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International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882

Volume 5, Issue 2, February 2016

Efficiency of Plasma onto Denim Faded Garments


Bahira G. Gabr1 and Nasser N.Morgan2, 3
1
Clothing department, Faculty of Applied Arts, Helwan University, Cairo, Egypt
2
Physics department, Faculty of Science, Al-Azhar University, Cairo, Egypt
3
Al-Azhar Center of plasma technology, Al Azhar University, Cairo, Egypt
Abstract
Denim is defined as being traditionally a 3/1 warpfaced twill fabric made from yarn-dyed warp and
undyed weft yarn. Washing denim jeans is one of the
polluting activities in the textile and clothing industry.
Plasma treatment onto textile is an environmentally
friendly inexpensive process, when compared to the
traditional denim fading methods.
Atmospheric
pressure glow discharge has been utilized onto indigo
dyed denim, Oxygen and water vapor have been used
as working gases during the discharge process.
Various tests were taken examining the efficiency of
treated plasma faded denim; bending length, E, SEM
and ATR spectrum charts were obtained.
In
conclusion the optimum denim wash was for oxygen
APGD with highest current and least duration, where
E was highest value.
Keywords: Indigo dye, Atmospheric pressure glow
discharge (APGD) and color hue.

friendly inexpensive process, when compared to the


previously mentioned denim fading methods. The
production of faded looks in fabric using conventional
technologies involves large amount of water and most
of which being highly contaminated by chemical
products used in the process. Also the time-consuming
and old-fashioned processes are not suitable for mass
production and increase the production cost (Yang, C.
Q 2003; Montazer and Maryan 2008).
Indigo is extensively used for dyeing denim. Indigo
dye is known thousands of years ago, as a natural dye
attained from special plants; chemically the industrial
indigo is classified as a type of vat dyes, C.I. Vat Blue
1, produced by BASF of Germany in the 1890s
(Chakraborty and Chavan 2004). Indigo is a vat dye,
which needs to be reduced to its water soluble leucoform before dyeing (Vuorema 2008); as insoluble in
water, should be reduced using sodium hydro-sulphite
and sodium hydroxide, giving soluble in water
oxygen-free leuco indigo (white indigo), which by turn
oxidize by air giving back the blue insoluble indigo
(Hardwood et. al. 1999), with molecular formula
C16H10N2O2 seen in Figure1.

1. Introduction
Denim is defined as being traditionally a 3/1 warpfaced twill fabric made from yarn-dyed warp and
undyed weft yarn. Typical cotton construction: 32x19;
45x54 tex; 310 g/m2. More recently, other weaves
have been used in lighter constructions (The Textile
Institute 2002). Denim wash, is the discharging of
indigo dye to give the worn-out appearance for a piece
of a garment; Washing is an aesthetic finish creating a
worn look and softer hand in denim products (Halleb
2015). Washing denim jeans is one of the polluting
activities in the textile and clothing industry. Widely,
from the 1970s denim wash was done using pumice
stone, super-stone which is pumice wash for longer
period of time or sand-blasting. By the 1980s, acid
washed denim was done using a stone wash with a
weak chlorine; denim jeans is tumbled in a dry
washing machine with chlorine wetted pumice stones,
afterwards potassium permanganate was used instead
of chlorine. It was mentioned, by Yang et al. 2003,
that enzyme wash is commonly used as a wet process
technique in the clothing industry. Laser fading denim
is important as it is not a wet process; precisely
controlled faded patterns can be obtained. CO2 Laser
treatment is a clean production process (Kan C. 2014).
Plasma treatment onto textile is an environmentally

Fig.1: Insoluble indigo (Oxidized Indigo) - Water soluble indigo (Oxygen


Free Indigo)

