
List of Tables
Table 1 Properties of Silica Aerogels................................................................................8
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1 Introduction
The aerogels are the lightest of the solid materials, also called "solid smoke." Aerogels
were first time produced by Samuel Stephens Kistler in 1930. He made silica aerogels
by using gas in place of the liquid phase. Kistler also used alumina, ferric oxide, rubber,
cellulose was also used for the preparation of aerogels. However, there was not much
work done on the aerogels till 1968 when a team of researchers at Claude University
rediscovered aerogel with a more simplified procedure for the manufacturing of
aerogels. Since then, aerogels have been used in optics, waste management, for
insulation purposes, sensors, as catalysts as well as dust collectors. Silica aerogels are
the most used among the aerogel's family (Pierre, 2011).
The term aerogel is used because gels are used for their manufacturing. However, the
physical properties of aerogel differ from the gel properties such as aerogels are rigid,
have high porosity and high surface area. Aerogels provide excellent insulation and
highly resistive structure. The refractive index of aerogel is shallow (Reichenauer,
2008).
2 History of Aerogels
Kistler invented aerogel in 1930. The named aerogel was given to it because the air
successfully replaced the liquid component of the wet gel without causing any distortion
of the solid structure. The aerogel was prepared by reaction of water glass in the
presence of an acid catalyst. The chloride ions formed were then removed through
washing, followed by supercritical drying. Although the properties of the aerogel were
exciting, however, the interest in the aerogels did not start till 1970. The main reason
behind the lack of interest was due to a prolonged and time-consuming process for the
preparation of aerogels (Pajonk, 1994).
However, the aerogel took the interest of the researchers and scientists from 1970. The
water glass system used for the preparation of aerogels was replaced by organic
precursors, which significantly decreased the preparation time of aerogels (Pierre,
2011). Teichner's group in France used tetraethylorthosilicate (TMOS) and carbon
dioxide for drying the aerogels. The hydrolysis and condensation reactions became
more controllable, and a forward step was initiated for describing the reaction
mechanism for the formation of aerogels. Two international conferences on aerogels
were held in 1985 and later in 1988. The aerogels were the main topic of discussion in
both the conferences, which promoted the idea of development and preparation of
aerogels on a larger scale (Riffat & Qiu, 2013).
During the 1990s, carbon and organic aerogels were prepared along with surface
modified drying techniques. During this period, considerable efforts were made for
studying the applications as well as the industrialization of aerogels. This made
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aerogels a competitive material both in terms of cost and properties (Smirnova &
Gurikov, 2018). The 21st century has seen a massive upsurge in aerogels. In this period,
different oxide aerogels are prepared using inorganic salts and gelation accelerator.
CNT aerogels, single-element aerogels, graphene aerogels are also prepared since
2004. The applications, properties, and commercial prospects are developed in the 21 st
century (Cuce, Cuce, Wood, & Riffat, 2014). The number of papers published on
aerogels since its invention in 1930 is shown in the figure below.
Figure 1 Number of Publishing per Year on aerogels (Du, Zhou, Zhang, & Shen, 2013)
The aerogel is supposed to fill the gap between the differences of density in liquids and
gases. Aerogel is sometimes also termed as a new state of matter, not just a material.
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Figure 2 The Density of different states of matter vs. The Enthalpy of the system (Du et al., 2013)
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4 Production of Aerogels
The aerogels are synthesized by using both organic and inorganic precursors. The
production process of aerogels is divided into three steps:
Gel-Formation
Solvent exchange
Drying
In this report, the production process of silica aerogel is considered, as it is the most
commonly used aerogel and provides the desired characteristics of the aerogels.
