Introduction 1

INTRODUCTION

Plasma is the least organized collection of atomic nuclei and electrons i.e. it is
a mixture of these two components. Plasmas can conduct electric currents and
can be manipulated by electromagnetic fields. Because this characteristic also
occurs if the atomic bond is not completely organized, and thus atoms have
not given up all electrons, the term ionised gas and plasma are used
synonymously. Plasma is thus characterised by the following properties:
 Contains an increased number of charge carriers (conductivity),
 Quasineutrality (same number of positive and negative charges in a
unit volume),
 Increased energy and heat content,
 Creation of equilibrium states (charge carrier formation and
recombination is stationary),
 Existence of speed and energy distribution functions (permit the
characterization of the plasma by temperature) 1-3

CLASSIFICATION OF PLASMAS

Plasmas can be classified in various ways:

1) Based on their current-voltage characteristic they can be classified as:

Glow discharge
Glow discharge is the oldest type of plasma; it is produced at reduced pressure
and assures the highest possible uniformity and flexibility of any plasma
treatment. The plasma is generated at a gas pressure in the 0.1-10 MPa range.
The electromagnetic field is in the range of 0.4-0.8 kV and the broad
frequency range is 0-2.45 GHz.

Corona discharge
Corona discharge is formed at atmospheric pressure by applying a low
frequency or pulsed high voltage over an electrode pair, the configuration of

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Introduction 2

which can be one of many types. Typically, both electrodes have a large
difference in their size. The corona consists of a series of small lightning-type
discharges; their inhomogeneity and the high local energy levels make the
classical corona treatment of textiles problematic in many cases. It is
generated at gas pressures equal to atmospheric pressure. The electromagnetic
field is greater than 15>kV and has a frequency range of 20-40 kHz.

Dielectric barrier discharge (DBD)

Dielectric barrier discharge is formed, by applying a pulsed voltage over an
electrode pair, of which, at least one is covered by a dielectric material.
Though also here lightning-type discharges are created, a major advantage
over corona discharge is the improved textile treatment uniformity.

2) Depending on the temperature of ions and electrons, and the degree of

ionisation, plasma can also be classified as hot plasma and cold plasma. Here
the word “cold” expresses the low energy content of the plasma. It is a non-
thermal or nonequilibrium plasma, with the gas atoms at ordinary
temperatures and electrons at considerably high temperatures. The hot plasma
is the thermal or equilibrium plasma, with all components approaching
complete or local thermodynamic equilibrium4-7

3) AC discharges are preferred over DC driven discharges in plasma systems

for a number of reasons. First, as the frequency of AC increases, the energy
transfer into the discharge becomes more efficient, especially at frequencies
between 100 kHz and 1 GHz, the RF regime. Also, in a DC discharge, charged
particles from the plasma can accumulate on the substrate surface causing
unwanted charging effects. By alternating the direction of the current flow
sufficiently rapidly, these charging effects can be reduced. At RF frequencies,
this alternation is sufficiently rapid to almost completely eliminate charging
effects.

4) Plasma is usually classified into two different types depending upon the
electron affinity of the process gases used. Process gases can be arranged
roughly in the following order of increasing electronegativity:

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Introduction 3

ArN2<CF4<CF2Cl2<Cl2<CFCl3<SF6<CCl4

Electropositive Plasma:
These are discharges consisting mainly of species, which do not form negative
ions easily. Examples are noble gases like Ar, He and some unreactive gases
like N2. In this plasma, the number of positive ions is almost exactly equal to
the number of electrons, although both are much lesser than the number of
neutrals.

Electronegative Plasma:
Electronegative Plasma contains a significant number of species, which have a
positive electron affinity. In these cases, the number of free electrons is
significantly reduced as a result of capture by electronegative species to form
negative ions. Electronegative Plasma requires higher power to sustain and is
difficult to initiate. This makes electronegative plasma unstable and often non-
uniform. The electron temperature is also much higher than in electropositive
plasma.8

PLASMA CHEMISTRY

In low-pressure plasmas, the kinetic energy is different for ions and electrons.
The electrical energy stored in the plasma is converted into the following
energy forms:
 Movement energy of the charged particles (electrons, ions).
 Excitation energy of activated particles,
 Electromagnetic radiation, which is emitted as visible UV and IR light
and is a result of the recombination of the charged and activated
particles.
The following elementary processes occur in plasma:
1.excitation: A2 + e- A2 + e-

2.dissociation: A2 + e- 2A + e-

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Introduction 4

3.ionisation: A2 + e- A2+ + e-

4.ionising dissociation: A2 + e- A + A+ +2 e-

5.dissociation into radicals and ions: AB + e- A + B-

6.electron capture: A2 + e- A- + A

7.radical formation due to radiation.