Although desired fading effect could be achieved by


methods mentioned above, the following problems
were encountered: (i) difficulty in application and time
consuming due to problem in work; (ii) decrease in the
wear resistance of the product; (iii) inability to create
standard and reproducible designs; (iv) successful
application of designs is not possible on all textile
surfaces; (v) inability to create required shades; (vi)
inability to produce identical fading effect on both
sides of the products; (vii) loss of quality (Yang, C. Q
2003; Cheung HF et al., 2013). In addition, textile and
clothing industries use various chemicals in their
different processes such as denim wash; chemicals
afterwards cause pollution in the effluents which could
damage the equipment and the clothing product itself
(Aly AS et al. 2004). In a clothing factory time is
crucial, the super stone wash can take up to six hours,
while enzymes fading denim can take in between

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International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 5, Issue 2, February 2016

85mins to as little as 55mins (Nielsen 2012). A


sample of 20 x20 cm would take 45minson a 70cm/sec
CO2 laser machine, the same area would be faded in 6
to 10mins on a 10X14cm plasma head.
In order to cope with problems in conventional denim
faded processes, technologies should be adopted for
treating garments. The plasma treatment, being a dry
and low cost treatment, would be an alternative. A
previous paper, compared knitted fabric color fading
using atmospheric plasma to enzymatic process,
resulted on same color hue for both treatments
(Cheung H.F. et al. 2013).
A number of studies dealt with the effect of
conventional denim wash. Tarhan and Sariisik (2009)
studied the effects of sand blasting, laser application
and enzyme silicone wash on fabric physical
properties, hand, breaking and seam strengths and
fabric stiffness. Sular and Kaplan (2011) studied the
influences of some washing (rinse, enzyme wash,
stone, bleach) and special treatment processes on some
physical, mechanical properties and hand of two types
of denim fabrics. More recently, Halleb et al. 2015,
studied the tactile properties of stone, super stone and
stone bleach washed denim, subjectively through a
trained panel of 10.
There have been some studies in which the influence
of some conventional washing and special treatments
on the mechanical and physical properties of denim
fabrics were determined (Halleb et al. 2015); none has
researched the effect of Plasma onto those physical,
mechanical properties and color change affecting the
garments three dimensional look, durability and
appearance. The aim of this paper is to test for denim
washed garments efficiency, physical, mechanical
properties andE, utilizing plasma treatment.
Moreover, the SEM and ATC of treated Atmospheric
pressure glow discharge APGD denim were
determined.
A plasma is a partially ionized gas includes ions,
electrons, UV, and visible radiation, free radicals as
well as excited neutral species. A non-thermal plasma
is a type of plasma with electron temperature much
higher than ion temperature. The energetic electrons
can initiate reactive species in the plasma volume,
without excessive heat that make the plasma suited to
apply for textile processing. In addition, plasma is an
efficient source for generating large variety of
chemically active functional groups; such as oxygen
functional groups: =CO, =C=O,OC=O, COH,
COOH produced on the fabric surface through the
interaction between the plasma and carbon surface
(Chan et al. 1996; Hakeimet al. 2008; Morent et al.
2008). A plasma can also be regarded as an efficient
tool for generating energetic UV radiation and reactive
plasma species like O, O+,O2+ OH, H2O2, O3, etc
(Kanazawa et al. 1988; Moisan et al. 2001; Laroussi,
M. 2005; Morgan et al. 2009). Atmospheric pressure

glow discharge (APGD) appears as an attractive


solution to realize non-thermal atmospheric pressure
plasma suitable for different varieties of plasma
application including surface treatment of polymers
and textiles (Kanazwa et al. 1987; Eliasson, B. and
Kogelschatz, U. 1991; Okazaki et al.1993;
Kogelschatz et al. 1997; Morgan et al. 2010).
Even though, recently studies were conducted using
Plasma onto textile materials. The use of Plasma was
mainly limited to the increase wettability properties of,
mostly, synthetic materials, achieving higher color hue
using various printing processes. Alzeer et al. 2014
studied the effect of the plasma on the treatment and
modification of the surface a printing properties of the
wool. Salem and Morgan (2014) surface of polyester
and polyamide fabric were modified by atmospheric
pressure glow discharge Plasma under different
operating conditions to improve the printability of the
fabric. As well the printability of ink-jet was increased
using surface plasma treatment upon intended textile
substrates. In 2012 Cheung et al. inspected color
fading of a reactive dye (C.I. Reactive Blue 19) dyed
textile fabric using atmospheric pressure plasma
(APP)treatment. Significant color-fading effect was
achieved, for comparison purpose, there active dyed
textile fabric was subjected to conventional enzymatic
color-fading process, and experimental results revealed
that the APP induced color-fading effect was
comparable with conventional enzymatic color-fading
process. Indigo dyed woven garments is expected to
act differently, when faded by APGD, to the reactive
dye used in that mentioned study.