4.1 Gel Formation
The sol-gel process is used for preparing silica gel. The sol is prepared by using a
silica solution and catalyst. The silica solution usually used in the production of gel
formation is silicon alkoxide, tetraethoxysilane, and polyethoxydisiloxane. Potassium
silicate is also used; however, the difficulty in the purification of potassium silicate
restricts it is used. As a result of this reaction, gelation takes place. The classification
of gels depends upon the dispersion medium used in the gel processing. This
dispersion medium is a hydrogel, alcogel, and aerogel (Smith, Maskara, & Boes,
1998). This stage describes whether the gel is monolith, granules, or is in the form of
powder. The shape is given to the aerogel through molding, casting, or by pyrolysis.
The microstructure of the aerogel also arises at this stage. Therefore, the aging and
drying methods are carried out in such a way that the microstructure of the aerogel
is not destroyed (Soleimani Dorcheh & Abbasi, 2008).
The two reactions involved in the sol-gel process are hydrolysis and condensation.
Both these reactions are affected by metal alkoxide activity, pH of the solution,
solvent, the ratio of water/alkoxide, and additives used. The reaction mechanisms of
both these processes should be studied while conducting the experiments, as these
reactions provide the information of the gels being produced (Tabata et al., 2010).
For example, a soft gel is formed when an acidic solution is used for the formation of
sols. Very low density with a linear chain of silica particles is formed when the acidic
solution is used. However, as the pH is increased, i.e., the solution becomes more
essential, then the cross-linking between the polymer chains increases and results in
more branched shaped structures rather than linear structures of silica particles. The
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Figure 3 The synthesis paths of Silica Aerogels by direct and two-step methods (Koebel, Rigacci, &
Achard, 2012)
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The solvent exchange method is carried out when conducting the experiments in the
laboratory. There is no solvent exchange process to produce aerogels in the
industries. In commercial production, the solvents which directly dries when undergo
reaction are used. The aging process helps in achieving a uniform pore size
distribution by re-organizing the microstructure of the aerogels (L. W. Hrubesh,
Coronado, & Satcher, 2001). The diameter of the pores in the aerogels can be
increased or decreased by changing the solvent exchange time. It has been studied
that as the concentration of the aging solution is increased, the bulk density is
decreased whereas pore size and surface area of the aerogels are increased.
Similar properties are achieved by increasing the aging time of the aerogels.
Therefore, for producing silica glass-based transparent aerogels, the aging time
should be long enough to increase the wet gel modulus. This wet get modulus is
essential in producing monolithic aerogels (Vareda, Lamy-Mendes, & Durães, 2018).
During the solvent exchange method, the aerogel network shrinks as the solvent
evaporates. This shrinkage can be eliminated by using low-pressure solvents such
as ionic liquids. Ionic liquids provide not only very low vapor pressures but also
possess excellent solvent properties as well. It has been established that whatever
route for solvent exchange is used, the aging time demonstrates the maximum
stiffness and strength of the wet aerogels (Yokogawa & Yokoyama, 1995).
4.3 Drying
This is the third and most crucial step for the preparation of aerogels. There are two
prevalent drying methods. One is ambient pressure drying, and the other one is
supercritical drying (Baetens, Jelle, & Gustavsen, 2011).
4.3.1 Supercritical Drying
This method is first and widely used for the preparation of aerogels. The supercritical
drying is achieved at a pressure higher than the vapor pressure, and the
temperature of the aerogel is increased slowly. When the critical temperature is
reached, the liquid is transformed into a gas. The supercritical drying is usually
distinguished as:
I. High-temperature supercritical drying (HTSCD)
II. Low-temperature supercritical drying (LTSCD)
4.3.1.1 HTSCD Process
The aerogels prepared by HTSCD are of higher quality because of the hydrophobicity
and shrinkage of the aerogel is also minimum. The steps involved in the HTSCD are
(Błaszczyński, Ślosarczyk, & Morawski, 2013; Dowson, Grogan, Birks, Harrison, &
Craig, 2012):
The aged gel containing the solvent in the pores is placed inside an autoclave,
and the temperature of the autoclave is slowly increased until the critical
temperature of the solvent is reached. Usually, this temperature varies from 300
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to 600K depending upon the solvent used. Methanol is usually used as a solvent
in the preparation of silica aerogels.