8.formation of new molecules, atoms and radicals by neutralisation,

recombination and structural reorganizations1

Plasma chemistry is concerned with the reactions occurring solely in the bulk
plasma and also reactions between plasma particles. In the plasma states, the
electromagnetic radiation is produced when excited molecules move to lower
levels of energy, giving up the difference in the energy to the radiative
electromagnetic field. Some of this radiation is re-absorbed by the plasma and
some of it is lost to the plasma environment. Broadly plasma reactions can be
divided into two:
1) Formation of new bonds (creation of molecules)
2) Destruction of existing bonds (creation of simpler molecules or free
radicals)
To break such bonds, the particle selected for the purpose must be able to feed
energy from its own reserve into the molecular system in which the “cleavage”
is to be effected. The ease with which such dynamic cleavage can be carried
out depends to some extent on the kind of particle selected for the task. That is
the nature of the exciting agency chosen will determine to some degree the
efficiency with which particular bonds are broken or, conversely, the ease with
which certain bonds can be created.
A complication that must be accepted is that in any given type of reactor, in
which plasma reaction takes place, there will usually be several different
particles, which are simultaneously inducing the formation of a given bond

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Introduction 5

and also destroying such bonds. It is the outcome of this competition, which
determines the net yield.
Let us consider the formation of oxygen radicals:

Production of oxygen radicals: The oxygen atom has an affinity for

electrons. However, it is possible to produce stable negative oxygen ions in the
plasma. The various reactions are:

O2 + e O+O+e

O2 + e O*2 + e

O2 + e O+2 + 2e

O2 + e O++2 + 3e

O2 + e O++ + O + 3e

O2 + e O+ + O - + e

O2 + e O+ + O -

In the first of the reactions listed, showing the direct production of the free
radical O, the symbolism is misleading in that the states of the two oxygen
atoms are shown as identical. One of the two atoms will be in a triplet P state,
the other a singlet D state. One further point of interest is that the negative
oxygen ion appears to have an excited state with a binding energy of the order
of 0.2 eV. This would make the excited negative oxygen ion have about the
same energy as a neutral atom.9

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Introduction 6

PLASMA EQUIPMENT

Process gas
in

Glow Discharge Excited gas species

(Vacuum UV) Atom
Molecules
Ions
Electrons
Free radicals
Metastables

Substrate
Chemically
modified Surface

Electrodes
RF Power Process
Supply Gas out
Fig. 1: Schematic of the surface modification of a substrate in a gas
plasma reactor.

Plasma is a partially ionised gas containing ions, electrons, atoms and neutral
species. To enable the gas to be ionised in a controlled and qualitative manner,
the process is carried out under vacuum conditions. A vacuum vessel is first
pumped down via rotary and root blowers, sometimes in conjunction with
high-vacuum pumps, to a low to medium vacuum pressure in the range of 10 -2
to 10-3 mbar. The gas is then introduced into the vessel by means of mass flow
controllers and valves. Although many gases can be used, commonly selected
gases or mixtures of gases for plasma treatment of polymers include oxygen,
argon, nitrous oxide, tetrafluoromethane and air.
A high-frequency generator, which can be in the kHz, MHz or microwave
range, then ionises the gas into plasma, forming an environment that has been
referred to as “the fourth state of matter”.
The formed reactive particles react in a direct way with the surface without
damaging the bulk properties of the treated part. In fact, the surface
modification is limited to the outermost 10 to 1000 A of the substrate. One

