Proceedings of the 5th International Conference on Nanostructures (ICNS5)

6-9 March 2014, Kish Island, Iran

X-ray Diffraction: A Multifunctional method for Graphene type structure characterization

N. S. Faal nazaria, M. M. Saffaria,b* , E. Bazyara
a

X-ray Lab, KEFA Nanolaboratory complex, Tehran, 1391314631, Iran

b
X-ray Lab, Tarbiat Modares University,Tehran, Iran
*Saffari@modares.ac.ir

Abstract: Graphene has been prepared by different methods were examined by X-ray diffraction (XRD). In this work,
we try to review some abilities of XRD method for investigating of graphene type structures. Exactly structural
investigation of graphene and graphene oxide (GO) were carried out by studying interlayer d spacing. Average number
of layers, as a key parameter of graphene application, were determined by XRD method for different samples.
Crystallite size and impurity composition also indicated by XRD analysis. Finally with regard to various type of
information which this analytical method can appear from this type of material, we could introduce XRD as a
multifunctional method to graphene characterization.

Keywords: X-ray diffraction, Interlayer distance, Number of layer, Graphene, Graphen oxide.
Introduction
The discoveries of the carbon nanostructures, such as
the 0D fullerenes and their mass production, the 1D
carbon nanotubes, and 2D graphene substantially
contributed to the fast development of nanoscience. The
carbon nanostructures have emerged as likely candidates
for a wide range of applications, driving research into
novel techniques for synthesizing and charachterizing
these nanostructures [1]. But these days, it has been
extensively studied in the last several years on graphene.
Graphene is a single-layer planar sheet of sp2 bonded
carbon atoms that are packed in a two-dimensional
honeycomb lattice [1]. The fast uptake of interest in
graphene is due primarily to a number of exceptional
properties that it has been found to possess. Various
methods have been developed to produce graphene,
including mechanical [2], physical [3], and chemical
methods [4]. After synthesizing by each of following
methods, the most important part of research refers to
characterize the samples. Many great techniques are
being used to characterize graphene. We discuss here x
ray diffraction technique, as one of the most important
methods with a particular emphasis on the identification
of graphene. We try to demonstrate XRD abilities to
characterize various properties of these multifunctional
materials.

Materials and method

As we work in a laboratory service center, there are
different kinds of graphene and graphene oxide specimen
which send us to test. So, we used the pattern of theses
samples to determine the abilities of XRD method to
identify graphene type structure. Sample tests are
different kinds of graphene and graphene oxide with
different Synthesis procedures, as listed in Table 1. XRD
patterns were obtained with a diffractometer (XPert Pro
MPD-PANalytical) using Cu K radiation. All Patterns
were obtained in a same program which fixed with
02020 step interval and 00s/step counter time by
scanning line detector mode of the PIXcel detector.

Table1: Sample test specification

Code

Sample type

G1

Synthesis method
Chemical reduction of GO

G2

Chemical reduction of GO
Graphene

G3

Electrochemical

G4

CVD

GO1

Hummers method

GO2

Graphene Oxide

GO3

Hydrothemal
Staudenmaier method

Results and Discussion

Crystal structure specification
One of the most important parameters of different type
of graphene, which determine structure and application of
these materials, is interlayer distance [5]. XRD is known
as a simple method for structural investigation of
crystalline material like Graphene. In the XRD pattern of
GO samples (Fig. 1), the strong and sharp peak about 2
10 corresponds to an interlayer distance of .8.4
(d002) for the AB-stacked GOs which reported in the
literature, due to the existence of oxygen-rich groups on
both sides of the sheets and water molecules trapped
between the sheets [5]. There are meaningful relation
between GO interlayer spacing and synthesis method
(But we havent addressed this issue in this article). After
reduction of the GO samples (by different methods), the
characteristic peak of GO disappears, which indicates that
the interlayer distance of GO is considerably reduced by
removal of oxygen-containing functional group. A new
diffraction peak of graphite (002) about 26.462 appears.
The van der Waals attraction between two adjacent layers
becomes dominant as compared to those of surface
functional groups, leading to the restacking of the
graphene layer which formed the graphite [6]

Proceedings of the 5th International Conference on Nanostructures (ICNS5)

6-9 March 2014, Kish Island, Iran

Fig.1: XRD patterns of GO (left) and graphne (right) samples

Graphene samples (G1,G2,and G3) show a broad (002)

peak at 2 = 26819, 26812, and 238., respectively.
Upon using a Lorentzian function to fit each (002) peak
of G1, G2, and G3, are estimated d002 to be 3.40, 3.41,
and 3.31, respectively (Table 2). If we want to determine
this parameter of graphene by another technique like
HRTEM there is very difficult procedure to prepare and
examine sample (especially in Graphene).
Determining Number of layer and crystallite size
Another key parameter for determining application of
graphene is the average of number of stacking layer [3].
Some literatures reported this parameter for random
layered (graphene) of the coals by Scherrer formula [.-9].
Weve used these equations (eq. (1) and (2)) in grapheme
and GO XRD pattern parameters to calculate the average
number of layers.
09
002

002

(1)

The stacking height (L002) of the crystallite is determined

using the equation where is the wavelength of X-ray
used, B002 is the Full Width at Half Maximum of the
(002) peak and is the corresponding scattering angles
[10]. If each parallel layer consists of N layers, L002 for a

parallel layer group is obtained by

002

002

(2)

We have fitted the (002) profiles to obtain the number

of layers of the grapheme and GO samples. In table2, the
numbers of layers in graphenes are found to be 4 to 10
while in GOs these are 6 to 22. In both graphenes and
GOs, calculated average number of layers confirms
properties and some of results of other characterizing
methods (There arent addressed here).
If we use other methods like AFM cross-section height
profile analysis [11], HRTEM, or FESEM to determine
the number of layers for Graphene and GO[3112], there
are difficult sample preparations and the results are
localized for some random particles comparing XRD
results which are average of whole sample. In the other
hand, there are some restrictions in calculating layer
numbers by the other methods like Raman spectroscopy
[3].
Impurities Identification
In some synthesis Procedures, some impurities remain as
by product [3, 13]. XRD is the first and simplest method
for identification these materials. Fig. 3 shows XRD
pattern of Graphene which synthesis by CVD method. It

Table 2: D spacing, Number of layers and crystallite size from the X-ray diffraction patterns of the graphene and GO samples

Proceedings of the 5th International Conference on Nanostructures (ICNS5)

6-9 March 2014, Kish Island, Iran

indicate that catalysts of process (CoO and Mo2C)

remain in graphene. These data helps to design synthesis
process to reach pure products.

Fig.2: Composition identification of G4

Conclusions
In conclusion, a comparative study of graphene and
GO samples prepared by different methods has been
carried out by X-ray diffractometry. In terms of the
interlayer distance, number of layers, crystallite size as
well as impurity composition, of graphene prepared by
various synthesis methods can be compared by simple
XRD pattern. So we can recommend this technique as a
powerful and multifunctional method to characterizing
graphene type structures.

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