Sols
are
dispersions
of
colloidal
par.cles
in
a
liquid.





Colloids
are
solid
par.cles
with
diameters
of
1‐100
nm



 
 
 
 
 
 
 
 
 



A
gel
is
a
interconnected,
rigid
network
with
pores
of


submicrometer
dimensions
and
polymeric
chains
whose


average
length
is
greater
than
a
micrometer.

 Interest
in
the
sol‐gel
processing
of
inorganic
ceramic
and
glass
materials
began
as
early
as
the
mid‐1800s
with

Ebelmanl,
and
Graham’s
studies
on
silica
gels.
These
early
inves.gators
observed
that
the
hydrolysis
of
tetraethyl

orthosilicate
(TEOS),
Si(OC2H5),
under
acidic
condi.ons
yielded
SiO2
in
the
form
of
a
"glass‐like
material”.
Fibers

could
 be
 drawn
 from
 the
 viscous
 gel,
 and
 even
 monolithic
 op.cal
 lenses
 or
 composites
 formed.
 However,

extremely
 long
 drying
 5mes
 of
 1
 year
 or
 more
 were
 necessary
 to
 avoid
 the
 silica
 gels
 fracturing
 into
 a
 fine

powder,
and
consequently
there
was
liQle
technological
interest.



…Roy
and
coworkers
recognized
the
poten.al
for
achieving
very
high
levels
of
chemical
homogeneity
in
colloidal
gels

and
used
the
sol‐gel
method
in
the
1950
and
1960s
to
synthesize
a
large
number
of
novel
ceramic
oxide
composi.ons,

involving
AI,
Si,
Ti,
Zr,
etc.,
that
could
not
be
made
using
tradi.onal
ceramic
powder
methods.
During
the
same
period

Iler's
 pioneering
 work
 in
 silica
 chemistry
 led
 to
 the
 commercial
 development
 of
 colloidal
 silica
 powders,
 Du
 Pont's

colloidal
 Ludox
 spheres.
 Stober
 et
 al.
 extended
 Iler's
 findings
 to
 show
 that
 using
 ammonia
 as
 a
 catalyst
 for
 the
 TEOS

hydrolysis
reac.on
could
control
both
the
morphology
and
size
of
the
powders,
yielding
the
so‐called
Stober
spherical

silica
powder.


The
final
size
of
the
spherical
silica
powder
is
a
func.on
of
the
ini.al
concentra.on
of
water
and
ammonia,
the
type
of

silicon
 alkoxide
 (methyl,
 ethyl,
 pentyl,
 esters,
 and
 alcohol
 (methyl,
 ethyl,
 butyl,
 pentyl)
 mixture
 used,
 and
 reactant

temperature.


 Precursor

Solu/ons

Sol‐Gel

Hydrolysis,
polimeriza.on

Sol
 Technologies

Coa.ng


Xerogel
film

Extrac.on
of


Wet
Gel

solvent


Furnace

Xerogel

Heat


Heat


Dense
film
 Aerogel
 Dense

 Uniform

 Ceramic



Ceramics
 par.cles
 fibres

 Main
step
of


THE
SOL‐GEL
ROUTE

1

Solu.on
of
precuros:

alkoxide,
salts,
complexes

solvent,
addi.ves


2

Gel

porous
and
amorphous
solid


3

Final
product

amorphous,
nanocrystalline,
crystalline


Hydrolysis
 Densifica/on


1
 2
 3

Condensa/on

 Hydrolysis
and
condensa.on
of
Silicon
Compound


Genera.on
of
reac.ve
species:
hydrolysis
 ‐ 
Kind
of
catalyst
(pH)

‐ 
Kind
of
molecular
precursor

‐ 
Water:OR
ra.o

‐ 
Solvent

‐ 
Temperature

‐ 
Addi.ves
(e.g.
electrolytes,







Network
forma.on:
condensa.on
 surfactants,
complexing
agent)

‐ Precursor
concentra.on

‐ Rela.ve
concentre.on
of
the

precursors
in
mul.‐component

systems

 Influence
of
the
catalyst


Acidic
condi.ons


Alkaline
condi.ons

(similar
F‐)


Hydrolysis
reac.ons: 
X=R 
Y=H


Condensa.on
reac.ons: 
X=R
or
H; 
Y=





Si


Alcohol
exchange: 
 
X=R,
 
Y=R’


pH
dependence
of
hydrolysis
and
condensa.on



OR

Si
RO

OR
RO

H 2O Hydrolisis
and
condensa5on

Condensa.on


c a t.

occur
concomitantly!


