A Review of Pulsed Plasma Synthesis Methods For Preparation of Polymer Thin Films

International Journal of Trend in Scientific Research and Development (IJTSRD)
Volume 8 Issue 2, March-April 2024 Available Online: www.ijtsrd.com e-ISSN: 2456 – 6470
A Review of Pulsed Plasma Synthesis

Methods for Preparation of Polymer Thin Films
Kajal Kushwaha1, Sunil Singh1, Vivek Dwivedi1, Navnit Misra1, Rajendra Kumar2
1
Department of Physics, Brahmanand College, Kanpur, Uttar Pradesh, India
2
Department of Physics, Rama University, Kanpur, Uttar Pradesh, India
ABSTRACT How to cite this paper: Kajal Kushwaha

Conducting polymers are prominent materials in respect of their easy | Sunil Singh | Vivek Dwivedi | Navnit
synthesis in the form of thin films and sensitive response regarding Misra | Rajendra Kumar "A Review of
their physical and chemical properties. We in this paper present an Pulsed Plasma Synthesis Methods for
overview of different pulsed plasma polymerization methods for Preparation of Polymer Thin Films"
Published in
synthesis of polymer films tunable catechol bearing thin films and International Journal
plasma coatings from acetylene, acrylic acid and maleic anhydride of Trend in
plasma. After going through over 40 recent works of plasma Scientific Research
polymerization methods using pulsed plasma technique, we have and Development
discussed the existing challenges and have suggested the ways which (ijtsrd), ISSN: 2456-
can help students and researchers intended to work in polymerization 6470, Volume-8 | IJTSRD64703
field with simple and useful plasma synthesis methods for Issue-2, April 2024,
preparation of polymer thin films. pp.582-593, URL:
www.ijtsrd.com/papers/ijtsrd64703.pdf
KEYWORDS: Conducting polymer, Polymerization, Pulsed plasma,
Polymer films Copyright © 2024 by author (s) and
International Journal of Trend in
Scientific Research and Development
Journal. This is an
Open Access article
distributed under the
terms of the Creative Commons
Attribution License (CC BY 4.0)
(http://creativecommons.org/licenses/by/4.0)
INTRODUCTION
A new path in the sensing applications and detection  In another method, thin film coatings from maleic
of hazardous gases in the environment is being anhydride plasma acetylene and acrylic acid are
explored with the application of conducting polymer taken as functional groups in the plasma adhesive
based sensors. Conducting polymer synthesized in the bond.
form of thin films have been used in sensing
 In all above synthesis methods pulsed plasma
applications. Many review papers and studies in polymerization technique is used with different
previous years have been presented using plasma suitable methodologies.
polymerization techniques. However very few of
them provide the convincing view of plasma One of the first documented studies by N. Bondt et.al.
polymerization techniques for aniline thin films. is 1790s reports for polymer synthesis methods as the
first document de wilde et.al. [1], Berthelot et.al. [2,3]
Good conductivity, greater stability, higher solubility
studied arc synthesis of hydrocarbons. German
in organic solvents ease of preparation of various scientist presented the first study of synthesis of
conducting polymers such as polpyrrole, polystyrene, various organics using glow discharge [4-7].
polyphenylene and polyaniline are the benefits that
make conducting polymers attractive. Goodman [8] reported the first application of these
plasma polymers. Further studies reported
 In the other way with the knowledge of versatile applications [9-14] of various substances with
chemistry of polyphenols and catechols. The property improvement of materials. Plasma synthesis
catechols based polymers are reported which are is now adopted for various application such as surface
valuable in production of water-resistant and modification [15-18] and layer deposition for
biomedical adhesives. electrical devices [19-22]. Plasma state is ionized
@ IJTSRD | Unique Paper ID – IJTSRD64703 | Volume – 8 | Issue – 2 | Mar-Apr 2024 Page 582
International Journal of Trend in Scientific Research and Development @ www.ijtsrd.com eISSN: 2456-6470
gases consisting of photons, electrons, ions, neutral researchers working to synthesize plasma polymers
particles, radicals and metastable particles. Plasma is can select the best method for their experiments.
free space with equal number of positive and negative
Polyaniline (PANI) is the best sensing material
charged particles behave as neutral [23,24]. among conducting polymers. The response conditions
These plasma can artificially be generated in the determine their morphology, structure and physical
laboratory by electric discharge [25,26]. Plasma properties. The semiconducting properties of PANI
generated by this method is called non thermal or thin films modulated by the absorption and de-
cool plasma [27]. This technique provides a safeguard absorption of gases depicted significant role in
to substrates or substances due to low temperature of chemical sensors [32]. Pulsed plasma method has
heavy particles. Plasma polymerization is been widely use for the preparation of
advantageous due to its simple installation, fast semiconducting polymer films mainly (PANI) [33].
processing, low cost, low temperature and green The film so prepared was analyzed for its electrical,
synthesis [28-31]. optical, and structural characteristics. Two main
In this paper, we have presented plasma drawbacks of plasma polymers are
polymerization with pulsed plasma technique by 1. They have poor selectivity and easily react with
different approaches and have compared plasma chemical agent.
parameters through characterization of plasma 2. Even after accurate measurements; cause the
polymers, like Fourier Transform Infrared sensor signal to be non-linear.
spectroscopy (FTIR), X-ray Photoelectron Today sensors are very much used for environmental
Spectroscopy (XPS). Also through kinetics of monitoring and protection [35]. These sensors are
deposition and dependence of chemical and physical fabricated with the polymer thin films, which are
properties. Our purpose in this review is to provide a polymerized by plasma methods with which we are
reference to recent devices and methods of pulsed mainly concerned in our present study.
plasma polymerization and hope that student and
1. Toxic gases in factories

