Thesis Muhammad Tanveer

Graphene coated yarns and their knitted structures for smart textile
applications
A thesis submitted by
Muhammad Tanveer
(16-NTU-6012)
In partial fulfillment of the requirements for the degree of
Master of Science
in
Advanced Materials Engineering
Faculty of Engineering & Technology
National Textile University, Faisalabad

Aug- 2020
1
DEDICATION
This modest effort is dedicated to my

Family
&
Teachers
ii
CERTIFICATE
National Textile University, Faisalabad
This thesis, carried out and written by Mr. Muhammad Tanveer under the direction of his
supervisors and approved by all the members of thesis committee, has been presented to and
accepted by the Dean, Faculty of Engineering & Technology, in fulfillment of the
requirement of the degree of Master of Science in Advanced Materials Engineering.
Co-Supervisor Supervisor
Internal Examiner External Examiner
Director, Postgraduate Dean, Faculty of Engineering

Studies & Research & Technology
Date:
iii
ACKNOWLEDGEMENT
All praises are for Allah Almighty who always guided and helped me all the way through my
life. He blessed me with an ability to learn and expand the spectrum of my knowledge &
wisdom. Efforts to accomplish this milestone could not be possible without His countless
blessings & guiding principles taught by my Prophet Muhammad PBUH.
My parents, being the inspirational beacons & supporting hands, at all times encouraged me to
keep on learning whatever the circumstances would be. They spent golden years of their lives
for my upbringing, growth, and development. They stood by me in every situation & credit of
my every accomplishment certainly goes to them. I am deeply indebted for their affection,
prayers, and support. Continuous encouragement & support my wife, brothers (Muhammad
Saeed Tahir, Muhammad Munir), and my sister always helped me to move on to achieve the
ultimate of my personal & career goals.
I would like to extend deepest sense of gratitude to my supervisor Prof. Dr. Tanveer Hussain,
co-supervisor Dr. M. Bilal Qadir, and Dr. Ahsan Nazir for consistent supervision &
support during this research project.
May Allah bless all of them with good health and a happy life, Aameen.
Muhammad Tanveer
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TABLE OF CONTENTS
DEDICATION .......................................................................................................................... ii
CERTIFICATE ........................................................................................................................ iii
ACKNOWLEDGEMENT ....................................................................................................... iv
TABLE OF CONTENTS .......................................................................................................... v
LIST OF FIGURES ............................................................................................................... viii
LIST OF TABLES .................................................................................................................... x
ABSTRACT ............................................................................................................................. xi
Chapter 1 Introduction .............................................................................................................. 1
1.1. Background .................................................................................................................... 1
1.1.1. Mechanism of smart textiles ................................................................................... 1
1.1.2. Graphene and its properties .................................................................................... 2
1.2. Applications of graphene ............................................................................................... 3
1.2.1. Applications of graphene in general ....................................................................... 3
1.2.2. Applications of graphene in textiles........................................................................ 4
1.2.3. Applications of smart textiles ................................................................................. 4
1.3. Literature review ............................................................................................................ 6
1.3.1. Recent trends in smart textiles ................................................................................ 6
1.3.2. Recent trends in graphene-based textiles ................................................................ 8
1.3.3. Graphene oxide and its reduction.......................................................................... 11
1.4. Research gap ................................................................................................................ 12
1.5. Research problem ........................................................................................................ 12
1.5.1. Statement of the research problem ........................................................................ 12
1.5.2. Significance of the research problem .................................................................... 12
1.6. Research aims & objectives ......................................................................................... 12
1.6.1. Overall aim ............................................................................................................ 12
1.6.2. Specific research objectives .................................................................................. 13
1.6.3. Research hypotheses ............................................................................................. 13
1.6.4. Scope of the project............................................................................................... 13
Chapter 2 Materials and methods ........................................................................................... 14
2.1. Yarns ............................................................................................................................ 14
v
2.2. Chemicals..................................................................................................................... 14
2.3. Equipment .................................................................................................................... 14
2.4. Methods ....................................................................................................................... 15
2.4.1. Experimental factors and their levels .................................................................... 15
2.4.2. Response variables ................................................................................................ 16
2.5. Sample preparation methods ........................................................................................ 18
2.5.1. Preparation of graphene oxide (GO) dispersion ................................................... 18
2.5.2. Preparation of GO coated yarn samples ................................................................ 18
2.5.3. Reduction of GO coated yarn samples .................................................................. 18
2.5.4. Preparation of fabric samples ................................................................................ 18
2.6. Testing methods ........................................................................................................... 19
2.6.1. Particle size analysis ............................................................................................. 19
2.6.2. Yarn tenacity ......................................................................................................... 20
2.6.3. Functional group analysis ..................................................................................... 21
2.6.4. Yarn morphology .................................................................................................. 21
2.6.5. Fabric surface resistivity and vertical resistance................................................... 22
2.6.7. Fabric thermal resistance ...................................................................................... 23
2.6.8. Fabric thermal conductivity .................................................................................. 23
2.6.9. Fabric moisture management ................................................................................ 23
2.6.9. Ultraviolet protection testing ................................................................................ 24
Chapter 3 Results and discussion ............................................................................................ 25
3.1 Characterization of graphene oxide (dispersion) .......................................................... 25
3.1.1. Graphene oxide elemental analysis ....................................................................... 25
3.1.2. Zeta sizer analysis ................................................................................................. 26
3.2. Chemical interaction of GO with textiles .................................................................... 26
3.2.1. Chemical interaction of GO with cotton ............................................................... 26
3.2.2. Chemical interaction of GO with polyester .......................................................... 27
3.2.3. Chemical interaction of GO with nylon ................................................................ 28
3.3. Yarn and fabric testing ................................................................................................. 28
3.3.1. Yarn linear density, CV% and, tensile properties ................................................. 28
3.3.2. Ultraviolet protection factor (UPF) ....................................................................... 31
3.3.3. Measurement of surface resistivity and vertical resistance ................................... 36
3.3.4. Thermal resistance and thermal conductivity ....................................................... 38
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3.3.5. Liquid moisture management properties (OMMC) .............................................. 40
3.4 Analytical testing .......................................................................................................... 42
3.4.1. Fourier transform infrared spectrometer (FTIR) analysis ..................................... 42
3.4.2. Scanning electron microscope (SEM) analysis ..................................................... 45
3.5. Analysis of variance: ANOVA and main effect plots ................................................. 47
3.5.1 Analysis of variance of ultraviolet protection factor (UPF) .................................. 47
3.5.2. Analysis of variance of surface resistivity ............................................................ 48
3.5.3 Analysis of variance of vertical resistance ............................................................. 49
3.5.3 Analysis of variance of thermal resistance ............................................................ 50
3.5.3 Analysis of variance of thermal conductivity ........................................................ 51
3.5.3 Analysis of variance of liquid moisture management (OMMC) ........................... 52
Chapter 4 Conclusion and Future Recommendations ............................................................. 54
4.1 Conclusion .............................................................................................................. 54
4.2 Future Research Recommendations ........................................................................ 55
References ............................................................................................................................... 56
vii
LIST OF FIGURES
Figure 1: Working mechanism of smart textiles [2]. ................................................................ 2

