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Preparation of Carbon Foams and Its Surface Fuctionalization Using Nitric Acid

This document discusses the preparation and functionalization of carbon foams using nitric acid. It describes different types of carbon foams and their properties. The experimental section outlines the process of treating carbon foam with nitric acid at varying times. Characterization methods including SEM, TGA, FTIR and compressive strength testing are also presented. Key results showed that acid treatment introduced oxygen functional groups on the carbon foam surface and decreased compressive strength after long treatment times.

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Dr. Dipen Shah
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50 views

Preparation of Carbon Foams and Its Surface Fuctionalization Using Nitric Acid

This document discusses the preparation and functionalization of carbon foams using nitric acid. It describes different types of carbon foams and their properties. The experimental section outlines the process of treating carbon foam with nitric acid at varying times. Characterization methods including SEM, TGA, FTIR and compressive strength testing are also presented. Key results showed that acid treatment introduced oxygen functional groups on the carbon foam surface and decreased compressive strength after long treatment times.

Uploaded by

Dr. Dipen Shah
Copyright
© © All Rights Reserved
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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PREPARATION OF CARBON FOAMS AND ITS SURFACE

FUCTIONALIZATION USING NITRIC ACID

SATISH M. MANOCHA*, KALPESH PATEL AND L. M. MANOCHA

Department Of Materials Science


Sardar Patel University, Vallabh Vidyanagar – 388 120, India
*E-mail: [email protected]
Contents

 Introduction
 Experimental
 Characterization
 Results & discussion
 Conclusions
 References
What are Foams
 Foams are rigid, porous materials consisting of an interconnected
network of ligaments.
 These can have open cell structure where pores are interconnected to
one another forming three-dimensional (3D) cellular materials made of
interconnected solid struts, forming a network.
 The closed cell structure where pores are isolated from one another.
open-cell foams closed-cell foams

The Voronoi tessellation model


Introduction
There are several types of carbon foams, depending on the raw material
(precursor) and the manufacturing process employed to produce the foam.

Major categories of carbon foams

Partially-graphitic carbon foam Non-graphitic carbon foam

Graphitic carbon foam Reticulated vitreous


Coal based foams carbon foam (RVC)
Pitch based foams
Thermosetting resin based foam like
polyurethane, polyfurfuryl alcohol,
phenol-formaldehyde resin, etc.

Fig : Franklin models for isotropic and graphitizing carbons


Properties of carbon foam

Excellent filtration Easily machinable to Near net


capacity shape

Specific surface
area Extremely
lightweight
Permeability
Electrically conductive
Controlled
porosity

High thermal High chemical &


stability & oxidation mechanical
Variability: stability
resistance structure, density,
geometry
Applications of carbon foams involve thermal managements, electrodes, catalyst supports and
filters owning to their novel features such as adjustable thermal-conductivity and electrical
conductivity, high porosity, low thermal expansion coefficient, high-temperature tolerance, etc
Experimental
Overview of template route for making carbon foam
FUnctionalization Carbon foam

Carbon foam

At 100 °C Conc. Nitric acid

Carbon foam treated


for 0, 3, 6, 7, 8 and 9
hour
Filtered, washed
Dried at 150 °C
thoroughly with dist.
water

Functionalized Carbon foam


( Neutral pH and Nitrate ion free)

Higher etching rate after 9 hour treatment results into the decrease
in the strength of carbon foams.
Characterization

 Thermal properties by TGA (Thermo Gravimetric Analysis – TG - 50,Mettler)

 Surface morphology by SEM (Scanning Electron Microscope) (Hitachi S3000N)

 Compressive strength by UTM (Universal Testing Machine) (INSTON 5500 R)

 Gas Chromatograph (GC) (Sigma instruments Pvt. Ltd.)

 FTIR Spectrophotometer, Shimadzu 8300 FTIR


Results
&
Discussion
… PHYSICAL VIEW OF CARBON FOAM …

As such PU 150 0C 300 0C HTT


foam cured foam foam

700 0C HTT 1000 0C HTT


500 C HTT
0
foam foam
foam
Fig : Physical view of carbon foam at different
temperature
 At 1000 0C, the carbon foam produced has glassy appearance.
 It is also noticed that the sound of carbon foam when it strike with ceramic tiles
Surface morphology of carbon foam

Fig : SEM images of carbon foam (A) and (B) shows uniform distribution of porosity,
(C) single pore, (D) pore wall or pore boundary
 SEM image shows that the pore diameter varies from approximately 100
µm to 450 µm.
Physical properties of carbon foam

Weight KEROSENE
Density (g/cc) =(g) POROSITY
Volume
(cc)

Compressive
strength

2.5 X 2.5 X 2.5 cm


Density, Porosity & Compressive strength Vs Temperature

Compressive strength, MPa


% Porosity
Density, g/cc

Temperature, ºC
Gas Permeability measurement of samples using GC

: Conditions :
Injector temperature – 100 °C
Column/oven temperature – 60 °C
Detector temperature – 60 °C
Column – 13X Molecular sieves

Carbon foam (47.45 X 38.17 X 23.46 mm)


Carrier Gas – Ar
Sample Gas Blank Through sample %
N2 1737366 1722370 98.62
O2 2025081 1996705 98.57
H2 13512571 13490485 99.88
He 10443443 10403798 99.6
Carrier Gas – N2
Sample Gas Blank Through sample %
O2 2027111 1979074 97.63
Ar 19197270 19006912 98.78
H2 6063112 5994717 98.87
Water permeation
through carbon
foam
Geometry optimized structures of carbon surface models I,
II, III and IV

Functional groups like – C=O, – CHO, – OH and – COOH


FTIR analysis of Fictionalized carbon foam

 1200 cm-1 due to stretching


vibration of phenol-O group
 1384 cm-1 an increase in the
already available oxygen
functionalities
 2889, 2973, 3580, 3620 and
3684 cm-1 corresponding to four
different –OH groups
 Carbonyls peaks of lactone and
Fig: Acid treatment of carbon foam at 7 hr, 8 hr and 9 hr cyclic ketone are observed at 1784
and 1712 cm-1
 Intense peak at 1219 cm-1 is
ascribed to the C-O stretching and
–OH bending mode of phenolic
and carboxylic groups
 Intensity increase at 1085 cm-1
indicating the addition in basic
oxygen functionalities
 Peaks at 1680 and 1634 cm-1
stretching frequency of carbonyl
groups
Fig: Acid treatment of carbon foam at 0 hr (as such carbon foam), 3 hr and 6 hr
Conclusions
PROPERTIES OF CARBON FOAM

 At 1000 0C, Density = 0.12 g/cc (density can be controlled)

 Porosity = 80 % (By kerosene porosity method)

The average pore size varies between 100 to 600 μm (measured by SEM)

 The Strut thickness of about 25 to 80 μm. (measured by SEM)

 At 1000 0C, compressive strength = 0.52 Mpa


References
1. Gallego NC, Klett JW. Carbon foams for thermal management. Carbon 2003;41:1461-6.
2. Poko graphite,Inc., 1601 South State Street, Decatur. TX 76234, USA, Poco foams
datasheet.
3. G.tondi, V. Fierro, A. Pizzi, A. Celzard, Tannin-based carbon foams, carbon
2009;47:1480-92.
Open close model : Bicerano & Associates Consulting

Acknowledgement

Author wishes to thank University Grant Commission, New Delhi for their financial
support under office order no. C/Meri.Fellow/Mat.Sci./2918. Author is also thankful
to Sophisticated Instrumentation Centre for Applied Research and Testing for
providing their testing facility.

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