BITS PILANI K.

K BIRLA GOA CAMPUS

PREPARATION OF GRAPHENE
FINAL REPORT
J Lakshmi Saradhi Reddy
2012A1PS426G

Submitted in partial fulfillment of Lab Project (Jan 2015-May 2015)

INDEX
Serial Topic
No.

Page No.

1.

Introduction :Graphene

2.

Properties of Graphene

3.

Graphene and its Applications in various

fields

4.

Existing methods for preparation of Graphene

5.

Hummers Method

Bibliography

12

GRAPHENE
In simple terms, graphene, is a thin layer of pure carbon; it is a single, tightly
packed layer of carbon atoms that are bonded together in a hexagonal honeycomb lattice. In more complex terms, it is an allotrope of carbon in the structure of a plane of sp2 bonded atoms with a molecule bond length of 0.142 nanometres. Layers of grapheme stacked on top of each other form graphite,
with an interplanar spacing of 0.335 nanometres.It is the thinnest compound
known to man at one atom thick, the lightest material known the strongest
compound discovered (between 100-300 times stronger than steel), the best
conductor of heat at room temperature and also the best conductor of electricity known Other notable properties are its unique levels of light absorption of
white light, and its potential suitability for use in spin transport. Graphene's
stability is due to its tightly packed carbon atoms and an sp2orbital hybridization a combination of orbitals s, px and py that constitute the -bond. The final pz electron makes up the -bond. The -bonds hybridize together to form
the -band and -bands. These bands are responsible for most of graphene's
notable electronic properties, via the half-filled band that permits free-moving
electrons.

Individual layer of Graphite - Graphene

Graphene layer placed on top of each other- Graphite

GRAPHENE & Its Properties

Electronic Properties
One of the most useful properties of graphene is that it is a zero-overlap semimetal (with both holes and electrons as charge carriers) with very high electrical conductivity. Carbon atoms have a total of 6 electrons; 2 in the inner
shell and 4 in the outer shell. The 4 outer shell electrons in an individual carbon atom are available for chemical bonding, but in graphene, each atom is
connected to 3 other carbon atoms on the two dimensional plane, leaving 1
electron freely available in the third dimension for electronic conduction.
These highly-mobile electrons are called pi () electrons and are located above
and below the graphene sheet. These pi orbitals overlap and help to enhance
the carbon to carbon bonds in graphene. Fundamentally, the electronic properties of graphene are dictated by the bonding and anti-bonding (the valance and
conduction bands) of these pi orbitals.
Tests have shown that the electronic mobility of graphene is very high

Mechanical Strength
Another of graphenesstand-out properties is its inherent strength. Due to the
strength of its 0.142 Nm-long carbon bonds, graphene is the strongest material
ever discovered. Not only is graphene extraordinarily strong, it is also very
light at 0.77milligrams per square metre (for comparison purposes, 1 square
metre of paper is roughly 1000 times heavier). It is often said that a single
sheet of graphene (being only 1 atom thick), sufficient in size enough to cover
a whole football field, would weigh under 1 single gram. Graphene also contains elastic properties, being able to retain its initial size after strain. In 2007,
Atomic force microscopic (AFM) tests were carried out on graphene sheets
that were suspended over silicone dioxide cavities. These tests showed that
graphene sheets (with thicknesses of between 2 and 8 Nm) had spring constants in the region of 1-5 N/m and a Youngs modulus (different to that of
three-dimensional graphite) of 0.5 TPa. Again, these superlative figures are

based on theoretical prospects using graphene that is unflawed containing no

imperfections whatsoever and currently very expensive and difficult to artificially reproduce, though production techniques are steadily improving, ultimately reducing costs and complexity.

Thermal conductivity
Thermal transport in graphene is an active area of research, which has attracted attention because of the potential for thermal management applications.
Early measurements of the thermal conductivity of suspended graphene reported an exceptionally large thermal conductivity of approximately
5,300 Wm1K1, compared with the thermal conductivity of pyrolyticgraphite of approximately 2,000 Wm1K1 at room but measured range of
thermal conductivities between 1,500 2,500 Wm1K1 for suspended single layer graphene.Potential for this high conductivity can be seen by considering graphite, a 3D version of graphene that has basal planethermal conductivity of over a 1000 Wm1K1 (comparable to diamond). In graphite, the
c-axis (out of plane) thermal conductivity is over a factor of ~100 smaller due
to the weak binding forces between basal planes as well as the larger lattice
spacing. In addition, the ballistic thermal conductance of graphene is shown to
give the lower limit of the ballistic thermal conductances, per unit circumference, length of carbon nanotubes.

Chemical
Graphene is the only form of carbon (or solid material) in which every atom is
available for chemical reaction from two sides (due to the 2D structure).
Atoms at the edges of a graphene sheet have special chemical reactivity. Graphene has the highest ratio of edge atoms of any allotrope. Defects within a
sheet increase its chemical reactivity. The onset temperature of reaction between the basal plane of single-layer graphene and oxygen gas is below
260 C. Graphene burns at very low temperature (e.g., 350 C ).Graphene is
commonly modified with oxygen- and nitrogen-containing functional groups
and analyzed by infrared spectroscopy and X-ray photoelectron spectroscopy.