Figure 2: Graphene oxide Structure (Left) and reduced graphene oxide (Right) [4]. .............. 3
Figure 3: Smart textiles applications in health care [7]. ........................................................... 5
Figure 4: Smart textiles applications in military and defense [7]. ............................................ 6
Figure 5: Smart textiles applications in fashion, entertainment, and sportswear [7]. ............... 6
Figure 6: (a) Graphene-based fibers in the form of knitted fabric, (b) graphene-based fibers in
round shape [13], (c) a knitted structure with a combination of cotton and graphene-based
fibers, (d) structure developed using graphene-based fibers [14]. ............................................ 8
Figure 7 TEM based Illustration of a graphene oxide nano-sheet [16]. ................................... 9
Figure 8. Scanning electron microscopy of graphene oxide coated cotton fiber. (a) left side is
the illustration of fiber as a whole and (b) right side is the enlarged view of graphene oxide on
the surface [16]. ...................................................................................................................... 10
Figure 9: Socks knitting machine. .......................................................................................... 19
Figure 10: Zetasizer Nano ZS. ................................................................................................ 20
Figure 11: Tensorapid 5 as single yarn strength tester. .......................................................... 20
Figure 12: PerkinElmer spectrum two-Fourier transform infrared spectrometer. .................. 21
Figure 13: Quanta 250 FEI scanning electron microscope. .................................................... 22
Figure 14: Static Lab (static electricity tester). ....................................................................... 22
Figure 15: Sweating guard hot plate. ...................................................................................... 23
Figure 16: Moisture management tester. ................................................................................ 24
Figure 17: Labshere UV-2000S ultraviolet protection tester. ................................................. 24
Figure 18: Zeta size analysis of GO. ....................................................................................... 26
Figure 19: Chemical interaction of GO with cotton during reduction [35]. ........................... 27
Figure 20: Chemical interaction of GO with polyester during reduction [36]. ...................... 27
Figure 21: Chemical interaction of GO with polyester during reduction [37]. ...................... 28
Figure 22: Linear yarn densities of cotton yarns. ................................................................... 29
Figure 23: Linear yarn densities of polyester yarns. ............................................................... 29
Figure 24: Linear density of nylon yarns. ............................................................................... 30
Figure 25: CV% of cotton, polyester, and nylon. ................................................................... 30
Figure 26: Tenacity for cotton samples and a decreasing trend for polyester and nylon samples.
................................................................................................................................................. 31
Figure 27: Ultraviolet protection factor (UPF) of cotton, nylon, and polyester. .................... 32
Figure 28: UVA blocking of reduced GO coated fabrics. ...................................................... 33
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Figure 29: UVB blocking values. ........................................................................................... 34
Figure 30: UVA transmittance values..................................................................................... 35
Figure 31: UVB transmittance values. .................................................................................... 36
Figure 32: Surface resistivity and vertical resistance of cotton. ............................................. 37
Figure 33: Surface resistivity and vertical resistance of polyester. ........................................ 37
Figure 34: Surface resistivity and vertical resistance in nylon samples. ................................ 38
Figure 35: Thermal resistance and thermal conductivity values of cotton. ............................ 39
Figure 36: Thermal resistance and thermal conductivity values of polyester. ....................... 39
Figure 37: Thermal resistance and thermal conductivity values of nylon. ............................. 40
Figure38 Liquid moisture management properties of cotton (OMMC). ................................ 41
Figure 39: Liquid moisture management properties of polyester (ommc). ............................ 41
Figure 40: Liquid moisture management properties of nylon (OMMC). ............................... 42
Figure 41: FTIR analysis of cotton, GO-coated cotton, and reduced-GO-coated cotton. ...... 43
Figure 42: FTIR analysis of untreated polyester with GO-coated and reduced-GO-coated
polyester. ................................................................................................................................. 44
Figure 43: FTIR analysis of untreated nylon, GO-coated nylon, and reduced-GO-coated nylon.
................................................................................................................................................. 45
Figure 44: SEM images of untreated cotton, polyester, and nylon yarns. .............................. 46
Figure 45: SEM images of reduced GO treated/coated cotton (C6), polyester (P6) and, nylon
(N6) yarn. ................................................................................................................................ 46
Figure 46: Main effects plot for the ultraviolet protection factor. .......................................... 48
Figure 47. Main effects plot for surface resistivity (Ω). ......................................................... 49
Figure 48: Main effects plot for vertical resistance (Ω). ......................................................... 50
Figure 49: Main effects plot for thermal resistance (m2K/W). ............................................... 51
Figure 50: Main effects plot for thermal conductivity (W.m-1.K-1) ........................................ 52
Figure 51: Main effects plot for liquid moisture management (OMMC). .............................. 53
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LIST OF TABLES
Table 1: Specifications of yarns. ............................................................................................. 14