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Introduction 7

distinguishing characteristic of plasma is a visible glow discharge, with

colours ranging from blue-white to dark purple, depending on the type of gas.
Plasma systems generally comprise of 5 main components: the vacuum vessel,
a pumping group, a gas introduction and gas-control system, a high-frequency
generator and a microprocessor-based system controller. Various optional parts
can then be added to adapt a base system to handle particular applications or
substrates, such as special barrels for small pieces, modified electrode racks or
guiding systems for textiles or fibres10
Furthermore, the plasma process can be carried out in different manners:
 The substrate can be treated directly in the plasma zone.
 The substrates can be positioned outside the plasma; this process is
called the remote process.
 The substrate can be activated in the plasma followed by a subsequent
grafting.
 The substrate can be treated with a polymer solution or gas, which will
be fixed or polymerised by a subsequent plasma treatment10

SURFACE MODIFICATION PROCESSES

The process of plasma surface modification of textile substrates can be divided

into four distinct mechanisms:
 Ablation/Etching/Cleaning
The ability of plasma processing to break down weak covalent bonds in a
polymer through bombardment with high-energy particles is known as
ablation. This affects the outermost molecular layers of the substrate exposed
to the plasma, which boils off and is removed by the vacuum. Because the
chemistry of any layers of surface contamination is also generally made up of
weak C-H bonds, plasma treatment can remove contaminants such as oil films
or injection molding additives, thereby leaving behind a uniformly clean and
active polymer surface.

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Introduction 8

Fig. 2: Ablation

 Crosslinking
Crosslinking is the setting up of chemical links between the molecular chains
of polymers. Plasma processing with inert gases can be used to crosslink
polymers and produce a stronger and harder substrate micro-surface. The bond
breaking occurs on the polymer surface, but since there are no free radical
scavengers, the molecule can do one of three things:
1. Recombine with the by-products and revert back to its original state.
2. It can react with an adjoining free radical on the same chain, forming a
double or triple bond (called unsaturation).
3. It can form a bond with a nearby free radical on a different chain
(crosslink).
Under certain circumstances, crosslinking through plasma treatment can also
lend additional wear or chemical resistance to a material. Medical applications
for plasma-induced crosslinking include catheters, clinical instruments and
contact lenses.

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Introduction 9

Fig. 3: Crosslinking

 Activation
The replacement of surface polymer groups with chemical groups from the
plasma is called activation, or more correctly molecular modification. During
activation, the plasma breaks down weak bonds in the polymer and replaces
them with highly reactive carbonyl, carboxyl and hydroxyl groups. Activation
can also be performed with amino groups or other functional groups. The
resulting change in the substrate characteristics will be determined by the type
of chemical groups incorporated into the surface.

Fig. 4: Activation

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Introduction 10

 Deposition/Plasma polymerisation/Plasma-enhanced Chemical

Vapour Deposition (PECVD)
In plasma deposition, a thin polymer coating is formed at the substrate surface
through polymerisation of the process gas. Depending on the selection of the
gas and process parameters, these thin coatings can be deposited with various
properties or physical characteristics. Coatings produced in this manner
through plasma deposition exhibit different properties than films derived from
conventional polymerisation, including a high degree of crosslinking and
extremely strong adherence to the substrate11-12

Fig. 5: Plasma Polymerisation

ADVANTAGES OF PLASMA TREATMENT

 Surface layers of the substrate can be modified homogeneously in

seconds or in minutes without alteration of its bulk properties
 It is applicable to all suitable for vacuum processes i.e., almost free
choice of substrate materials
 The surface properties of those polymers, which are difficult to modify
with wet chemicals, can also be changed
 Different types of chemical modification are possible by choosing the
appropriate gases, most of which are environmentally friendly
 Chemical consumption is low
 Since the process is performed in a dry, closed system, it is safer as
well as environmentally friendly
 It increases product performance levels

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Introduction 11

 It decreases unit cost and at the same time, improved quality is

obtained
 Tailor-made products can be obtained
 It saves water, materials and energy7, 10-12

DISADVANTAGES OF PLASMA TREATMENT

 Expensive, high vacuum equipment are required

 There are difficulties in scaling up the process to production scale
including replacement of the batch process with a continuous process
 The optimal process parameters are system dependent, and since it is
such a complex process, a good understanding of plasma-polymer
interaction is yet to be achieved7

