Date:22.10.

2015

MIDDLE EAST TECHNICAL UNIVERSITY

METALLURGICAL and MATERIAL ENGINEERING

MATERIALS PROCESSING LABORATORY

Sol-Gel Processing
NAME / SURNAME: Uur AYDOAN
ID:2034882
SECTION: 1
GROUP MEMBERS: Batuhan AY, Uzay Anl BLGN, Ouzhan BULUT, Bar
AKDUMAN, Fatih AKSU, smail AVCI, Glistan AKMAK
LABORATORY ASSISTANT: Ekim SARA
: Doancan TGAN

Abstract
The aim of the experiment was finding the effect of pH in sol-gel processing by using
TEOS, distilled water, ethanol, HCl and NaOH. Sol-gel processing includes hydrolysis step
and condensation step and after this steps 4 sample were gotten at different pH value.
Gelation time were observed for 4 sample.
Introduction
The name sol-gel gets from the way that small scale particles or atoms in an answer
(sols) agglomerate and under controlled conditions in the end interface together to frame a
reasonable system (gel).
Despite the fact that sol-gel is for the most part saw as a moderately new mechanical
innovation, it is utilized widely as a part of various commercial ventures, for example, rough
powder produce, optical strands, and so forth. Like every new technology, on the other hand,
the scaling-up to full mechanical misuse has been moderate.
There are two nonspecific varieties of the sol-gel method. One is known as the
colloidal system, the other is known as the polymeric (or alkoxide) course. The contrasts
between the two stem from the sorts of beginning materials (antecedents) that are utilized.
Both courses include suspending or dissolving the precursor in a suitable fluid, for the
most part water for the colloidal course and liquor for the polymeric course. The forerunner is
then actuated by the expansion of a corrosive, (for example, hydrochloric corrosive) or a base,
(for example, potassium hydroxide). The enacted forerunners then respond together to frame a
system. The system develops and ages with time and temperature until it is the extent of the
compartment. Right now the consistency of the fluid increments at an exponential rate until
gelation happens, that is, no more stream is watched.
Sol-gels can be prepared before gelation by a scope of routines including splashing to
deliver coatings and powders, attracting from a fluid to create strands and handling in a vessel
to create aerogels and stone monuments.
Utilizing sol-gel techniques, defensive coatings can be made at unassuming (under
150C) temperatures. These coatings can be customized for particular applications including:
mechanical assurance for delicate substrates, (for example, plastics and metals), concoction
insurance for receptive substrates, and natural security for uncovered surfaces. Coatings can
2

likewise be made that give a substrate further utilitarian properties; these incorporate hostile
to reflection and against ruining for glass and plastics, and UV obscurity for plastics.
A wide range of commercial enterprises could profit by receiving sol-gel in light of its
flexibility in creating an extensive variety of materials with diverse properties. Current
illustrations are found in the development, gadgets, correspondences, car and biomedical
parts.[1]

Advantageous and disadvantageous of sol-gel[2]

Advantage
1. Better homogeneity from raw materials.
2. Better purity from raw materials.
3. Lower temperature of preparation.
a. Save energy
b. Minimize evaporation loses
c. Minimize air pollution
d. No reactions with containers, thus purity
e. Bypass phase separation
f. Bypass crystallization
4. New noncrystalline solids outside the range of normal glass formation
5. New crystalline phases from special properties of gel.
6. Better glass products from properties of gel.
7. Special products such as films.
Disadvantage
1.High cost of raw materials
2.Large shrinkage during processing.
3.Residual fine pores
4.Residual hydroxyl.
5.Residual carbon.
6.Health hazards of organic solutions
7.Long processing times

Sol-gel process

Figure

1.

Sol-gel

processing

(Adapted

from

http://cheminfo.chemi.muni.cz/materials/InorgMater/sol_gel.pdf)

Figure

2.