Table 2: Specifications of chemicals. ..................................................................................... 14
Table 3: Equipment for sample development. ........................................................................ 15
Table 4: Equipment for testing. .............................................................................................. 15
Table 5: Experimental factors and their levels ....................................................................... 16
Table 6: Response variables.................................................................................................... 16
Table 7: Design of experiment ................................................................................................ 17
Table 8: GO specifications...................................................................................................... 25
Table 9: Elemental analysis. ................................................................................................... 25
Table 10. General linear model for ultraviolet protection factor (UPF) versus main yarn (Tex),
concentration, no. coating cycles). .......................................................................................... 47
Table 11. General linear model: surface resistivity versus main yarn (Tex), concentration, no.
coating cycles). ....................................................................................................................... 48
Table 12. General linear model: vertical resistance versus main yarn (Tex), concentration, no.
coating cycles) ........................................................................................................................ 49
Table 13. General linear model: thermal resistance versus main yarn (Tex), concentration, no.
coating cycles .......................................................................................................................... 50
Table 14. General linear model: Thermal conductivity versus main yarn (Tex), concentration,
no. coating cycles. ................................................................................................................... 51
Table 15. General linear model: liquid moisture versus main yarn (Tex), concentration, no.
coating cycles .......................................................................................................................... 52
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ABSTRACT
The aim of this research is to develop yarns with high strength, electrical conductivity, and
thermal conductivity and to use these yarns in knitting structures to analyze their impact on the
electrical and comfort properties of end garments. In this study, 18 different graphene oxide
(GO) coated yarn samples are developed; 6 each of cotton, polyester and nylon. Two levels of
concentration (1 Wt. % and 2 Wt. %) and three levels of coating cycles (1, 2 & 3) are used to
coat the yarns. These coated yarn samples are then treated with sodium hydrosulfite (Na2S2O4)
to get reduced graphene oxide yarns. Knitted structures of all 18 yarns are developed on 144
needle circular socks knitting machine. Yarn count, tenacity, CV%, fabric thermal & electrical
conductivity, ultraviolet protection and electrical properties are investigated. Qualitative and
quantitative investigation of electrical, thermal, UV, and physical properties of graphene-
coated samples is done. The level of the coatings is estimated by scanning electron microscope.
To check the level of reduction of GO, FTIR analysis is done. Yarn linear densities of cotton
from 29.23 Tex to 29.86 Tex, polyester from 35.22 Tex to 36.88 Tex and nylon from 31.76
Tex to 33.17 Tex are increased. The coefficient of variation (CV %) of yarns is increased from
0.42 to 1.4 considering all the samples. The tenacity of cotton is increased from 16.69 cN/tex
to 17.44 cN/tex while in the case of nylon and polyester yarns, it is reduced from 34.92 cN/tex
to 30.49 cN/tex and 34.89 cN/tex to 30.67 cN/tex respectively. Ultraviolet protection factor
(UPF) values of cotton, nylon and polyester are increased from 97.94 to 1772, 177 to 1971 and
107 to 1991 respectively. Surface resistivity and vertical resistance values of cotton, polyester
and nylon are decreased significantly with increase in GO concentration and number of coating
cycles. The thermal conductivity of cotton, nylon and polyester is significantly increased with
the increase in concentration of reduced graphene oxide. All these factors lead to GO as a
prominent material to be utilized in smart textile applications.
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Chapter 1
Introduction
1.1. Background
“Smart Textiles” are defined as the functional textiles that can respond to external
environmental factors like temperature, pressure, voltage, light, heat, magnetism, etc. for
protection, communication, monitoring, health care, enhanced performance, comfort, fashion,
and decoration. Advanced textiles utilize materials like fibers, yarns, and fabrics in individual
form or as a product of two or three substrates along with specialized electronic components.
Such advance products can have a better response to environmental stimuli so when
conventional textiles are incorporated with advanced electronics, they provide a roadmap for
the development of specialized and delicate materials. Such textile materials can lead to the
development of flexible fabrics like typical wearable textiles providing all benefits of modern
electronics. Sometimes, these look just like ordinary textile fabrics but have specialized
applications.
Smart textiles can be classified as “Passive E-Textiles”, “Active E-Textiles” and “Ultra
Performance E-Textiles”. The passive category includes textiles which rather than changing
themselves against environmental changes remain the same but may provide additional
benefits like bullet resistance, anti-bacterial activity, etc. Active category includes the smart
textiles that can automatically respond to the environmental changes. Few examples are
thermoregulating, heat-storing, electrically, and thermally resistant fabrics. The Ultra-smart
category can be defined as intelligent textiles that can respond to the changing environmental
factors and can change themselves in a pre-determined way to perform a delicate function.
This category utilizes multi-disciplinary scientific fields along with conventional textiles
leading to the successful induction of smart technologies in every aspect of life. Newly
developed specialized materials i.e. fibers, fabrics and delicate electronic devices have
revolutionized the world by providing specialized smart textiles that can be utilized as ordinary
wearable garments as well [1].
1.1.1. Mechanism of smart textiles

Energy storage, flow, conversion, and the flexibility of textiles are the key features required in
smart textiles. E-textiles can utilize textile materials like cotton, polyester, and nylon as a
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substrate for incorporating electronic features. Three mechanisms are of vital importance and
are always the part of smart textiles; 1-Sensing, 2-actuation and 3-controlling. Smart textiles
utilize specialized materials, electronic, and communication components in order to respond
to an external environmental factor. Energy conversion or transformation is involved when an
external factor acts on a smart textile substrate. Such a process leads to response as far as input
is processed and is analyzed. Smart textiles work on the basis of input energy that is required
to bring the materials under specific changes. When external environmental factors act on it,
smart textiles create resistance, or they can absorb such stimuli. The working mechanism of
smart textiles is shown in Figure 1 [2].
Figure 1: Working mechanism of smart textiles [2].
Electronic functionality is the top desirable feature in textiles along with comfort-ability
features like flexibility, feel, and wear-ability. Incorporating such functional properties,
sometimes, comfort properties are compromised leading to stiff wear. When fabric’s feel and
wear-ability are not up to the level of comfort, this leads to the dissatisfaction of the wearer.
The main challenge to improve comfort is to control stiffness but the first step is to test stiffness
using some standard test method. To improve the comfort level and to reduce stiffness, a right
testing method is required [3]. conectivity is missing
1.1.2. Graphene and its properties
Why graphene, compared with what it is better
Graphene can be produced by the reduction of graphene-oxide by following a standard
reduction reaction. Graphene-oxide can be synthesized by applying strong oxidizing agents on
graphite powder. Graphene-oxide has a number of functional groups like OH, CO, and COH
that make joint with a basic carbon structure. Graphene-oxide is a poor conductor for electrons
and can be utilized to make dispersion with water. When reduced, graphene-oxide gets many
other functional groups like OH and has excellent electrical properties. Reduction through
2
chemicals is a cost-effective method to reduce the graphene-oxide [4]. Figure 2 is the
illustration of graphene-oxide (left) and a structure of reduced graphene oxide (right).
Figure 2: Graphene oxide structure (left) and reduced graphene oxide (right) [4].
Graphene is a material with extraordinary strength, stiffness, thermal conductivity, and

electrical conductivity. Graphene is a single-layered graphite structure. The high conductivity
and lowest resistivity of graphene at room temperature is the key attention area. It has a
chemically stable structure that is highly sensitive to electrical inputs due to its single layered
formation. Graphene has excellent UV protection, antimicrobial, thermal & electrically
conductive, and superior mechanical properties. Utilizing UV protection, mechanical/tensile,
antimicrobial and thermal properties of graphene can bring important outcomes in the form of
health safety, better performance and superior comfort properties for sportswear, health care
and many more [5].
1.2. Applications of graphene
1.2.1. Applications of graphene in general