2. Materials and Method


Characteristics of the tested fabric
Denim fabric has been picked out from the Egyptian
market, expected for the middle class of the clothing
market. The fabric is warp indigo dyed with white
weft yarns, twill 3/1 woven structure, 65% cotton and
35% polyester, yarn density 32x22 yarns/cm2 of
weight 309g/m2 and thickness 0.678mm.
Atmospheric pressure glow discharge (APGD)
The discharge cell shown in Fig.2 consists of two
metallic parallel square electrodes of 25x25 cm2, 1mm
gap space, separated by glass sheet through an O ring.
The ground electrode stands on Acrylic sheet with
inlet and out let opening for gas insertion and
exhaustion. High voltage AC transformer (0-10kV),
generates a 50 Hz sinusoidal voltage was used as a
power source for driving discharge. A limiting resistor
RL was used to limit the current and protect the AC
power supply. The textile sample stands on the ground
electrode in the gap space shown in Fig.1. The current
and voltage waveforms have been measured, using 100
MHz digital storage oscilloscope (GWinstek GDS810S 100MHz), through potential divider (1:1000)

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85

International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 5, Issue 2, February 2016

represented by resistor R1 and R2. The discharge


current was measured through 100 ohm resistance
R3connected between the ground electrode and the
ground.

Fig.2 Schematic diagram of APGD discharge cell


Fig.3 shows the current voltage waveform for
atmospheric glow discharge with oxygen as working
gas at gap space nearly 1 mm with applied voltage 7
kV and discharge current 3mA. It is shown that the
glow component is superimposed with a large number
of streamers which indicate that the discharge is a
glow like nature i.e. glow discharge superimposed with
filamentary discharge.

APGD treated Denim physical, mechanical and


durability Properties
In the current research physical properties, Thickness
and Weight were tested for all untreated and treated
samples. Mechanical property of bending length,
utilizing Fixed-angle flexometer of BS3356, were
investigated for all tested fabrics, illustrating drapeability of tailored garment. Color hue K/S, which
shows deepness in color, has been examined for all
plasma treated samples, E was calculated in
reference to the control untreated denim sample, using
the Optimatch 3100, ISO105-Jo1:1989. Finally, ATR
and SEM using Quanta FEG 250 were done
investigating surface change due to various conditions
of plasma treatments. Burker VERTEX 70 FTIR
spectrophotometer, spectra measured in spectral range
400-4000 cm-1 in Mid-IR region, with resolution 2cm-1
using ATR technique. Comparison was done between
those mentioned properties before and after plasma
treatments, exemplifying the influence of plasma
fadingout process onto denim fabric.
3. Results and Discussion
The FPO is devoted to the Oxygen APGD, while FPS
is for water vaporAPGD. Table 1 below shows the
obtained denim from plasma treatment either Oxygen
or Water vapor, illustrating the different duration and
power used.

Table 1: APGD duration and currents used


Untreated
APGD
Duration
Power

FPO1
O2
3min
3mA

FPO2
O2
5min
3mA

FPO3
O2
3min
10mA

FPO4
O2
5min
10mA

FPS5
H2O
3min
3mA

Weight g/m2 and Thickness mm


Weight in physics is the force that gravitation exerts
upon a body, equal to the mass of the body times the
local acceleration of gravity. While thickness is the
measure of the smallest dimension of a solid figure.
An average of three and five readings was calculated
for weight and thickness, alternatively. From the
charts above, weight and thickness varied for denim
washed fabric when using different APGD type, either
Oxygen or Water vapor, duration and power.