APPLICATIONS

 Adhesion promotion
Many polymers have a low to medium surface energy-examples include
polypropylene, polyethylene, polyamide and Teflon. This characteristic makes
it difficult to effectively apply adhesives or coatings. Through the use of
oxygen plasma, one can modify the surfaces of these materials such that they
obtain the best possible contact with the adhesive or coating.
The physical or chemical activation process forms a surface with an optimal
number of bonding sites that is entirely free of non-contact zones such as
bubbles or pinholes. For example, plasma processing can increase the surface
energy of polypropylene from 29 to 72 dynes/cm, which is approximately the
value of full water contact. Medical applications include surface preparation
for adhesive bonding of catheters and balloon catheters, dialysis filters and
bonding needles to syringe hubs10

 Cleaning
A clean surface on a device or component is deceptively difficult to attain.
Conventional cleaning methods can be incapable of removing certain surface
films, leaving a thin contamination layer. With plasma treatment, it is possible

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Introduction 12

to achieve outgassing and to completely remove contaminant films. In the

same way that weak chemical bonds are removed in the activation process,
contamination layers can be eliminated even from complex surfaces.
Plasma will remove non-visible oil films, microscopic rust or other
contaminants that typically form on surfaces as a result of stocking or previous
manufacturing or cleaning processes. Even injection moulding additives,
silicone-based compounds, release agents and partially absorbed contaminants
can be effectively removed from plastics, metals and ceramics. Plastic
additives not visible to the eye but capable of negatively influencing
subsequent manufacturing can be eliminated by plasma without destroying or
changing bulk substrate properties.
Extremely sensitive instrumentation parts or implants can be cleaned via
plasma processing. Ultrafine cleaning of components, electronic assemblies,
medical consumables, connectors and needles are typical applications10

 Hydrophilic properties
A specially developed plasma activation process can be used to make a
substrate surface hydrophilic. An important secondary effect is fast drying.
This permanently hydrophilic character can impart to woven or nonwoven
textiles, the capability to be used as blood filters or filtering membranes for
various applications, including micro filtration components for dialysis filter
systems10, 12

Fig. 6: Increase in hydrophilic property after plasma treatment

 Hydrophobicity
Through the use of semi-continuous textile treaters, it is possible to plasma
polymerise the surface of nonwovens and other textiles so that they become
hydrophobic. This technique is becoming popular with device manufacturers
looking for replacing conventional methods or improving results through

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Introduction 13

plasma technology. Applications include hydrophobic treatment of paper,

textiles and filter elements 10, 12

Fig. 7: Increase in hydrophobic property after plasma treatment

 Biocompatibility
The activation of surfaces to prepare them for cell growth or protein bonding
is another important application of plasma modification. Examples of in vitro
uses of plasma treatment include preparation of petri dishes and microtiter
plates for laboratory experiments or drug production purposes. The process
can also be used to enhance the biocompatibility of implants –for example, by
treating the surface of a device to increase the adherence of a
haemocompatible coating. Among the applications in this domain are vascular
grafts, lenses and drug delivery implants10

 Low friction coating

Some silicones and polymers such as polyurethanes have a typically high
coefficient of friction against other surfaces. By plasma treating components
made of such materials, a polymer coating with a lower coefficient of friction
can be applied to create a more lubricious surface10

 Barrier coating
Plasma modification can be used to deposit thin, dense barrier coatings that
have the effect of decreasing the permeability of plastic parts to alcohol or
other liquids or vapours. For example, plasma treatment of high-density
polyethylene can decrease the material’s permeability to alcohol by a factor of
10. 10

 Sterilisation
Gas plasmas are increasingly being employed to sterilise the surfaces of
medical components or devices. The method uses less toxic materials and can
be more cost-effective than irradiation.10

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Introduction 14

 Spin finish removal

Very often, surfaces are contaminated with spin finish (sizing). The presence
of a spin finish can significantly limit performance or largely influence coating
adhesion. The combination of the partial cleaning and activation gives good
results to wettability or achieved impregnation. A cleaning of the surface is
required prior to further production steps. The spin finish present at the surface
can be completely removed (100%). 12