(b) Polyaniline formation (c) Conducting
and industries.
polymer
(d) Applications of PANI (e) PANI morphology (f) Plasma polymerization is a

process of synthesis thin
polymeric film in a low-
pressure
(g) Plasma polymerization technique (h) On coating techniques for surface

protection
In recent years polymer has attracted people’s attention for its new invention. Being light strong and flexible and
suitability of thermal, electrical, high specificity, and oxidation resistance, these are very useful for
optoelectronics, biosensors, chemical sensors, and electronic display. Plasma polymerization is a process of
synthesizing polymeric thin films in low pressure electric discharge [37]. This technique is being applied for
protection of membranes for reverse osmosis, insulating layers for semiconductors and protective coatings for
optical components, we have focused too.
Here we present a review on pulsed plasma deposition techniques, materials, and their characterization by
different workers with an inclusion of their basic instrumentation.
Experimental:
Materials and methods:-
We have studied the experimental arrangements of different workers for plasma polymerization.
Inductively coupled Pulsed Plasma Polymerization (PPP):-
Rajendra Kumar et.al. (38) used pulsed plasma polymerization to make a variety of films. Using conducting
polymer such as polyaniline [39, 40, 41], polyethylene [42], Polypyrrole [43] etc. In their method a number of
volatile organic compounds could be use to the plasma reactor. In their system contamination of the film could
be avoided due to no use of oxidants and solvents [44]. A thermocouple gauge is used with capacitance
monometer to monitor reactor pressure. Thermocouple guage is calibrated in absence of plasma and during
deposition of film it was removed. After enough monomer has reached to reactor, 1.8 µF capacitor was
discharged and during activation of plasma, with decay time constant 10µs, the RF coil was excited with a
damped sinusoid of 290kHz. After completing 10 such plasma shots the reactor was evacuated and fresh
monomer vapor was refilled. The substrate holder and RF coil separations were varied. Glass plates and indium
tin oxide (ITO) were used as substrates and the choice of substrate depended on the method of characterization.
The reagent-grade aniline (Aldrich; 98.5) monomer purified with triple distillation were stored in a dark bottle in
nitrogen affinity. Profilometer was used to measure thickness of plasma polymerized aniline films.
Fig. 1. Shows a typical schematic diagram of plasma polymerization unit with an argonatmospheric
plasma brush
Atmospheric Aerosol Assisted (PPP):-
In another working Vincent Jalaber et.al. [45], who used an environmentally friendly technique of pulsed plasma
technique where plasma deposition were performed on mirror polished stainless steel (ss) disks and slicon
wafers polished on both faces. A home synthesized Dopamaine Acrylamide (DoA) was produced according as
Patil et. al. (2015) [46]
The 2-hydroxyethyl methacrylate monomer (HEMA 97%), the micro-BCA protein assay kit, liquid precursor
mixture were managed in their desired form. The substrates were cleaned with acetone and absolute ethenol for
5minutes each and dried under nitrogen flux.
Atmospheric pressure dielectric barrier discharge (AP-DBD) was used to deposit the coatings. The discharges
were produced between two plane parallel electrodes generating a 19cm2 plasma discharge area with electrode
gap 1mm, the sample placed in between. The droplet size distribution of the precursor spray was centrered
around 1µm. A corona generator with a 10kHz sinusoidal signal was used to substrate plasma. Modulated
electrical excitation was used to deposit coatings. The applied voltage, the current and the charge were
determined using sutiable processes. The average power value was given as
Wa (W) =Wpeak (W) ×tON/ tON + toff.
Functionlized Coatings From (PPP):-