The electronic features and functionalities of graphene are well known. The strength,
conductivity, and UV protection properties make it one of the most feasible materials for
electronics. Electrons flow within the monolayered atomic structure of graphene is far better
than any other material as it makes it more sensitive and approachable to the control. The
quality of electronic flow is excellent as electrons do not scatter and move longer distances
without deviations. The uniqueness of the electronic properties of graphene has made it more
attractive than any other electronic material. Being lightweight and super strong, graphene is
being used in modern electronics, electrical circuits with minimum resistivity values, energy
harvesting, medicine, chemistry and in improving industrial processes. Due to its extraordinary
3
electrical properties, graphene has been used in batteries and solar cells to improve their
efficiencies [4, 5].
1.2.2. Applications of graphene in textiles
Graphene is applied to different textile substrates for surface modification to get its
applications in textiles. Textile applications include; transparent coatings and circuits to
develop electrical conductivity, conducting inks and coatings, UV protection coatings, super-
capacitors, thermal conductivity, sensors, tires, and water filtration systems. Graphene coating
on different types of substrates like polypropylene, nylon, and polyethylene made by different
extrusion methods is done to get some conducting materials for textile applications. The effect
of shape and size of fibers is also considered to check the impact and quality of graphene
coating. The electrical conductivity of graphene-coated fibers has been assessed in different
situations i.e. in bending and flat fiber positions. Effect of change in surface morphology of
fibers can change in graphene coating quality and hence can lead to change in sheet resistance,
transmittance values, and intensity [6].
1.2.3. Applications of smart textiles
Conductive features in textiles have made it possible to develop lightweight, flexible wearable
electronic textiles with specialized featured like power and data flow for many applications
like sports, medicine, health care, computing, and much more.
Health-related wearable monitoring systems are replacing conventional electronic devices and
are more accurate due to the quality of electronic flow in materials that are integrated at the
nanometer scale. Such monitoring devices can perform their functions during routine activities.
need to explain more abt fig 3
Figure 3 is an example of health care application of smart textiles. The development of UV
protection textiles, anti-bacterial, and biosensing systems are the key examples of recent
developments. Electrical conductivity features in textiles have opened new doors for the
development of human-friendly wearable electronics that will be more energy-efficient,
accurate and long-lasting. The latest developed devices include heart monitoring, blood
pressure measuring and monitoring, diabetic monitoring and neuro sensing devices [7].
4
Figure 3: Smart textiles applications in health care [7].
Smart textiles are also used for defense purposes including protection and safety as the most
important factors. The second important factor for military and defense personnel is
communication that needs delicate wearable devices to get timely information. In addition to
this, there are a variety of smart textiles that help to enhance the performance and working
efficiency of the wearer. In such areas where life threats increase due to hazardous impacts of
external factors like toxic fumes and gases, smart textiles are utilized to cope with all such
situations. Smart textiles equipped with communication components help for a quick response
against any situation. Figure 4 shows a specific communication system in smart textiles for the
military.
Smart materials in the form of fibers, yarns, chemical coatings, and finishes utilize electronic
circuits that are removable according to requirement. Such smart textiles are intensively used
for the purpose of fashion, sportswear, and many other fields. Sports and athletic activity can
be enhanced using smart textiles. This category helps in monitoring health, performance and
activity time. Specialized garments with better moisture management properties can be used
for improved performance. During intense sports activities, muscular vibrations can be
controlled using specialized materials. Specialized shoes and garments with tracking devices
and performance monitoring components are being used in sports events. Figure 5 shows
fashion and sportswear smart textile applications [7].
5
Need more explanation of figure 4
Figure 4: Smart textiles applications in military and defense [7].
Figure 5: Smart textiles applications in fashion, entertainment, and sportswear [7].
1.3. Literature review
1.3.1. Recent trends in smart textiles

The thermal conductivity of some specialized nanomaterials like carbon-based graphene and
carbon nanotubes is extraordinary. Such materials have displayed excellent thermal
conductivity values. Graphene has much higher values of thermal conductivity as compared to
carbon nanotubes. Many other materials have been used to enhance thermal conductivity like
Boron nitride. This is widely used to develop conducting materials for industrial and
engineering applications. The application of carbon nanotubes on the cotton substrate has been
reported with a rise in thermal conductive values by more than 150%. Due to nano-scale
coating, air-permeability reduced, and wetting time increased. Although all these materials
showed excellent thermal conductivity values when applied individually but the thermally
conductive coatings showed extraordinary results when uded on composites. The thermal
spell mistake
6
conductivity of the woven Cotton fabric was enhanced through the coating of a composite of
multiwall carbon nanotubes/graphene and multiwall carbon nanotubes/boron nitride. The best
results were obtained through graphene. Keeping the air permeability constant, graphene was
the best thermal conductive material among these materials. A reduction in air-permeability
was assessed against graphene-coated material while other coatings showed better results of
air-permeability leading to the highest thermal conductivity values of graphene-coated fabric
[8].
Boron Nitride had better thermal conductivity values than “Multiwall Carbon Nano Tubes”.
An important fact about the difference in thermal conductivity values was observed.
Theoretical values differ from the real-time achieved values when used in the form of
composites due to weak “van der Waals” forces. Considering hydrophilic property, it was
observed that graphene and “MWCNT” coatings showed better results as compared to Boron
Nitride coating that appeared with a hydrophobic surface. “MWCNT” had superior results of
air-permeability as compared to other coatings. The effect of these coatings on the fabric shade
was also assessed [9].
The thermal conductivity of knitted cotton fabric was enhanced by coating it with graphene-
oxide. The 1st comparison was drawn between the untreated fabric and graphene-oxide coated
fabric. Secondly, when the graphene-coated fabric was passed through different reducing
solutions, thermal conductivity was further improved [10]. The Super-hydrophobicity and
electrical conductivity of cotton fabric have been enhanced using graphene coating. Graphene-
oxide was coated first and then reduced to graphene using ascorbic acid. Shedding and water
contact angles were used to analyze hydrophobicity while resistivity was used to calculate
conductivity [11].
Research and development of novel materials like graphene fibers that are produced using the
wet spinning technique are very attractive. Incorporating nanometer scaled graphene with
different macro-level substrate materials has opened doors for the development of the modern
electronic and scientific revolution. The feasibility of the bulk level production of this fiber
has enabled researchers to work on various new applications. Numerous electronic applications
like robotic devices, capacitors, and actuating devices are excellent examples.
Graphene-based fibers are in their early stages of development and need theoretically proven
systems. There is a need to work on the mechanical area as well as to improve the conductivity
7
efficiency of graphene-based fibers. So far, the strength that is achieved in graphene-based
fibers is in a range of 0.64-0.66 GPa. The electrical conductivity and strength of these fibers
are still lower as compared to carbon-based fibers. For the delicate industrial utility of
graphene-based fibers, it is also important to improve mechanical strength [12].
To improve strength and mechanical performance, there are different approaches, such as to
incorporate nanoscale metallic wires with graphene-based fibers. Production of graphene-
based fibers is itself a big challenge. Graphene oxide is utilized to develop graphene-based
fibers with numerous uncertainties in their physical and chemical quality parameters. Such
parameters lead to the formulation of manufacturing process and explain end-product
properties. Mechanical strength varies with the varying size of graphene nanosheets. Figure 6
shows (a) Graphene-based fibers in the form of knitted fabric, (b) graphene-based fibers in
fibers, (d) structure developed using graphene-based fibers [14]. Current researches of
graphene-based fibers are based on new manufacturing techniques rather than focus on the end
product quality parameters. Production of wet spun graphene-based fibers can be enhanced if
practical grounds of these fibers are explored through coordination among researchers [13, 14].
(a) (b) (c) (d)
Figure 6: (a) Graphene-based fibers in the form of knitted fabric, (b) graphene-based fibers in
fibers, (d) structure developed using graphene-based fibers [14].
1.3.2. Recent trends in graphene-based textiles