Fig. 4: Weight of APGD washed denim

FPS6
H2O
5min
3mA

FPS7
H2O
3min
10mA

FPS8
H2O
5min
10mA

Weight, in general, decreased by the increase of


current used for both Oxygen and Water Vapor, this
specifies the increase of etching effect caused by
plasma when used for denim color wash. In most
cases, an increase in weight started to appear when
time increased, which can be an indication for a
reverse action, or the re-layering of indigo when
APGD duration increased. This directs that to achieve
the optimum weight before and after treatment, lower
current should be utilized with the least duration,
Oxygen APGD washed denim showed higher loss in
weight compared to Water vaporAPGD washed
garments. In discussion, regarding weight loss, in line
with the resultant data of this research, during APP
(Atmospheric Pressure Plasma) treatment, the fiber
surface was subjected to localized ablation, and only
surface etching would be resulted. On the whole, APP
treatment introduces lower percentage weight loss; the
APP treatment affects only the surface of the material

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86

International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 5, Issue 2, February 2016

and no effect on the bulk properties of the materials


(Cheung et al. 2013).

Fig. 5: Thickness of APGD washed denim


From figures 4&5 above, thickness varied with a slight
value from control untreated denim; it seems that an
increase in thickness accompanied with a decrease in
weight, for Oxygen APGD, seen in FPO3&4. The
plasma treatment etched the indigo layers, causing
yarns to stretch out with a decrease in weight. Swollen
yarns of APGD, either Oxygen or water vapor,
directed to increase in thickness; for water vapor
APGD the increase in thickness followed by increase
in weight, due to absorbed water molecules causing
yarns to be heavier. In general, APGD treated denim
washed garments can suffer a difference in weight and
thickness, when compared to unwashed garments.
Color Hue K/S and E of faded denim
K/S was considered for indigo at 400-435 nm, while
E was obtained using the daylight, a is a good
indicator for indigo, as it indicates the red-green
difference, nevertheless, E was considered into this
paper. It is noted that Plasma treated fabric have a
reduction in a value, which indicates that fabric will
turn greener than the untreated fabric (Kan et al. 2011).
As a general rule, if there is a total color difference of
E equal to 0.2 between two samples, these samples
can be considered visually different (Mercer H 2014).
The less K/S the more fading observed, which is clear
into the APGD Oxygen, compared to APGD Air; the
reason is that during the Plasma treatment, the oxygen
plasma would oxidize the dyes in the fabric surface
leading to a color-fading effect (Ghoranneviss et al.
2006).

color difference human eye can see, any E higher


than 1 is noticeable. However a study by Mahy et al.
1994 assessed a just noticeable difference of 2.3 E.
From figure above E showed variations in resultant
data, the highest shows the biggest difference when
compared to the control untreated sample, on another
words the higher E indicates a higher fading for the
denim garments. All plasma faded denim samples
ranged between 2 and 4. The most influencing factor
was APGD type, where all Oxygen treated samples
gave higher E between 3 and 4, on the other hand, all
treated APGD Water vapor obtained a less fading
effect of E less than 3. The higher the current used
the higher denim fading obtained, where 3mA gave
less E values compared to 10mA, for both Oxygen
and Water vapor APGD. For the least current used
3mA, either Oxygen or Water vapor, little fading took
place increased by increasing duration from 3min to
5min. The highest current used 10mA showed better
fading at 3min with increasing duration 5min E
started to decrease once more, this appeared for both
Oxygen and Water vapor APGD. FPO3 gave the
highest value of E 4, this was Oxygen APGD at
10mA for 3min duration, showing the best noticeable
fading effect for indigo dyed denim garments. During
the Plasma treatment, thermal oxidation effect may
occur in the fabric surface leading to certain degree of
yellowness (Kan et al. 2011).

Fig.7 E of APGD washed denim


Bending Rigidity
Bending length is an indicator, in most cases, for
drape-ability of a two dimensional textile material
when tailored into the three dimensional piece of
garment. Bending length was obtained in this research
for all untreated and APGD washed denim samples.