In the second step of the process, the pressure of the fluid is decreased at a
constant temperature.
The autoclave is then cooled to room temperature at the ambient pressure.
4.3.1.2 LTSCD Process
The LTSCD also has the same steps as that of HTSCD. However, the difference is that
carbon dioxide is used for replacing the solvent from the gel pores. The temperature of
the autoclave is kept between 4C to 10C, and the pressure is maintained at 100 bar.
The shrinkage of the aerogel, in this case, is, therefore, not because of the evaporation
of the solvent. But due to the replacement of solvent by the liquid carbon dioxide
(Vareda et al., 2018).
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Figure 5 Images of Ambient pressure Dried MTMS Based aerogels prepared at various MeOH/MTMS
molar Ratios (S): (a) S= 21, (b) S=28 and (c) S = 35.
there will be dead ends for the transmission of thermal energy. Air is also present in the
pores of Silica, which can transport thermal energy. Infrared radiations can be
conducting the thermal energy with aerogels at higher temperatures, but at lower
temperatures, radiative transport is much low (Shukla, Pradeep, & Suneesh, 2006).
7 Applications of Aerogels
Aerogels are used in different applications, both commercially and for domestic
purposes. Some of these applications include thermal insulation in buildings, fire
retardation, as a purification agent, as a catalyst and sensors. These applications are
discussed in detail below
7.1 Aerogels in Building Applications
The aerosols can be used in roofs, facades, windows, etc. in the building applications.
Also, the aerogels are used in air purification, for sound insulation, and as fire
retardation as well.
7.1.1 Aerogel In windows, and Roofs
Although the cost of the aerogels is very high, the insulation properties of aerogels are
comparable to the traditional materials. This insulation is very much favorable in the
building industry. Efforts are being made to reduce the cost of the aerogels and develop
different types of aerogels for buildings. Aerogels are a new transparent insulating
material because of this high transmittance and thermal performance against the
sunlight as well as daylight. The monolithic aerogels and granular aerogels are being
developed for the insulation of windows and roofs in many applications. The aerogels as
thermal insulating material against daylighting are shown in the figure below.
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Figure 6 High-Performance thermal insulation for daylighting using Aerogels (Kalwall, 2010)
Aspen Aerogels Inc. has developed an aerogel called space loft, which is used as
insulating material. The thermal conductivity of space loft is 13.1 mW/(mK) at 0C. This
thermal conductivity is 2.5 times lower than other insulating materials (Baetens et al.,
2011).
Nanogel is another aerogel insulating material used for the insulation of pipes. The
thermal conductivity of Nanogel is 14 mW/(mK), while that of polyurethane is 28
mW/(mK). The nano gel efficiently fills the gaps present in the pipes. However, the
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major drawback of this material is that the performance durability is not insured by the
manufacturer (Smirnova & Gurikov, 2018)s.
7.2 Aerogels as Catalyst:
Aerogel catalysts can be obtained from the sol-gel technique, with drying it up to the
supercritical region. The catalytic application includes partial oxidation, oxidative
coupling, and hydrogenation. Mostly catalysts are binary mixed oxides aerogels. For
example, oxides of nickel, copper, lithium, and iron are associated with oxides of
aluminum, silicon, and magnesium. Pure zirconia oxides are a suitable catalyst to
produce methanol. Zirconia shows positive behavior within the formation of methanol,
as there will be a reaction between copper and zirconia (Kim & Hyun, 2003). In recent
days, the aerogel series of Silica with lanthanum and niobium were produced. The
surface area of this product was ranging between 700-800 m 2/g before the reaction
starts. These kinds of catalysts are being used in the oxidative coupling of methane.
The ratio of methane to oxygen is 3:1 at 800C temperature and atmospheric pressure.