OR

Hydrolisis
 RO
RO
Si
OH

OH OR OR OH OR

Si Si Si Si Si
RO RO OR RO OR
OH O O
RO RO OR RO OR

OR OR OR OR
OH OR OR

Si Si Si Si Si
Si Si RO OR
HO

RO OR RO OR

OH O O
HO O OR OR O OR
RO OR O

Si Si Si
RO RO OR
OH O
RO OR

RO

OH

Si
HO OR

OH
HO OR

RO

RO Si

OH
OR
Si
O

O
O Si HO
RO

Si RO O OR

Si OR RO
RO
O OR O
RO Si Si
RO OR

OR

O RO
O OR Si

Si O
RO

OH RO
RO Si
OR
RO O OR

Si

RO

O RO R
 Influence
of
the
Subs.tuents


Steric
and
electronic
influence
of
–OR
groups:


Reac.on
Rate 
Si(OMe)4
>
Si(OEt)4
>
Si(OnPr)4
>
Si(OiPr)4 



Electron
density
@
Silicon 



Acid
catalysis: 
reac.on
rates
decrease
from
lel
to
right


Base
catalysys: 
reac.on
rates
increase
from
lel
to
right 


 Acidity
of
Si‐OH
groups


Lowest

Higest

 pH
and
Network
Structure


Alkaline
condi.ons



 
















 
X=R
or
H; 

Y=





Si


Nucleofil
aQack
@the
most
condensed
Si
atoms

 pH
and
Network
Structure


Acidic
condi.ons


Reac5ons
@
the
least
condensed
Si
atoms

 Alkoxy
group

/
H2O
ra.o


Theore.cally



Rw
=
2

 
 
Si(OR)4 → SiO2 



Rw
=
1 
 
Si(OR)4 → Si(OH)4 without condensation

In practice:

More H2O (lower Rw) favors the formation of Si-OH over Si-O-Si (hydrolitic depolimerization)

Even with Rw > 2 only mixtures of [SiOx(OH)y(OR)z]n (2x+y+z = 4) are obtained 


Metal
Oxide‐based
systems


Si(OR)4
vs.
M(OR)n

 Reac.vity


Si(OiPr)4
<<<
Ti(OiPr)4
<
Zr(OiPr)4
<
Ce(OiPr)4


Stronger
Lewis
acid
than
silicon
alkoxides:

Hydrolysis
Ti(OR)4
ca.
100
.mes
faster
than

Nucleofilic
aQack
is
favoured

That
of
Si(OR)4

Strong
increase
of
hydrolysis
rates


i)  Catalyst
is
not
required

ii)  Modera.on
of
metal
alkoxides
reac.vity

 Strong
metal‐anion
interac5on
may
influence
sol‐gel
processing


‐ 
sol‐gel
reac.ons
may
proceed
differently
when
different
salt
of

the
same
metal
are
employed


‐ Strong
coordina.on
of
the
counter‐ion
blocks
coordina.on
sites
thus


leading
to
to
a
smaller
degree
of
condensa.on


‐ The
complete
removal
of
the
counter‐ion
from
materials
may
be
difficult
or


may
require
special

post‐synthesis
procedure

 ORGANIC‐INORGANIC
HYBRID
SOL‐GEL
MATERIALS

It
is

aQrac.ve
to
combine,
for
example,
an
inorganic
glass
with
an


organic
polymer
on
a
molecular
level



It
is
equally
self‐evident
that
the
condi.ons
required
for
processing
a


glass
are
en.rely
incompa.ble
with
the
much
lower
processing


temperatures
needed
for
polymers



This
all
changed
with
the
realiza.on
in
the
1980s
that
organic


components
could
be
combined
with
inorganic
glasses
using
the
sol‐gel


process



One
of
the
first
well
known
example
of
organic‐inorganic
material
:


inorganic
pigment
or
fillers
dispersed
in
organic
component
(solvents,


surfactant,
polymers,
…)
–paint
and
polymer
industries
–op.cal
or


mechanical
proper.es
improvement

ORGANIC‐INORGANIC
HYBRID
SOL‐GEL
MATERIALS


Organic
or
bioac.ve
components
can
be
combined
in


nanomaterials
through
sol‐gel
chemistry,

thanks
to:


