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IJSRD - International Journal for Scientific Research & Development| Vol.

4, Issue 03, 2016 | ISSN (online): 2321-0613

Characterization Technique of Nanofibers


Latika Susheel Chaudhary1 Prerana Ravindra Ghatmale2 Dr.S.S.Chavan3 Dr.R.N.Patil4
1,2
Research Scholar 3Associate Professor 4Professor
1,2
Department of Nanotechnology
1,2,3,4
Bharati Vidyapeeth Deemed University College of Engineering, Pune
Abstract Nanofibers because of its unique properties it is a series of looping and spiraling motions which is caused due
used in various field and application. There are many to the electrically driven bending instabilities. To reduce the
different methods to produce these nanofibers, out of all them bending instabilities caused due to the repulsion of
Electrospinning is the most promising technique to produce electrostatic charges, the jet elongates to undergo large plastic
continuous nanofibers. It becomes an essential part to analyze stretching that finally causes significant reduction in diameter
the diameter, thickness as well as strength of these nanofiber [3]. Due to the size of nanofibers it is difficult to form
to understand the different mechanical, chemical, optical different assemblies through physical manipulation. But by
properties of these as-spun nanofiber. This paper using electrospinning technique it is easy to fabricate various
concentrates on explaining some of the main technique used nanofiber assemblies in situ . Formalas has series of patents
to analyze and characterize the nanofibers along with the [1934 to 1944], stating the experimental setup for the
reported example. production of polymer fibers using electrostatic force[2].
Key words: nanofiber, electrospinning, characterization There are various parameters which affect transformation of
polymer solutions into Nanofibers. These parameters can be
I. INTRODUCTION categorized:
Nanotechnology is study of manipulation of matters at atomic (1) Solution Parameters which involves concentration of
and subatomic scale. It is combination of physics, chemistry, polymer solution, molecular weight, viscosity,
biology and other fields of engineering applied together to conductivity/surface charge density,
manipulate and develop system in nanometer range. (2) Process Parameter includes voltage, flow rate, collectors,
Nanomaterials can be classified according to different Distance between syringe tip and the collector,
dimensions. The first is zero dimensional structure(0-D) (3) Ambient Parameters such as humidity, solution
which is nanoparticles, nanoshells, nanoporous silicon, the temperature, air velocity.
second is one dimensional structure(1-D) such as nanorods Fiber diameter is the most important structural
,nanowires, nanotubes nanofibres,the third is three characteristic in Nanofiber. Here in paper the different
dimensional structure examples are discs, quantum wells, techniques to characterize nanofibers will be studied. The
ultrathin films.Fibers having diameter in nanometer range are structural and morphological properties of Nanofibers can be
known as Nanofibers. These nanofibers can be produced by characterized by Scanning Electron Microscope (SEM),
various polymeric solution. When reduced from micrometer Transmission Electron Microscope, Atomic Force
to nanometer range They have unique properties such as Microscope(AFM). The chemical characterization is
extraordinarily high surface area per unit mass, improved performed using FTIR, NMR Techniques, Raman
pore size, better surface properties, thin layer , highly porous, Spectroscopy. By using the AFM, SEM and TEM technique
high permeability, low basic weight, retains electrostatic the Bending Test and Youngs Modulus was obtained which
charges and cost effective Polymeric Nanofibers can be can be used to characterize the Mechanical properties of
obtained. Because of such interesting properties of Nanofiber. Apart from the above mentioned methods X-Ray
polymeric nanofibers they are used in various field for many Diffraction(XRD) ,Field Emission Spectroscopy(FEM),TG-
important application[1]. There are many different processes DSC,UV-IS are some of the technique that were also used to
to produce these nanofibers such as Drawing, Template analyze the property of nanofibers[1,2,3,4]. The main aim of
Synthesis, Phase Separation, Self-Assembly, Electrospinning paper this paper is to explain the principle ,working and its
etc [2]. Out of the all technique Electrospinning is the most related examples of how the AFM,SEM,TEM and XRD
reliable and efficient technique to produce nanofibers on techniques were used to analyze nanofibers. The organization
large scale. It produces continuous polymeric nanofibers and of the paper is in following manner first part paper is
thus allowing it to manipulate and control the fiber diameter, Introduction to Nanofibers, Electrospinning Process,the
surface area, porosity of resultant fiber as well as weight per various parameters affecting electrospinning working, the
area. In a typical Electrospinning setup it requires a high second part of paper consist on explaining the applications of
voltage source, a flat tip needle, syringe and a conducting nanofibers in various field thus explaining importance of
collector. The principle working of Electrospinning involves nanofibers, the fourth part concentrates on characterization
a polymer solution which is charged using a high electric techniques and its reported examples and lastly conclusion on
voltage source. This charge is either applied by inserting the analysis technique of nanofibers.
electrode directly in the solution or by applying it to the
needle from which the solution is ejected. A jet is ejected
from the charged polymer solution when the applied electric
field or electrostatic repulsion overcomes the surface
tensions. As the intensity of the electric field is increased, the
hemispherical surface of the polymeric solution present at tip
of the capillary tube gets elongated and forms a structure
called as Taylor Cone. As it reaches the target, the jet forms