A detailed working on electrical conductivity and electrical resistivity values of a graphene-
coated acrylic fabric was carried out based on temperature variations. Acrylic woven fabric
was coated with graphene oxide dispersion that was prepared from natural graphite using
“modified Hummers and Offeman method”. This graphene-coated fabric was then passed
through the aqueous solution (sodium hydrosulfite) to convert graphene-oxide to graphene
[15]. Many researchers have worked to enhance the electrical conductivity of textile materials
8
by coating graphene. The electrical conductivity of the graphene-coated fabric of cotton was
enhanced using the “dip and dry” method to immobilize graphene-oxide (GO) on cotton fabric.
Then this fabric was brought under various types of reducing agents to convert graphene-oxide
to graphene. The research reported Na2S2O4 as the best reducing agent leading to better
electrical conductivity as well as improved mechanical strength.
Cellulosic materials lose their stability with increasing temperature and tend to degrade. So,
producing graphene using high-temperature reduction of graphene oxide cellulosic coating is
not feasible. Further, due to the hydrophobic nature and unavailability of functional groups on
the graphene surface, adsorption is low hence lowering the quality of the end product. There
are some other limitations as well, like high prices and availability of reliable sources. Hence,
coating the cellulosic material with graphene oxide and then its reduction at a relatively lower
temperature is a more feasible method for a high quality of the graphene-coated cotton product.
To apply graphene on cellulosic materials, it needs to have some functional groups that are
more likely to make it water dispersible. Hummer’s technique was used to synthesize graphene
oxide in the form of two-dimensional structures with functional groups like OH, COOH, CO,
and COO [16]. The developed product was able to be dispersed in water, had an insulating
behavior and had a brownish shade. Figure 7 illustration (TEM) shows an amorphous graphene
oxide structure.
Figure 7 TEM based Illustration of a graphene oxide nano-sheet [16].
This method of producing graphene-coated cellulosic material was done in two processes. The
process is to apply graphene oxide on the cellulosic base using the “dip and dry” mechanism.
As graphene oxide and cellulose material have different types of functional groups, they create
an attraction for each other by creating bonding, i.e. Van der Waal attractions leading to a
uniform coating of graphene oxide on the cotton substrate. Different analytical techniques have
been used to characterize the coating. Figure 8 shows scanning electron microscope (SEM)
9
images of graphene oxide coated cotton fiber. (a) left side is illustration of fiber as a whole and
(b) right side is the deep down view of graphene oxide on the surface [16]. Amazingly, the
structural and surface nature of the cellulosic material was not altered due to the reason that
thickness of the graphene oxide nano-sheet was very thin, and it was uniform and
homogeneous through the fiber surface. Secondly, this coated fabric was passed through a
reduction mechanism to reduce graphene oxide. The electrical conductivity of this reduced
fabric was increased prominently [16].
Figure 8. Scanning electron microscopy of graphene oxide coated cotton fiber. (a) left side is
the illustration of fiber as a whole and (b) right side is the enlarged view of graphene oxide
on the surface [16].
The research revealed that uniform coating of graphene oxide on the cellulosic substrate was
observed using SEM. The reduction step was the critical area of focus, so different types of
reducing agents were used and their effect on electrical conductivity was assessed. Changes
in the color of coated cellulosic material were the identification of graphene oxide coating, its
reduction and application of graphene on the fabric. Cotton fabric with white as a generic color
was changed to brown shade after coating with graphene oxide and after the reduction process,
the color was changed to black [17]. The reduction of graphene oxide to graphene need to be
characterized and the most feasible indicator is electrical conductivity. Characterization
indicated that graphene oxide coated cellulosic material showed no electrical conductivity. The
reduction process of graphene oxide coated material leads to enhanced electrical conductivity
[18].
Different reducing agents in graphene coating on cellulosic material showed different electrical
conductivity values. Different reducing agents showed excellent electrical conductivity values
on graphene oxide coated cellulosic material. The mechanical strength of graphene oxide
coated cellulosic material, graphene-coated cellulosic material, and original cellulosic material
10
was characterized. Although few reducing agents had a negative effect on strength of cellulosic
material, however, Na2S2O4 showed no major change, so it was considered as the most suitable
reducing agent among a group of five reducing agents. It was deemed to be feasible for
industrial applications. Factors like concentration, reaction time, and a number of coating
cycles were studied [19].
1.3.3. Graphene oxide and its reduction