Chemical

processing

of

sol-gel

http://cheminfo.chemi.muni.cz/materials/InorgMater/sol_gel.pdf)
4

(Adapted

from

Figure 3. Schematic diagram showing effect of relative rates of hydrolysis and condensations
reactions

on

gel

structure.

http://nptel.ac.in/courses/103103026/module2/lec7/4.html)

(Adapted

from

Figure

4.

pH

effects

of

dissolution

and

gelation

(Adapted

from

http://in.ncu.edu.tw/stchiang/ch848/related/set1/The%20Sol-gel%20Gateway
%20%20Educational%20materials.files/solgel.htm)
Procedure
Equipments
1. Laboratory Hood with adequate bench space
2. Spin Coater
3. Hot-plate
4. pH-meter and thermometer
5. Volumetric (Micropipettors) or weight-based measuring (Balance) units
Consumables
1. TEOS (Tetra ethylorthosilicate-12 mL)
2. Ethanol (24 mL) and DI-water(15mL)
3. HClaq and NaOHaq
4. Borosilicate glass beakers (20x-50 mL)
5. Magnetic bars (10x)
6. Polystyrene test tubes and tube holders
7. Parafilm
8. Volumetric measuring cylinders
1. Take 12mL TEOS, 15mL distilled water, 24mL ethanol
2. Mix TEOS, distilled water and ethanol at the same time
3. Put this mixture in the beaker and add magnetic fish and put this beaker on the hot plate
and turn the mixture effect of the magnetic field at the room temperature
4. Add 1M HCl and take sample 1 when pH reaches 1.8 pH in the tube and cover parafilm
5. Add 1M NaOH and take sample 2 when pH reaches 4.8 pH in the tube and cover parafilm
6. Add 1M NaOH and take sample 3 when pH reaches 5.9 pH in the tube and cover parafilm
7. Add 1M NaOH and take sample 4 when pH reaches 7.1 pH in the tube and cover parafilm
8. Save the sample physical and structural properties such as color and gel condition
9. 1 week later save the sample physical and structural properties and difference between the
initial and final form
Results
In this experiment mixture was blurry in beginning. When HCl added the color of the
mixture became transparent. When the mixture reached 1.8 pH the color of mixture was
transparent and this mixture gelation time was the longest one at the 1.8 pH. As a result of this
viscosity is the lowest one. After this step NaOH was added and pH of the mixture reached
4.8 pH. During the insertion process the color of the mixture turned white color and gelation
6

time slightly decrease the effect of the pH. As a result of this viscosity increased. The process
continued and when the mixture reached 5.9 pH the color of the mixture became more white.
Also, gelation time decrease the effect of the pH and viscosity increased. Finally, when the
mixture reached 7.1 pH the color of the mixture the most white one. Moreover, gelation time
decrease the effect of the pH and it was the shortest one. As a result of this viscosity was the
highest one.

Figure 5. 1.8 pH one day later

Figure 6. 1.8 pH one week later

Figure 7. 4.8 pH one day later

Figure 8. 4.8 pH one week later

Figure 9. pH 5.9 one day later

Figure 10. pH 5.9 one week later

Figure 11. pH 7.1 one week later

Discussion
Distilled water was used because of at the beginning of the experiment needed pure
density. With the addition of HCl the mixture of the color changed and transparent because of
the gelation time. If the mixture more acidic gelation time increased and the mixture became
more liquid so the mixture color was transparent. With the increase of the pH the mixtures
gelation time decrease and the mixture became more gel so the mixture color became less
transparent. When the gelation time increase the mixture more gel and viscosity increased.
The reason of the adding HCl before the adding NaOH increased the hydrolysis speed.
References
[1]

FAQ: What is sol-gel processing? (n.d.). Retrieved November 19, 2015, from
http://www.twi-global.com/technical-knowledge/faqs/process-faqs/faq-what-is-sol-gelprocessing/
[2]

Brinker, C., & Scherer, G. (n.d.). Sol-Gel Science. Retrieved November 30, 2015, from
https://books.google.com.tr/books?
id=CND1BAAAQBAJ&pg=PA839&lpg=PA839&dq=disadvantages of solgel&source=bl&ots=adwPK2UjhB&sig=wfr6zypKaiqSaizfoIUg6IFPcY&hl=tr&sa=X&ved=0ahUKEwivgrnlpbbJAhUq_HIKHUFgBowQ6AEISTAF#v=onepa
ge&q=rate of&f=false