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Characterization Technique of Nanofibers
(IJSRD/Vol. 4/Issue 03/2016/529)

sample surface. AFM is a non destructive technique and can


also perform mechanical characterization by deflecting one
end of the nanofibers with an AFM tip while keeping the
other end fixed. It works on the principle of measuring the
force between a sharp probes and surface at a very short
distance. These forces depends on the type of sample,
operating modes and condition used during measurement.
The AFM works in three scan different modes:
1) Contact Mode
2) Non Contact Mode
3) Tapping Mode
Each modes has its own advantages and
disadvantages and can be chosen depending upon the type of
sample and information to be obtained.[6,24-25]

Fig. 1: Schematic Diagram Of Electrospinning Setup[22]

II. APPLICATIONS OF NANOFIBERS


Electrospun nanofibers due to their unique properties have
found application in various field such as biomedical, energy
harvest, storage & generation, environmental sector.
Following are some of the noted examples of as-spun
nanofibers in various sector:
A. Energy Harvest, Storage & Generation:
Electrospun Nanofibers such as Polyacrylonitrile(PAN),
Polyvinlyidenedifluoride(PVdf) have found application as
separator in Li-ion battery, because of nanoporous structure
they provide better ionic conductivity.CNF/Si composite
nanofibers have been reported useful as anode for Li-ion Fig. 2: Schematic Diagram of Atomic Force Microscope
battery. 1) Analysis of Nanofibers by AFM:
AFM has three main capabilities: Imaging, Force
B. Environment Conservation:
Measurement, Manipulation. Out of these AFM is used to
Electrospun Nanofibers are being used as materials for create 3 dimensional images to confirm the structure and
chemical sensors, filtration and adsorption of metal ions diameter of nanofiber obtained, secondly it is also used for
Nanowires obtained through electrospinning are used in the mechanical characterization. Some of the noted results are
application of sensors. Sno2 and MoO3 nanowires are used as follow:
in chemical sensors reported to have quick response time and W. Nuansing et al. reported 2D and 3D images of
better sensitivity for H2S and NH3.It has been reported that TiO2/PVP composite nanofibers calcined at 400,700 and
when Nylon-6 membrane was compared with HEPA(High 800C.AFM images confirmed that the obtained
Efficiency Particulate Air) filter, the nanofibers membrane nanofibers have cylindrical structures with varied
had better efficiency. diameters. Representation is shown in Fig 7.[13]
C. Biomedical Applications: S.-H. Lee et al. calculated Young Modulii of the Tio2
A lot of study have been reported to use electrospun and PVP/TiO2 which were 0.9 and 75.6 GPa nanofiber
nanofibers as tissue scaffolds, engineering bone tissues, cell by Three-Point Bending Test using AFM.[14]
culturing for muscle, bones and tissue. Nanofibers
membranes such as Poly(Este Urethane) area
(PEUU)/collagen blend , poly(L-lactide-co--caprolactone)
(PLL A-CL) have been reported to provide improved fiber
elasticity ,tensile strength ,better cell adhesion.[26-28]

III. CHARACTERIZATION TECHNIQUES


A. Atomic Force Microscope:
It was invented by Binning et.al in 1986.Atomic Force
Microscope works on the same principle as Scanning Probe
Microscope. It is used to determine the 3D profile of
nanostructures such as quantitatively measuring the surface
roughness, visualizing the surface nano-textures, probe local
changes in friction, measuring the surface forces, and
assessing the changes occurring in local elasticity over a

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Characterization Technique of Nanofibers
(IJSRD/Vol. 4/Issue 03/2016/529)

Fig. 4: Schematic Diagram Of Scanning Electron


Microscope[23]
The samples which are not conductive has to coated
with conductive layer and the process is called as sputter
coating[9].

Fig. 3: 2D And 3D Images Of Tio2/PVP Composite


Nanofibers Calcined At 400,700 And 800C[13]
B. Scanning Electron Microscope:
The Scanning Electron Microscope as the name suggest it
uses the electron beam to scan and form the image of the
sample. Unlike conventional microscopes which uses the
optical light to scan and magnify the sample, SEM makes use
of the electromagnetic fields to magnify the sample[7,8]. The
main advantage of SEM is that it has high depth of sharpness
which provides information about the sample when observed
at different distances from scanning level. It provides various
information of sample such as Topographical, Morphology,
Composition and Crystallographic Structure. The entire setup
is having vacuum space to ensure that the sample interacts Fig. 5: Electron/Specimen Interactions
with the beam and not the air. The samples which are to be 1) Analysis Of Nanofiber By Sem:
analyzed by SEM has to be conductive and should also SEM method allows to measure the diameters of as-spun
withstand vacuum environment. [6,9,23] nanofiber and also gives information about the
heterogeneities in the structure that impact the behavior of
nanofibrous materials. Some of the examples include:
X.Yang et al. analyzed PVA/zinc acetate composite
nanofiber and reported with the use of SEM, nanofibers
of diameter 50-100nm.[15]