For lanthanum-silica based aerogels, the conversion of methane was 20%, and the
selectivity was 30%. While niobium- silica-based catalyst has less selectivity of 8%
comparing the lanthanum-silica based aerogels. Catalyst based on aerogel series of
Silica with lanthanum and niobium called ternary aerogels gives an overall 40%
selectivity and 13% methane conversion. Aerogels, having a large surface area, are
being used in the solid superacid catalyst as a component (Wan, Zhang, Ma, & Zhou,
2018).
During the sol-gel step, metal is easily dispersed over the surface of aerogels, which
makes them attractive for the catalytic processes. The monodisperse distribution of
particles is also noted so that they can be easily fluidized. So, these aerogels can be
used in the large manufacturing industries, not only on a laboratory scale. By the sol-gel
process, 3-D dry structure is obtained, having all catalytic capabilities and high chemical
reactivities. Comparing many other catalysts, selectivity, and performance of the
aerogel catalysts are much higher (Lawrence W. Hrubesh, 1998).
It is being used in the Carbon dioxide conversion process. For the methane reforming
reaction, Ni-based catalysts were the cheapest among noble metal catalysts, showing
similar properties as of noble metal. However, the main challenge was, the sintering and
carbon deposition quickly deactivated Ni-based catalysts. Due to this reason, oxides of
Al, Mg, and Ca were used as a support. This method increases the stability of the
catalyst, and the dispersion of metal on the surface was significantly improved.
7.3 Fire Retardation
Silica aerogels can withstand temperature up to 1400 oC. Silica aerogels are non-
combustible in comparison to organic foams, which are highly combustible and release
harmful smoke when burnt. The excellent thermal insulation and heat resistant
characteristics of silica aerogels make them a strong candidate for halting the fire in
kitchens and places where heat is involved.
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Figure 7 (a) Aerogel with a mass of only 2 grams supports a 2.5 Kg brick, (b) Flower is protected from the
fame via the superior insulating property of aerogel (Riffat & Qiu, 2013)
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inhalation of these dust can cause some damage the human health. The potential
diseases which occur by inhalation of the dust powders are silicosis, emphysema, and
pneumoconiosis (Cuce et al., 2014). The dust from aspen aerogel can cause drying of
skin, throat, skin, and eye irritation. It can cause digestion problems if eaten in large
quantities. These problems are more prominent in people who install aerogels in
different applications (Schmidt & Schwertfeger, 1998).
Some of the safety measures that must be taken while using aerogels are as follows:
To prevent direct contact with the skin, rubber, or aluminum covers are used for
covering the aerogels.
Breath masks should be used while installing aerogels to avoid the inhalation of
the aerogels.
Gloves and protective eyewear must be used to prevent skin damage.
Allergic people should not be involved in the installation personally. This also
includes people who are not directly involved in the installation but have allergies
from dust or powders.
The installation should be completed as early as possible.
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Conclusion
Aerogel is a promising material having very low density, very low thermal conductivity,
and high porosity. It is considered one of the most widely used thermal insulation
materials in the future. However, the main hurdle for the preparation of aerogels is the
extensive time and cost of the material. These hurdles are restricting the use of
aerogels on a vast scale. Efforts are being made to produce cost-effective and low time-
consuming aerogels. The aerogels find its applications as an insulation material, fire
retardation, as a catalyst, in supercapacitors, and adsorption of heavy metals.
Moreover, the aerogels can be used in a vast environment-friendly technology and have
the potential to be a notable energy-saving material. Proper safety procedures should
be followed by the people who are involved in the installation of aerogels in different
applications. The scale-up of aerogel production to large-scale manufacturing plants will
lead to a reduction in unit cost and thus increase the competitiveness of aerogel
products with conventional materials.
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Reference Images
[1]. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5525157/
[2]. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5525157/
[3]. https://www.dora.lib4ri.ch/empa/islandora/object/empa%3A5435
[4]. https://www.hindawi.com/journals/jnm/2010/409310/
[5]. https://www.sciencedirect.com/science/article/abs/pii/S1387181106004525
[6]. https://www.kalwall.com/kalwall-products/
[7]. https://academic.oup.com/ijlct/article/8/1/1/742289
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