‐the
sol‐gel
sol
inorganic
chemistry
process


(‘chimiedouce’):
hydrolysis
and
condensa.on


reac.ons
occur
at
T<200°C



‐the
great
stability
of
the
Si‐C
bond


 Classification on the base of the nature of the chemical links

(interface) between organic and inorganic component

CLASS
I
HYBRIDS:only
weak
interac.ons
 CLASS
II
HYBRIDS:
organic
and
inorganic

are
present

between
organic
and
 part
are
linked
through
stong
chemical

inorganic
components
(H
bonds,
van
 bonds

der
Waals,
π−π
interac.ons)


Func.onal
molecule:
organic
dye
(linear

or
nonlinear
op.cal
proper.es),

complexes,
polimerizable
groups….

Rhodamine
 Rhodamine

6G
 B

 Film
by
sol‐gel


Rapid
gel
forma.on
by
film
deposi.on

Fast
evapora.on
of
the
solvent
from
a
thin
gel
layer

Xerogel

Which
material
can
be
coated?

Coa.ng
materials:

Glasses

Inorganic

Ceramics

Hybrid
inorganic‐organic

Metals

nanopar.cles

Polimers


Principal
coa.ng
techniques:


Dip
coa.ng


Spin
coa.ng


Spray
coa.ng


Flow
coa.ng

 Dip
coa.ng

Dip
coa.ng
technique:
the
substrate
is
immersed
in
a
liquid

and
then
withdrawn
at
well‐defined
speed
under
controlled


Condi.ons
(temperature;
humidity…)


dipping
 wet
layer

 solvent



forma.on
 evapora.on

 In
the
spin
coa.ng
process,
the
substrate
spins
around

an
axis
which
should
be
perpendicular
to
the
coa.ng
area


Applica.on
of
 Spreading
of

 Solvent


coa.ng
solu.on
 the
film
 evapora.on

SCHOTT AG - Color Effect Glass 07/05/09 10:13

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The main applications center on metal coatings as used in metal pretreatment, corrosion-protection
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According to Dr. Burkhard Standke of Evonik Degussa Technical Service, Dynasylan ® SIVO 121 has Protectosil® Building
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is virtually invisible. But it has extraordinarily high weathering resistance and, depending on the
concentration, is effective for up to three years."
Evonik Degussa, the global market leader in specialty chemicals, will supply the new water-based
impregnating agent initially to producers and formulators of wood preservatives and to wholesale
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woods. The new wood preservative from Degussa does not affect the expansion and contraction
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This makes it suitable also for woods without ground contact in exterior applications. Organofunctional
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insulation materials, as additives in paints and coatings, and in the electronics industry.
In addition, Protectosil ® , another product group from the Silanes Business Line, protects buildings
against graffiti and saves on the considerable cost of its removal. The Aerosil & Silanes Business Unit
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 Commercial
Isomers
Sunscreen


Core‐shell
capsule
for
carrying


SPF20
with
UV
Pearls®

func.onal
content

 Bibliography

L.
L.
Hench
and
J.
K.
West,

The
Sol‐Gel
process,
Chemical
Review,
1990,
90,
33‐72


A.
Pierre,
Introduc.on
to
Sol‐gel
Processing,

Springer
1998


N.
Hüsing
&
U.
Schubert,
Synthesis
of
Inorganic
Materials,
Wiley
VCH
(2000)


C.
J.
Brinker
&
G.
W.
Scherer


Sol‐Gel
Science:
The
Physics
and
Chemistry
of
Sol‐Gel
Processing


Academic
Press
Inc.:
San
Diego,

1990


C.
Sanchez,
B.
Julián,
P.
Belleville,
M.
Popall,
Journal
of
Materials
Chemistry,
2005,
15,
3559


G.
Kickelbick,
Hybrid
Materials:
Synthesis,
Characteriza.on
and
Applica.ons,
Wiley
VCH
(2006)