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Characterization Technique of Nanofibers
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(a) (b) Fig. 9: Heterogeneties in Polylactide Nanofiber(B)


Fig. 6: SEM Images for (A)PVA/Zinc Acetate Composite C. Transmission Electron Microscope:
Fiber, (B) Calcined at 700C In Transmission Electron Microscope a beam of electron is
Kumar et al. reported the result TiO2/PVP nanofibers passed through a thin specimen. An image of the sample is
with average diameter of 450nm with condition 10Kv obtained when the beam of electron interacts as it passes
and 1ml/h from the ethanol/acetic acid/PVP/Ti(OiPr)4 through the sample and it is magnified on the fluorescent
solution.[16] screen. TEM is used to study the composition, growth of
layers, defects in semiconductors. High resolution is used to
analyze the quality, shape, size and density of quantum wells,
wires and dots. The basic components of TEM machine
consist of : (a)Electron Source, (b)Electromagnetic Lens
System, (c) Sample Holder,(d)Imaging System [10-11].

Fig. 7: SEM Image of Tio2-PVP Composite Nanofibers


Electrospun at 10Kv and 1ml/H
SEM images depicting heterogeneities in polylactide
nanofibrous structures is shown in Fig.9

Fig. 10: Schematic Representation Of TEM Machine[11]


1) Analysis of Nanofiber by TEM:
TEM is useful for determining the structure and composition
Fig. 8: Heterogeneties in Polylactide Nanofiber(A) of individual particle present inside the as-spun
nanofiber[17]. Few of the examples of analysis of nanofiber
by TEM include:
Fig 11 shows TEM images of PLGA/Ag Nanofibers, In
the reported images it can be seen the presence of Ag
nanoparticle. The overall size of the nanofiber is between

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Characterization Technique of Nanofibers
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the range of 5 to 10nm and size of the Ag nanoparticle is target materials. Materials having regular structure
50 to 100nm[18] (crystalline structure), the scattered X-Rays goes through
Constructive and Destructive Interference. This is also
known as Diffraction. The diffraction of crystal is calculated
by Braggs Law:
n= 2dsin
Where, n=integer,
d=inter-planar spacing
The directions of diffraction depends upon the size
and shape of the unit cell of the materials. The intensities of
the diffracted waves depemd on the kind and arrangement of
atoms in the crystal structure[12]

Fig. 11: TEM Images Of PLGA/Ag Nanofiber[18]


M. Vahtrus et al. reported the analysis of TiO2 nanofiber
which revealed morohology and confirmed that there are
no defects inside the structure.[19]

Fig. 14: Diagram representating the process of X-Ray


Diffraction
1) Analysis of Nanofiber by X-Rd:
X-Ray diffraction is used to study the crystalline structure of
the nanofibers. It has prove useful to study nanofibers at
Fig. 12: TEM image of TiO2 Nanofiber[19]
different phases when calcinated.
R. Rani, S. Sharma reported the TEM images Of SnO2
Kumar et al. by using the technique of XRD studied the
nanofibers which were obtained after calcinations[21]
phase evolution and crystal structure of the electrospun
TiO2.[16]

Fig. 13: TEM Image Of Sno2 Nanofiber


D. X-RAY DIFFRACTION TECHNIQUE(X-RD):
X-RD Technique basic principles depends on the dual
wave/particle nature of X-rays which is used to obtain the Fig. 15: XRD Pattern showing the transistion of anatase and
information about the structure of crystalline materials. Main rutile phase.[16]
use of this technique is to identify and characterize the Liu et al. reported different crystalline and structural
compound based on their diffraction pattern. properties when SiO2 nanofiber were pyrolyzed at
X-rays are produced by bombarding a metal target different temperature.[20]
(Cu, Mo usually) with a beam of electrons emitted from a hot
filament (often tungsten).When an incident beam of
monochromatic X-rays strikes the surface of the target
material, it leads to scattering of the X-rays from atom of the

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Characterization Technique of Nanofibers
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[3] Ramazan Asmatulu, Mehmet B. Yildirim, Waseem


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[4] MeiLing Hu, MingHao Fang*, Chao Tang, Tao Yang,
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Min The effects of atmosphere and calcined
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Research Letters 2013, 8
[5] Jakub Sirc, Radka Hobzova, Nina Kostina, Marcela
Munzarov, Martina Juklckova, Miloslav Lhotka, S
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Morphological Characterization of Nanofibers:
Methods and Application in Practice, Journal of
Fig. 16: XRD Spectra Of Sio2 Nanofiber Pyrolyzed At Nanomaterials.
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