Graphene oxide contains various functional groups that play a significant role in its
applications [11]. After the introduction of graphene oxide in the 19th Century [20], technical
advancements in advanced materials have been observed. Graphene oxide is a structure in the
sheet form. Graphene oxide sheet exists in the layer by layer atomic structure with micrometer
level width and atomic level thickness. This amazing atomic structure makes it possible to be
used as a covering on any substance for its post applications. Major advantage of using
graphene oxide is its dispersible nature that is compatible with polar as well aqueous solvents
[21]. As compared to different carbon applications, graphene oxide is better suitable to make
the combination with other chemicals due to its highly dispersible nature. Graphene oxide can
be converted to Graphene using some reducing agent or through a heating mechanism.
Graphene having high electrical and thermal conductivity with a two-dimensional strong
mechanical structure is a leading high-performance material and can be used for unlimited
technical applications [21]. Graphite is an abundantly available material that can be converted
to graphene oxide using an exfoliation method or a conventional chemical mechanism.
Abundantly raw material availability makes this product cost-effective. This will cause a
revolution in technical and engineering areas [22-25]. Application areas of graphene are not
limited and are leading research focus of modern engineering and science [26]. Primary desire
to get highly efficient technical components can be fulfilled using a combination of micro-
level graphene structures and combining them using some chemical bonding techniques [27].
graphene oxide can be mixed with different compounds and after its reduction, this is converted
to graphene which is electrically conductive. The major challenge that was faced was to
develop a combination of graphene oxide layers without using any binder or chemical. Such
methods have been successfully developed and utilized [19]. Revolution in developing
transparent nanometric sheets to develop transparent electrical structures for advanced
applications has been done by reducing graphene oxide to achieve Graphene. Now, the major
challenge is to utilize graphene-based technical materials on an industrial scale despite the
11
availability of numerous methods to convert graphene oxide to Graphene. Graphene-based
structures were produced on an industrial scale using graphene oxide as a coating material.
Graphene oxide was tropically coated on the fabric using a simple old dyeing method. These
coated fabrics were then reduced to achieve a highly conductive surface for electrical as well
as thermal purposes [28].
1.4. Research gap
Graphene is not applied to conventional textile yarns in the form of coatings using oxidation-
reduction methods, and its effect on the electrical, mechanical, chemical, comfort and moisture
management properties of knitted garments is not analyzed up-till now.
1.5. Research problem
1.5.1. Statement of the research problem

Available conducting materials are stiff and are difficult to be executed when used as textile
raw material. It is challenging to use available electrically conductive yarns in knitting due to
the high stiffness and lower efficiency of its running on the machine. As a result, wastages
increase leading to difficulty in using an industrial scale.
1.5.2. Significance of the research problem
Cheaper electrical and thermal conductive flexible yarns are the need of today’s world to be
used in smart textile applications. Graphene has been extensively used in wearable textiles in
different forms. However, existing methods of its applications are costly, so it has limited
applications. The development of cost-effective conductive yarns through the conventional
coating and drying methods using graphene can lead to the production of smart textiles with
better efficiency and with less cost. During this study, firstly, graphene will be applied to
different textile yarns then these yarns will be used in weft circular knitted socks. Electrical,
mechanical, thermal, and moisture properties of socks will be analyzed.
1.6. Research aims & objectives
1.6.1. Overall aim

This research aims to develop yarns with high strength, electrical conductivity, and thermal
conductivity and to use these yarns in knitting structures to analyze their impact on the
electrical and comfort properties of end garment.
12
1.6.2. Specific research objectives
 To study the effect of graphene-oxide concentration and coating cycles on the tenacity of
cotton, polyester, and nylon yarns.
 To study the ultraviolet (UV) protection, thermal, electrical, and moisture management
properties of knitted socks made from cotton, polyester, and nylon yarns coated with
graphene oxide.
1.6.3. Research hypotheses
The reduction of graphene-oxide coated yarns can create strong bonding between the yarn
surface and graphene leading to the development of yarns with better electrical and thermal
conductivity and it will be more cost-effective as compared to available yarns in the market.
1.6.4. Scope of the project

Conventional textile materials like cotton, nylon, and polyester are readily available in
Pakistan, and this research would provide a platform for the development of cost-effective,
flexible, and human-friendly smart textile materials without adding extra resources. This
project can provide a basis for the development of flexible conductive yarns that would be used
in conventional as well as modern smart textiles with better electrical and thermal
conductivities.
13
Chapter 2
Materials and methods
2.1. Yarns
Specifications of yarns used are given in in Table 1.

Table 1: Specifications of yarns.
Tenacity
Sr. No. Yarn Use Supplier
(cN/tex)
1 29 Tex combed ring-spun cotton yarn 16.69 Main Yarn Interloop Ltd.
32 Tex textured twisted nylon with 24

2 34.89 Main Yarn Interloop Ltd.
filaments
35 Tex textured twisted polyester with

3 34.92 Main Yarn Interloop Ltd.
36 filaments
2.2. Chemicals
Specifications of the chemicals used are given in Table 2.

Table 2: Specifications of chemicals.
Sr. No. Material Grade Supplier
Graphene oxide water dispersion (1 Wt%, 2
1 Lab grade Graphenea
Wt%)
2 Sodium hydrosulfite (Na2S2O4) Lab grade Merck
3 Hydrochloric acid (HCl) Lab grade Merck
2.3. Equipment
2.3.1. Equipment for sample development

The equipment used for socks knitting, processing, and finishing are listed in Table 3.
14
Table 3: Equipment for sample development.
Sr. No Equipment Name Model Manufacturer
Socks knitting: 168 needle,
1 3.75” cylinder dia and single GK616DF3, 2016 Lonati, Italy
cylinder machine
Tupesa, RS-Basic
2 Sample washing machine Ecostar
Plus 5C
3 Boarding/Pressing Ghibli, 2014 Tecnopea
4 Fabric cutter N/A Local
2.3.2. Equipment for testing

Equipment for testing are given in Table 4.
Table 4: Equipment for testing.
Sr. No Equipment Name Model Manufacturer
1 Zeta Sizer Nano ZS Malvern panalytical
2 Single yarn strength tester Tensorapid 5 Uster
Fourier Transform Infrared
4 Spectrum TWO PerkinElmer, USA
Spectrometer (FTIR)
Scanning Electron
5 Quanta 250 FEI
Microscopy (SEM)
Ultraviolet Protection Factor
6 UV-2000S Labsphere
(UPF) Tester
Static Lab
7 Static charge tester Climatest, code Mesdan, Italy
1722C
Moisture Management
8 M290 SDL Atlas
Tester (MMT)
9 Sweating guard hot plate M259B SDL Atlas
2.4. Methods
2.4.1. Experimental factors and their levels