Going through an other work by marisol Ji et. al. [47]. Where they used organic precursor as gaseous acetylene
(Air Liquid) and liquid acrylic acid (sigma-Aldrich). These were filled in a quartz tube in a low pressure. They
used elastomers as Poly ( acrylonitriel butadiene) rubber (NBR) and fluoroelastomer (FKM) respectively. The
polymerization process was carried out in the chamber and vaporised tanks to the low pressure.
The process of plasma polymerization was carried out in a capacitance radio frequency (RF, 13.56mHz) plasma
reactor. The residual pressures between 10-5 to 10-4 mbar was maintained with working pressure around 10-2
mbar. Two plates are separated by 12cm and powered with a caesor RF generator and a glow discharge is
injected between them. Plasma discharges were created for varying atmospheres.
Fig.2. Plasma Polymerization
Fig.3. 2- hydroxyethyl methacrylate monomer (HEMA)
Fig.4. Molecular structure of EGDMA homo polymerization

Preparation of PANI Thin Films:-
As in the entire review and analysis we have taken polyaniline (PANI) as one of polymers. Here is brief
preparation process of the same. The pulsed plasma polymerization of PANI is done in a plasma reactor by
pulsing of RF plasma. In which monomer injector also operates in a pulsed monomer.
The oscilloscope is provided to control the injection of vaporized monomer. As the pulse of monomer enters the
evacuated reactor, the maximum part of liquid is vaporized by flash boiling and rest is disintegrated into
droplets, collected by mesh separator at 20cm form injector nozzle. When the pressure reaches nearly 40Pa the
aniline pulses are injected in 10ms. Thin films are deposited with a state fill of vapour.
Fig.5. Formation of PANI thin film
Fig.6. Formation of Catechol
Film Characterizations:
The PANI thin films prepared by inductively coupled pulsed plasma polymerization (PPP) were characterized
using UV-Vis, FTIR, and other techniques like optical microscopy. The films grown on glass microscope slides
were used for FTIR measurements and optical absorption spectra was carried out with dc-nulling optical
transmittance bridge.
Fig.7. FTIR Spectra of unstirred synthesized polyaniine FTIR spectra of unstirred synthesized
polyaniline
Fig.8. Optical absorption spectra as a function of the photon energy of PANI thin film
Fig.9. SEM Image of thin films
Fig.10. Optical absorption spectra as a function of the photon energy of PANI thin film
Fig.11. Schematic representation of the atmospheric aerosol assisted plasma process.
Fig.12. (A) Example of pulsed voltage with tON of 5 ms and tOFF of 15 ms (B) mass deposited per pulse
(i.e., tON + tOFF) for a 15 ms tOFF and tON values ranging from 1 to 15 ms (error bars: means ±SD, n=3.
Fig. 13. SEM pictures for coatings deposited at 15 ms tOFF and tON of: (A) 1 ms, (B) 5 ms, and (C) 10
ms. AFM pictures for coatings deposited at 15 ms tOFF and tON of: (D) 5 ms and (E) 10 ms.
Fig.14. Table summarizing XPS analyses for pp(HEMA) and pp(DOA-HEMA) deposited at 1:15 ms
and 10:15 ms (A), XPS C1s envelope overlaps of pp(DOA-HEMA) deposited at 1 and 15ms tON and 15
ms tOFF(B).
Fig.15. ESI mass spectrum recorded for a pp(DOA-HEMA) deposited in a 1:400 ms pulsed mode.
Fig.16. Chemical schemes of (a) liquid N,N-dimethylacrylamide (DMA), (b) liquid ethylene glycol
dimethacrylate (EGDMA), and (c) solid dopamine methacrylamide (DOMA)
Factor Toff µs P(w) Q(sccm) T(mint)
T0ff (µs) 0.06 0.2 0.01
P(w) 0.08 -0.03 -0.07
Q(sscm) 0.06 -0.06 -0.20
T(mint) -0.21
Table 1: Effect (diagonal terms) and interaction (extra-diagonal terms) values calculated from the
DoE with different factors for pp-AA.
CC/CH response CO/CH response
Factor Toff (µs) P (w) t(mint) Toff (µs) P(w) t(mint)
Toff (µs) 0,36 -0,19 -0.06 -0,48 -0,15 -0,19
P(w) -0,19 0.02 0,42 0,21
T(mint) -0.25 0,81
Table 2: Effect (diagonal terms) and interaction (extra-diagonal terms) values calculated from the
DoE with different factors for pp-AA.
S. NO. Experimental condition Thickness (nm) Average deposition rate (nm/pulse)