 Surface preparation for prints, laminations and composites

Surfaces can be activated or prepared for printing, lamination or coating in a
way very similar to hydrophilic treatment. Also, materials difficult to bond to
can be imprinted after plasma preparation. A very significant secondary
advantage is that neither surface colour nor roughness is affected.
In this case, where shelf life prior to secondary processing is not a
consideration, the new atmospheric plasma is surely of high potential.12

 Preparation of fibres and roll goods prior to dyeing

It is still a problem to dye vivid colours on materials. Plasma treatment may be
the solution. For example, on wool it is possible to improve the dyeing after
plasma preparation, which results in more intense shades (150%) in
comparison to dyeing after conventional preparation. Additionally there is a
more homogeneous dyeing, a better soil release and increased shrink
resistance (3%). In fact, the plasma removes the natural oil always present in
wool.
Alternately, colour levels of a given intensity can be obtained using less
dyestuff, resulting in significant savings. Plasma pre-treatment also makes
polyester more intensely black. 12

1.9 SURFACE MODIFICATION BY GLOW DISCHARGE

Although plasmas can be created by diverse techniques such as flames,
electrical discharges, electron beams, lasers or nuclear fusion, the most
convenient way to create and sustain plasma is by gaseous electric discharges.
Elements of glow discharge experiment can be summarized as follows:
Electric power Coupling mechanism Plasma environment
Power

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Introduction 15

A.C. Pressure
R.F. Inductive Flow rate
D.C. Capacitive Type of gas / monomer
Microwave Resistive Electric and magnetic fields
Shape and size of electrodes
Distance between 2 electrodes

The plasma created by glow discharge processes has average electron energies
in the range of 0.1 to 10 eV and electron densities of 109 to 1012 per cubic cm.
in addition, the electron temperature of plasma is not equal to gas temperature,
but has a ratio Te/Tgas of 10 to 100. It is therefore possible to modify polymer
surfaces at ambient temperatures. During plasma treatments, etching, ablation
and re-deposition take place. Electron ion bombardment induces activated
species on the surface. These and such effects can be used advantageously for
several industrial processes13.
Plasma modification of the polymer causes an increase in the surface energy
of the polymer and an attendant improvement in surface wetting. Adequate
wetting of the surface by the adhesive contributes to an improvement in bond
strength by increasing the apparent area of contact over which the load is
distributed. This improvement in wetting directly contributes to the observed
improvement in the strength of the adhesive bond. However, the major
improvement of adhesive strength is dependent on the particular functional
group that has been created on the surface of the polymer. For many of these
applications, cold gas plasma surface treatment has become the preferred
industrial processing technique. Applications range from surface modifications
of plastics in the electronics industry to treatment of plastic automotive
components and biomedical devices. This technology has facilitated the
development of many products and increased use of plastics in these
applications.
Plasma processing is not one process but a "field of opportunities" which can
be classified into three categories that often overlap. These are:
(1) Plasma activation,
(2) Plasma-induced grafting, and
(3) Plasma polymerization.

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Introduction 16

Plasma activation is the alteration of surface characteristics by the substitution

of chemical groups or moieties for groups normally present on the polymer
chain being modified. In this category the surface modification effected by
direct and radiative energy transfer from plasmas excited in inert as well as
reactive gases to improve adhesive bonding, wettability characteristic and
printability of polymers. The assumed mechanism is free radical creation and
coupling of these free radicals with active species from the plasma
environment. Depending on the process and gas selected, a large variety of
chemical groups can be incorporated into the surface. These groups may be
hydroxyl, carbonyl, carboxylic, amino, or peroxyl groups. Most importantly,
the insertion or substitution of these groups in the polymer chain is under the
control of the operator. Therefore, the surface energies and the surface
chemical reactivity of plastics can be completely altered without affecting
their bulk properties.
In the second category i.e. plasma-induced grafting there are many potential
applications, but two which immediately spring to mind and have received
considerable attention to date relate to the modification of surfaces of films
and fibres for improving wettability characteristics and for flame retardancy
purposes.
The plasma polymerization refers to the formation of polymeric materials
under the influence of plasma. The advantage of plasma process is that the
materials, which cannot be polymerized by conventional methods, can be
polymerized and ultra-thin pinhole free film with good adhesion to the
substrate can be made.