Experimental factors and their levels are given in Table 5.
15
Table 5: Experimental factors and their levels
Factors Level
Sr. No Factors Units
1 2 3
32 Tex
29 Tex 35 textured
textured
1 Yarns - combed twisted
twisted
cotton polyester
nylon
2 Concentration (graphene-oxide) Wt% 1 2
3 Number of coating cycles - 1 2 3
2.4.2. Response variables

Response variables are given in Table 6.
Table 6: Response variables.
Response
No. Units Testing Equipment Testing Method
Variable
Standard
1 GO Particle size nm Zeta Sizer
Protocol
2 Yarn tenacity cN/tex Single yarn strength tester ASTM D 2256
Functional groups Fourier Transform
Standard
3 on developed yarn N/A Infrared Spectrometer
Protocol
samples (FTIR)
Morphology of Scanning Electron Standard
4 SEM Images
yarns Microscopy (SEM) Protocol
Standard
5 Fabric UPF - UPF Tester
Protocol
Fabric surface
Static charge tester; Static BS EN 1149-1,
6 resistivity and Ω
Lab BS EN 1149-2
vertical resistance
Fabric thermal
7 m2K/W Sweating Guard Hot Plate ISO 11092
resistance
16
Fabric thermal
8 W/(m.K) Sweating Guard Hot Plate ISO 11092
conductivity
Fabric moisture Moisture Management
9 OMMC AATCC 195
management Tester (MMT)
2.4.3. Design of experiment

The design of the experiment is given in Table 7.
Table 7: Design of experiment
Number
Concentration
Sample of
Sr. No. Main Yarns (wt% graphene-
Code coating
oxide)
cycles
1 C1 29 Tex combed ring-spun cotton 1 1
7 N1 32 Tex textured twisted nylon 1 1
13 P1 35 Tex textured twisted polyester 1 1

17
2.5. Sample preparation methods
2.5.1. Preparation of graphene oxide (GO) dispersion

Concentrated aqueous solutions of graphene oxide were prepared with concentrations of 1 wt%
and 2 wt% respectively, with subsequent stirring at 700 rpm for 60 minutes using a mechanical
stirrer.
2.5.2. Preparation of GO coated yarn samples

Yarn samples of 10 grams each of cotton, polyester and, nylon were collected using a yarn lea
making machine. Each sample was dipped in GO aqueous dispersion for 60 minutes with
continuous stirring at 500 rpm. These yarns were squeezed by passing through a squeezing
ͦͦͦͦͦ
ͦͦͦͦͦͦͦͦͦͦͦͦͦͦͦ
degree sign
roller (60 PSI) to remove excessive liquor and were then dried at 90 ͦͦͦͦͦC for 60 minutes in a hot
air oven. After drying, coated yarns were stored in dark packaging.
2.5.3. Reduction of GO coated yarn samples

GO coated yarns were reduced using a strong reducing agent; Sodium hydrosulfite (Na2S2O4)
with a concentration of 4 g/L with continuous stirring at 90 oC for 60 minutes. These yarns
were squeezed, washed, and dried in an oven at 120 oC for 30 minutes.
2.5.4. Preparation of fabric samples

The coated yarn samples were adequately marked and were used on 144N 4” SC, GL716-
circular knitting machine with 250 rpm speed to knit plain/flat fabric tubes. Figure 9 shows the
knitting machine that was used to develop fabric samples. The coated yarns were used as main
yarns and 20 70/24/2 DN Lycra/Nylon 5:95 as plaiting yarn. 50 cm long sample tubes with
standard courses were knitted. Knitted samples were developed while keeping the cross stretch
18
the same i.e. 23 cm. The knitted samples were washed at room temperature for 30 minutes
using a sample washer. After washing, samples were dried at room temperature for 24 hours.
Dried samples were passed through the cutting process to prepare 20×20 cm square fabric for
testing purposes.
Figure 9: Socks knitting machine.
2.6. Testing methods
2.6.1. Particle size analysis

GO particle size was analyzed using Zetasizer Nano ZS. 2 ml of graphene-oxide was taken and
dispersed using a water bath sonicator for 30 minutes. The sample was then placed in a glass
container and placed in Zetasizer Nano ZS. The test was performed at 25 oC for 60 seconds.
Figure 10 shows the Zetasizer Nano ZS testing machine. This instrument enables in measuring
zeta potential and particle size. The molecular size of GO was measured by using this
technique.
19
Figure 10: Zetasizer Nano ZS.
2.6.2. Yarn tenacity
Yarn tenacity is an indication of its strength. The tenacity of developed GO yarns was analyzed
through a single yarn strength tester (Uster’s tensorapid 5) which is shown in Figure 11. The
test was performed as per standard test method i.e. ASTM D 2256. The test speed was 1 meter
per minute at room temperature. The test was performed at 25 oC and 65% humidity.
Figure 11: Tensorapid 5 as single yarn strength tester.
20
2.6.3. Functional group analysis
Functional groups were analyzed through FTIR testing. A sample swatch was placed in the
tester and 16 scans were performed. The test was performed at 25oC and 65% humidity with a
standard wavelength. Spectra was saved for functional group analysis. PerkinElmer spectrum
two- FTIR is shown in Figure 12 that was used to test functional groups on treated and
untreated yarn samples.
Figure 12: PerkinElmer spectrum two-Fourier transform infrared spectrometer.

2.6.4. Yarn morphology
A scanning electron microscope (SEM) was used for the characterization of reduced-GO
coated yarns. The topography and morphology of treated fabric were analyzed. A Quanta 250
FEI scanning electron microscope, as shown in Figure 13, was used to investigate the
morphology of the developed yarns. During this testing, the sample was sputter-coated for 30
seconds and then placed in SEM. Images were taken at a resolution of ×500. Elemental and
compositional analysis was also carried out. Images of all samples were obtained by using this
technique.
21
Figure 13: Quanta 250 FEI scanning electron microscope.
2.6.5. Fabric surface resistivity and vertical resistance
Mesdan static lab tester was used for this testing as shown in Figure 14. Fabric surface
resistivity and vertical resistance were analyzed through ISO 11092 testing standard at 21˚C,
and 65% humidity. A fabric swatch of Standard fabric size (8×8 inch2) was taken. Before
testing, a blank machine scan was carried out to remove errors. The sample was placed in the
machine and the scan was taken on eight different positions of sample.
Figure 14: Static Lab (static electricity tester).

