STOBER METHOD

AND FORMATION
OF SILICA
MESOPOROUS
PARTICLES 1
 SILICA MESOPORE PARTICLES
Main Research Areas

 Drug Delivery

Tomado de Chandrababu R., et  Energy Storage

al, RSC Advances (2015)
Tomado de EATON, et al, www.eaton.com
(2021)

 Protection and insulation Covering (Painting

& electrical areas)
Tomado de EATON, et al,
https://sps.honeywell.com (2021)

2
SOL GEL METHOD
 Sol-gel method it´s defined, as a moisture method that employs a chemical solution (sol), or
colloidal particles (nanoparticles sol), to produce a 3D integrated network (gel).

 It is a synthesis method in which by means of molecular precursors, such as metallic alkoxides

and inorganic salts, it is possible to obtain an oxide skeleton, through hydrolysis and
polymerization reactions, which allow the synthesis of metastable phases of oxides, and even
of mixed organic and inorganic solids

3
SOL GEL METHOD
 A Sol is a suspension of colloidal solid
particles in a liquid

 A gel is a solid consisting of a least two

phases, a solid phase that forms a network,
which and inmobilzes a liquid phase

Water molecules trapped in

the solute

Tomado de Jian Lui., et al, Colloidal Spheres (2011) 4

SOL GEL METHOD
Precursors 𝑅 −𝑂𝑀 +𝐻 2 𝑂 ↔ 𝑀 (𝑂𝐻 )(𝑂𝑅)

 The most commonly used precursors in the

sol gel process are metal alkoxides, which
react with water through hydrolysis and
condensation reactions .

Alkoxides
5
SOL GEL METHOD
Two routes are generally described in the
literature, depending if the precursor is an aqueous
solution of an inorganic salt, or an alkoxide
dissolved in an organic solvent.
 Pre- route: obtaining Alkoxide
 1. Hydroxylation of the precursor; Formation of
𝑅𝑂𝐻 + 𝑀𝑋 ↔ 𝑅𝑂𝑀 MOH bonds. The hydroxylation of alkoxides by
hydrolysis thanks to the addition of water
 2. Condensation after hydroxylation; is followed
 Alkoxide hydroxylation by polycondensation process, which leads to the
elimination of water molecules through
𝑅𝑂𝐻 + 𝐻 2 𝑂 ↔ 𝑅𝑂𝑀𝑂𝐻 oxolation processes (formation of oxygen
bridges).
 3. Polymerization; which is the increase in the
 Condensation
connectivity of the skeleton that is produced by
+ the condensation reactions

6
STOBER METHOD
 One of the most citated Sol-gel methods, for obtaining colloids is the Stober process (1968),
generating multiple variations, but retaining as a general principle the use of a precursor , a
silicon tetra-alkoxide (TEOS), which is primarily

7
Tomado de Qiao Zhang., et al, NanoResearh(2009)
SIO2 SYNTHESIS BY STOBER
METHOD
Characterization
DLS
POT-ZETA
TEM
IR-
SPECTROSCOPY

Tomado de Rodríguez J., et al, UASLP(2021)

8
ETCHING PROCESS Characterization
TEM
GAS
PHYSISORPTION
DLS
POT-ZETA
IR-
SPECTROSCOPY

Tomado de Rodríguez J., et al, UASLP(2021)

 Abrasive methodology to develop a pore morphology (micropore, mesopore or macropore),

by means of “Surface protection etching”

9
GRAPHENE OXIDE
ATTACHING Characterization
TEM
GAS
PHYSISORPTION
DLS
POT-ZETA

10
 SIO2 HIDRODINAMIC RADIUS &
ZETA-P (DLS)
SiO 2 Size D istribution S iO 2 Zeta P otential D istribution
20 200000

Z-A verage (d.nm ): 181.8 Zeta potential (m V ): -31.9

15 150000 Z eta deviation (m V ): 7.26
P dl: 0.128
Intensity (P ercent)

Total C ounts
100000
10

50000
5

0
0

-100 0 100 200 300 400 500 600 -150 -100 -50 0 50 100 150
11
S ize (d.nm ) Zeta Potential (m V)
 SIO2@PVP HIDRODINAMIC RADIUS
& ZETA-P (DLS)
20 SiO 2@ PV P S ize D istribution S iO 2@ P V P Zeta P otential D istribution
160000

Z-Average (d.nm ): 202.8 140000

15 Pdl: 0.304 Zeta P otential (m V): -39.9

120000
Zeta D eviation (m V ): 27.5
Intensity (Percent)

100000

Total C ounts
10 80000

60000

5 40000

20000

0
0

-20000
-100 0 100 200 300 400 500 -100 0 100

S ize (d.nm ) Zeta P otential (m V ) 12

 HM-SIO2 HIDRODINAMIC
RADIUS & ZETA-P (DLS)
hm -SiO 2 Size D istribution hm -S iO 2 Zeta P otential D istribution
180000
20
160000
Z-A verage (d.nm ): 173.4
Pdl: 0.166 140000 Zeta Potential (m V): -40.9
15 Zeta D eviation (m V ): 13.0
120000
Intensity (Percent)

Total C ounts
100000
10
80000

60000

5 40000

20000

0 0

-20000
-100 0 100 200 300 400 500 -150 -100 -50 0 50 100 150
13
Size (d.nm ) Zeta Potential (m V)
 DLS SUMMARY

PARTICLE SIZE ZETA POTENTIAL MEASURE

Standard
Particle average Standard Deviation deviation
Particle Zeta Potential (mV)
diameter (d.nm) (d.nm)
(mV)

SiO2 181.8 69.35 -31.9 7.26

SiO2@PVP 202.8 48.89 -39.9 27.5
Hm-SiO2 173.4 47.78 -40.9 13.0

14
15