Fig.6 K/S of APGD washed denim

Fig.8 Warp Bending length cm of APGD washed


denim

E is the color change a number that represents the


distance between two colors; a E of 1 is the smallest

Untreated sample, in the warp direction, obtained


similar values for the Oxygen and Water vapor APGD

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87

International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 5, Issue 2, February 2016

at highest current 10mA and longest duration of 5min,


this is shown in FPO4 and FPS8 respectively. In
contrast, the lowest APGD Oxygen and Water vapor
for denim washed samples, showed much higher
bending length and by turn bending stiffness shown
from figure above at FPO1 and FPS5 respectively.
The more the current, duration or both, the less
stiffness the fabric obtained appearing in decreasing
bending length for FPO2,3&4 as well as FPS6,7&8.
Only warp bending length is considered, in this
research, as to clarify the effect of APGD onto the
indigo dyed cotton yarns.
The higher the current and duration of APGD washing
denim, either Oxygen or Water vapor, the more stable
bending length and by turn drape-ability this should
give to the assembled garment.
ATC Results
The resultant data showed no significance of
generating new groups. In this research, ATR was
applied for the untreated sample, FPO3 as the highest
difference in E for APGD Oxygen treatment, while
FPS7 showed the highest E for the APGD Water
vapor treated samples. Both FPO3 and FPS7 treated at
10mA for 3mins.
The results showed APGD
treatment on indigo dyed cotton warp fabric did not
affect the chemical structure of tested fabric, neither by
adding Oxygen nor Water vapor. The difference in
K/S and shown in E should be due to mechanical
effect upon indigo dye causing cracks within the dying
layer as shown in the SEM follows.

Frequencies 1673 cm-1 and 764cm-1 respectively.


1624 cm-1 and 1550cm-1 shows again both the NH2
primary and NH secondary Amide groups bend. As
well, 1297cm-1 C=O carbonyl group stretching in
figure above. Often, the frequency ranges for the
different classes of carbonyl compound overlap,
leading to the carbonyl frequency alone is not
sufficient to characterize the functional group, which is
why, spectral information of the other component
functional group is used for characterization (Coats J.
2000); as the case of indigo dye detected into this
study.
The weft polyester yarns are represented through the
ester group at 1732cm-1; Ester functional group C-OC ranges between 1750 and 1725 cm-1 (Coats J. 2000).
1030 cm-1 C-O primary alcohol stretch, 635cm-1 and
1366 cm-1 O-H hydroxyl group bends, 2920cm-1 C-H
stretching and 3330 cm-1 O-H hydroxyl group broad
stretch is seen from figure above, showing the warp
cellulose yarns.
From the results above, the itching effect of APGD
either O2 or Water vapor was evident without any
chemical change into the tested denim samples. Even
though, fading effect took place showed in the E
values obtained.
SEM Results
SEM results show the effect of plasma on the
morphology of Cotton/PES indigo dyed denim fabric.
Table 2: SEM of Untreated and Oxygen treated denim
at 3000X magnification
Untreated
Oxygen Plasma Treated

Fig.10 ATR spectrum of denim a- untreated sample, bOxygenFPO3 10mA for 3min, c- Water vaporFPS7
10mA for 3min.
Both C=O carbonyl group and N-H Amide group are
the functional groups identifying Indigo dye. In the
Figure above, primary amide NH2and secondary amide
NH groups are observed, indicating the presence of
indigo dye within tested fabric, these are at

In figures of table 2 above, the indigo dye clusters are


seen on surface of denim untreated fabric, while
atmospheric plasma contributed to the removal of
excess indigo giving a fading effect, with burnt surface
shown as cracks within plasma treated fibers. The
figures show the control untreated denim sample, and
the best faded APGD O2 sample.More SEM photos are
observed in Figures11, showing the effect of O2 APGD
and Water vaporAPGD, as well the different current
values and duration of plasma treatments, in the
process of indigo dyed denim wash.
FC, control untreated sample, shows the layers of
indigo dye appears on top of unwashed sample. FPO1,
3mA for 3min, Oxygen Plasma led to a very good
removal of indigo layers, leaving the warp yarns fully
covered with the deep blue indigo dye; a slight denim