Optical Properties
Graphene's unique optical properties produce an unexpectedly high opacity for
an atomic monolayer in vacuum

Uses Of Graphene in various fields

Graphene is used in areas including electronics, biological engineering, filtration, lightweight/strong composite materials, photovoltaics and energy storage.
Graphene is often produced as a powder and as a dispersion in a polymer matrix. This dispersion is supposedly suitable for advanced composites,paints and
coatings, lubricants, oils and functional fluids, capacitors and batteries, thermal management applications, display materials and packaging, inks and 3Dprinters materials, and barriers and films.
ELECTRONIC NANODEVICES
Field Effect Transistors
Transparent conductive films
ENERGY STORAGE DEVICES
Li- ion batteries
Ultra capacitors
Fuel cell and solar cells

SENSORS
Electrochemical Sensors
Biosensors
BIOMEDICAL ENGINEERING
Gene Delivery

Drug Delivery
Tissue Engineering
Cancer Therapy

Preparation Methods

Reduction of graphite oxide

Shearing
Solvent/surfactant-aided
Epitaxy
Silicon carbide
Solar Exfoliation
Liquid Phase Exfoliation
Microwave Assisted Oxidation
Electro Chemical Method

The method we followed in lab is chemical reduction of Graphite oxide prepared via Hummers method. Graphene oxide produced was chemically reduced used a reducing agent like Hydrazine Hydrate or Sodium Borohydride
to obtain Graphene.

We used Sodium Borohydride for reduction because it is relatively less hazardous and harmful to use when compared to Hydrazine Hydrate

Hummers Method
For Hummers method, the following chemicals required:
1. 2.5 grams graphite
2. 1.25 grams of sodium nitrate
3. Concentrate sulphuric acid

4.
5.
6.
7.

7.5grams of potassium permanganate

30% H2O2 solution (2.5 ml)
Hydrazine hydrate/ Sodium Borohydride(NABH4) - 2 grams
Ice bath and distilled water

Apparatus Required

2 500ml beaker
4 100ml beaker
1 litre beaker
spatula
stirrer rod

Preparation of Graphene oxide

1. 2.5 g of graphite powder and 1.25 g of sodium nitrate were mixed in a
beaker.
2. Concentrated sulfuric acid (165 ml) was added to the mixture and uniformly stirred in an ice bath (0 C).
3. While maintaining vigorous stirring, 7.5 g of potassium permanganate
was slowly added at a carefully controlled rate to keep the temperature
below 20 C.
4. The suspension was then stirred for 2 h in an ice bath.
5. After heating the solution at 35 C and stirring it for 30 min, 75 ml of distilled water was slowly added to the suspension, resulting in an exothermic reaction that heated up the suspension to 95 C.

6. Temperature was controlled at 95 C for 30 min under stirring to complete the reaction, after which the solution was diluted with 200 ml of
distilled water.
7. The solution was treated with a 30% H2O2 solution (2.5 ml) to reduce
residual permanganate into soluble manganese ions until the gas evolution ceased.
8. The cooled mixture was filtered, resulting in a yellow-brown filter cake
and then washed with a 37% HCl solution to remove residues, followed
by several washings with distilled water
Finally GO was obtained by centrifugation, and the precipitate was dried at 60
C for24 h.
The Graphene oxide obtained was dispersed in a beaker distilled water and sonicated it for 24 h.
The solution will be homogenous and add 2 g of Sodium Borohydride by heating the mixture up to 100 C for another 24 h to evaporate water.
The final solution is centrifuged to separate graphene and water , dried in an
oven at 80 C.
Weight of the graphene prepared is 1.8 g.
It is tested in die swelling characcerstics using 1 wt% polymer and got satisfactory results

10

Graphen oxide befor drying

Graphene oxide after drying

11

Graphene obtained after reduction

BIBLIOGRAPHY
1. Production methods of graphene and resulting material properties
UrszulaKosidlo, Marta Arias Ruiz de LarramendiFriedemann Tonner,
Hye Jin Park, CarstenGlanz, VieraSkakalov, Siegmar Roth, IvicaKolaric
2. Improved Synthesis of Graphene Oxide,Daniela C. Marcano, Dmitry
V. Kosynkin, Jacob M. Berlin, Alexander Sinitskii, Zhengzong Sun,
Alexander Slesarev, Lawrence B. Alemany, Wei Lu, and James M.
Tour*
3. Recent advances in applications of graphene,TapanK.Das and SmitaPrusty

4. Graphene Applications and Uses

12

Nanotechnologyhttps://www.google.co.in/search?q=Graphene+applications&biw=127
6&bih=715&source=lnms&sa=X&ei=c1JEVdhqzra5BKT6gIgL&ved=0
CAUQ_AUoAA&dpr=1#

5. Wikipedia Graphen production,http://en.wikipedia.org/wiki/Graphene#Production_techniques

6. GrapheneSythesisvs Voltage in a dry cell , scientific report, Dan

Avilla