Advantages and disadvantages of the glow discharge technique:

The principal advantages and disadvantages of the glow discharge technique

are set out in the table given below:
Advantages
1. Applicable to batch or continuous processing.
2. Low initial capital outlay.
3. Suitably applied to a wide range of systems.

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Introduction 17

4. Close control over experimental conditions.

Disadvantages
1. Cannot produce films to a specific formula.
2. Thick films are brittle and discoloured.

The glow discharge synthesis of polymers or modification of polymer surfaces

is a process of such flexibility, that either batch or continuous operation, can
be employed, whichever is the most desirable. The plasma process is a dry
reaction state and clean in nature when considering the problems of disposal of
solvent. The glow discharge technique often proves to be cost effective in
terms of power consumption, labour requirements and environmental
pollution. This contrasts with conventional solution techniques, which often
employ several steps and require solvents of high purity. Such synthetic
procedures are often carried out at temperatures greater than ambient.
RF and microwave generators are relatively inexpensive and vacuum systems
are readily constructed. Pumping requirements need not be elaborate since
moderate operating pressures are normally employed (~0.1-0.01 Torr).
Plasma techniques facilitate great control over operating conditions in terms of
pressure, flow rate, power, type of gas or monomer. For in-situ
polymerizations it is possible to coat the sample with the appropriate monomer
prior to introduction into the plasma reactor.
Turning now to the disadvantages, it can be seen that a previously unprepared
film cannot be synthesized to a given formula, and indeed it is not possible to
modify or to synthesize a ‘new’ polymer surface and, a priori, what the
resultant composition will be. Having first completed the experiment,
however, the glow-discharge technique may be relied upon to give
compositions and surface properties to a high degree of reproducibility.
When preparing thick films by plasma techniques, the products tend to be
brittle and discoloured. If this is an undesirable property, it is readily
circumvented by forming (grafting) the film on to a polymeric surface with the
required bulk properties.13-17

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1.10 IMPORTANCE OF PLASMA PROCESSES FOR SURFACE

MODIFICATION
In plasma free electrons gain energy from the imposed RF electric field,
colliding with neutral gas molecules and transferring energy dissociating the
molecules to form numerous reactive species. It is the interaction of these
excited species with solid surfaces placed in the plasma, which results in the
chemical and physical modification of the material surface.
For example, to enhance adhesion, treatment in oxygen plasma is generally
carried out. Oxygen plasma can be very reactive and forms numerous active
components. Even with this seemingly simple plasma you will find O +, O-,
O2+, O2-, O, O3, ionized ozone, metastably-excited O2 and free electrons. As the
components recombine, they release radiation, emitting a faint blue glow
along with UV radiation. The photons in the UV region have enough energy to
break the polymer's carbon-carbon and carbon-hydrogen bonds:

. .P .
PH + O + OH

. . .
PH + O H + PO
. .
P + O2 POO

. . .
PH + 2O P + H + O2

UV . .
PH P + H

All of these active species react with the polymer surface, in addition to
bombardment by photons, ions and neutral particles. This creates chemical
functionality on the polymer surface by incorporating hydroxyl, carbonyl, and
carboxylic acid groups. It is well documented that many conventional
adhesives chemically bond to these groups allowing improved adhesion. The
by-products of these reactions include CO2, CO, H2O and hydrocarbons of low
molecular weight that are readily removed by the vacuum system.
The effect of plasma on a given material is determined by the chemistry of the
reactions between the surface and the reactive species present in the plasma.
The resulting surface changes depend on the composition of the surface and

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Introduction 19

the gas used. Gases, or mixtures of gases, used for plasma treatment of
polymers can include air, nitrogen, argon, oxygen, nitrous oxide, helium,
tetrafluoromethane, water vapour, carbon dioxide, methane or ammonia. Each
gas produces a unique plasma composition and results in different surface
properties. For example, the surface energy can be increased very quickly and
effectively by plasma-induced oxidation, nitration, hydrolyzation, or
amination. Depending on the chemistry of the polymer and the source gases,
substitution of molecular moieties onto the surface can either make polymers
wettable or totally non-wettable. The specific type of substituted atoms or
groups determine the specific surface potential. For example, gases containing
oxygen are generally more effective at increasing the polymer surface energy.
14-16,18-19.

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