1. 13 Pa, 50 plasma pulses 32.78 0.66
2. 13 Pa, 100 plasma pulses 98.80 0.99
3. 27Pa, 50 plasma pulses 88.64 1.77
4. 27 Pa, 100 plasma pulses 157.5 1.57
5. 40 Pa, 50 plasma pulses 236.4 4.72
6. 40 Pa, 100 plasma pulses 314.7 3.15
Table 3: Film Thickness and Average Deposition Rate of PANI Thin Film
Fig.17. The plot of the current-voltage of the PPAni, PDPA, and PPAni-PDPA (a) linear plot; (b)
semi-log plot.
In atmospheric aerosol assisted PPP. Ultraviolet-visable (UV-Vis) absorption spectra was taken using Perkin
Elmer 950 UV-Vis NIR with 2ml resolution. FTIR was carried out in the Attenuated Total Reflectance (ATR)
mode using [45] Hyperion 2000 spectrometer. X-Ray photoelectron spectroscopy (XPS) was done with Kratos
Axis Ultra DLD instrument.
In functionalized coatings PPP, FTIR spectroscopy was performed with Burker Vertex 70v spectrometer in the
range 4000-400cm-1 and resolution 2cm-1 after 10minutes of sample deposition. XPS was done with Kratos Axis
Nova France. The Near Edge X-ray fine structure analysis-spectroscopy (NEXAFS) was performed at
Helmholtz-Zentrum Berlin fur Materialien und Energie (HZB). All concerned characterization modes are shown
in the diagrams.
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International Journal of Trend in Scientific Research and Development (IJTSRD)

A Review of Pulsed Plasma Synthesis

ABSTRACT How to cite this paper: Kajal Kushwaha

1. Toxic gases in factories

(d) Applications of PANI (e) PANI morphology (f) Plasma polymerization is a

(g) Plasma polymerization technique (h) On coating techniques for surface

Fig.2. Plasma Polymerization

Fig.3. 2- hydroxyethyl methacrylate monomer (HEMA)

Fig.4. Molecular structure of EGDMA homo polymerization

Fig.5. Formation of PANI thin film

Fig.6. Formation of Catechol

Fig.9. SEM Image of thin films

Fig.11. Schematic representation of the atmospheric aerosol assisted plasma process.

S. NO. Experimental condition Thickness (nm) Average deposition rate (nm/pulse)

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