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International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 5, Issue 2, February 2016

wash appears. With E equals 3.11. FPO3, 10mA for


3min, Stiffer look for warp yarns, with flattened fibers,
and with cracks within indigo causing the maximum
denim wash into this study. This is obtained using
Oxygen plasma at highest current and least duration.
E gave the highest value, in this study, of 4.FPO4,

10mA for 5min, the more time, oxygen plasma


treatment, directed to the accumulation of the indigo
dye once more on top of treated sample, still cracks
appear. Generally, plasma can bring out two types of
interactions with the surface Hsieh (2001).

Fig.11 SEM of various tested samples; a. untreated sample, b. c. &d. are Oxygen APGD washed denim, while e. f.
&g. are Water vapor APGD washed denim
The first type includes chain scission on the surface
which results in surface etching, cleaning, or
activation. The second type of interaction refers to
plasma induce polymerization or grafting. The latter is
obtained using non-polymerizing gases like helium,
argon, oxygen, air, and nitrogen (Kiran Kale, H., and
Desai, AN. 2011). In this research, form ART results
on no change into chemical active groups showing just
surface etching, cleaning or activation taking place
onto the denim APGD Oxygen and water vapor treated
samples. With E lowered slightly to 3.77. FPS5,
3mA for 3min, indigo layers are shown into the SEM,
with the least E value of 2.04, a quiet big difference
in shade in comparison to Oxygen PPT at the same
conditions of current and duration FPO1. FPS7, 10mA
for 3min, less indigo layers appear, when compared to
the FPS5, fibers are shown with more inter yarns,
showing the engraving effect of Water vapor plasma.
E got the maximum Water vapor APGD value of
2.72.FPS8, 10mA for 5min, as in FPO4, the longer the
Water vapor plasma duration than more accumulation
resulted for indigo dye on top of treated sample. The
cracks are lessened in comparison to FPS7 with the
same current and fewer duration. E is narrowed to
2.39.
Plasma faded denim, using O2, steered to a better
fading effect, when compared to Water vapor
atmospheric plasma. From resultant data, the increase
of current increases color differences represented
through E. While the time added in all plasma
treatments, led to a decrease in color differences, a
mechanical reverse treatment should have been

manipulated, so that the plasma atmosphere etching


effect stops and a layering effect took place. The
highest color fading observed into sample FPO3, with
E value of 4 in relevance to the APGD untreated
denim sample, where O2 plasma took place at a
maximum power, used in this study of 10mA. On the
other hand, the time for that particular sample FPO3
was the least which is 3mins.
Plasma is expected to have been mechanically etching
the surface of warp indigo dyed yarns, presence of O2,
when compared to APGD Water vapor, increased this
mechanical action without any chemical influence onto
APGD denim sample.

4. Conclusion
Washed denim is a desirable look in a garment that is
mostly time consuming and polluting process.
Atmospheric pressure plasma APGD is an
environmentally friendly and cheap process. In order
to substitute conventional fading such as stone, super
stone, enzyme and stone bleach, in this study, APGD
was examined, utilizing both Oxygen and Water vapor,
for its efficiency to denim wash. A woven
cotton/polyester twill indigo dyed denim was treated
using different AAP current and duration, a number of
eight different samples were obtained. Plasma is
expected to have been mechanically etching the
surface of warp indigo dyed yarns, APGD oxygen,
when compared to Water vaporAPGD, increased this
mechanical action without any chemical influence onto
APGD denim sample, as noted from the ATR charts.
SEM showed the engraved layers of indigo dyes,

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International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 5, Issue 2, February 2016

compared to control untreated sample. E, physical,


mechanical and durability properties varied for tested
APGD washed denim samples, in comparison to
untreated control sample. The optimum denim wash
was for oxygen APGD highest current and least
duration, where E was maximum was highest value.

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