22
2.6.7. Fabric thermal resistance
Fabric thermal resistance was measured using BS EN 1149-1 standard test method at
temperature:22.0˚C and humidity: 32.0%. Figure 13 shows SDL Atlas’s sweating guarded
hotplate hat was used to analyze fabric thermal resistance.
2.6.8. Fabric thermal conductivity
Fabric thermal conductivity was measured using BS EN 1149-2 standard test method at
temperature:22.0˚C and humidity: 32.0%. Figure 15 shows SDL Atlas’s sweating guarded
hotplate hat was used to analyze fabric thermal conductivity. Thermal conductivity was
calculated by dividing fabric thickness with thermal resistance.
Figure 15: Sweating guard hot plate.

2.6.9. Fabric moisture management
Overall moisture management (OMMC) was analyzed by using AATCC 195 standard test
method at 21˚C, and 65% humidity. Figure 16 shows the SDL Atlas’s moisture management
tester (MMT) that was used to analyze OMMC.
23
Figure 16: Moisture management tester.
2.6.9. Ultraviolet protection testing
Transmittance and blocking of ultraviolet radiation through coated sample fabrics was
calculated using UV-2000S (Labshere-USA) according to AATCC 183 standard test method
at a temperature of 21±1°C, the relative humidity of 65±2%, and wavelength range of 280-400
nm. Figure 17 shows the Labshere UV-2000S ultraviolet protection tester.
Figure 17: Labshere UV-2000S ultraviolet protection tester.

24
Chapter 3
Results and discussion
3.1 Characterization of graphene oxide (dispersion)
GO was synthesized by a proprietary modified Hummers method, washed with HCl-solutions,

and stored as an aqueous dispersion. GO dispersion was purchased from Graphenea. GO
dispersion was then analyzed for particle size using Zeta sizer. GO general analysis indicates
its viability for application on textiles. GO dispersion is stable and specifications provided by
the supplier are given in Table. 8
Table 8: GO specifications.
Sr. No Property Value
1 GO form Dispersion
2 GO Particle size 330 nm
3 Color Brown
4 Odor Odorless
5 Disperse-ability Polar solvents
6 Solvents Water
7 Concentration 1 wt%, 2 wt%
8 pH 2.2-2.5
3.1.1. Graphene oxide elemental analysis

The elemental analysis provided by the supplier is given in Table 9.
Table 9: Elemental analysis.
Sr. No Element Percentage
1 Carbon 49-56%
2-- Hydrogen 0-1%
3 Nitrogen 0-1%
4 Sulfur 2-4%
5 Oxygen 41-50%
25
3.1.2. Zeta sizer analysis
Four readings were taken, and the average particle size (diameter) was 328 nm. Below is the
size distribution graph that depicts the quality of GO dispersion. The size distribution peak can
be seen ranging between 200 nm and 600 nm. Figure 18 shows the zeta size analysis of GO.
Figure 18: Zeta size analysis of GO.
3.2. Chemical interaction of GO with textiles
3.2.1. Chemical interaction of GO with cotton

GO has an excellent affinity for textiles like cotton, polyester, and, nylon due to the availability
of reactive functional groups. OH, COOH and H groups on both structures play a vital role in
the development of bonds and hence water as a byproduct. Figure 19 shows the chemical
interaction of GO with cotton during the reduction [35].
26
Figure 19: Chemical interaction of GO with cotton during reduction [35].
3.2.2. Chemical interaction of GO with polyester
Graphene has a good affinity for polyester when reduced using a strong reducing agent. The
main point that should be kept in focus was temperature during reduction. The reduction should
be done at 90 oC using a strong reducing agent. Figure 20 shows the chemical interaction of
GO with polyester during reduction [36].
Figure 20: Chemical interaction of GO with polyester during reduction [36].

27
3.2.3. Chemical interaction of GO with nylon
Nylon makes a weak bond with graphene oxide when reduced. The main reason for this weak
bond is the unavailability of similar functional groups on the chemical structure of nylon.
Figure 21 shows the chemical interaction of GO with polyester during reduction [37].
Figure 21: Chemical interaction of GO with polyester during reduction [37].
3.3. Yarn and fabric testing
3.3.1. Yarn linear density, CV% and, tensile properties

Yarn parameters, i.e., linear densities (Tex), CV%, and tenacity, were tested for coated yarns.
An increasing trend in yarn linear densities (Tex) in all developed yarn samples with a
reduction of GO was found. CV% was increased with increasing graphene percentages and,
the number of coating cycles. The linear yarn density of untreated cotton (C0) was 29.23 Tex
while the treated sample; C6 had a linear density of 29.86 Tex. The reason for increasing yarn
linear densities (finer to coarser), in all the samples was due to the shrinkage behavior of
materials during the reduction of GO-coated at 90oC. Figure 22 shows the yarn linear densities
of cotton samples. A similar trend was observed in the case of polyester and nylon. In the case
of polyester (P0), the untreated linear yarn density was 35.22 Tex and its treated P6 (R-GO-
Polyester) sample had 36.88 Tex.
28
29.60
29.50
Yarn Linear Density (Tex)

29.40
29.30
29.20
29.10
29.00
C0 C1 C2 C3 C4 C5 C6
Figure 22: Linear yarn densities of cotton yarns.
In the case of polyester, Figure 23 shows the increasing trend in polyester linear densities.
36.40
36.20
36.00
35.80
35.60
35.40
35.20
35.00
34.80
34.60
P0 P1 P2 P3 P4 P5 P6
Figure 23: Linear yarn densities of polyester yarns.

Similarly, linear yarn densities of nylon samples were increased with an increasing percentage
of GO coating and coating cycles. Figure 24 shows the increasing trend in nylon linear yarn
densities (finer to coarser). The untreated nylon (N0) sample had a linear yarn density of 31.76
Tex while the sample with maximum GO concentration (N6), after reduction, had 33.11 Tex.
29
33.50
33.00

32.50
32.00
31.50
31.00
N0 N1 N2 N3 N4 N5 N6
Figure 24: Linear density of nylon yarns.

CV% of all these samples were analyzed and compared. Figure 25 shows an increasing trend
in CV% in the case of cotton, polyester, and nylon. A rising trend in CV% was found in all the
samples. Cotton showed a change in CV% from 1.06 to 1.4; polyester showed change in CV%
from 0.42 to 1.02 and nylon showed a CV% change from 0.62 to 1.06. The reason for this
increasing trend was the difference in the coating of all these materials. As yarn counts were
varying along with CV%, it was concluded that the coating was not uniform.
1.6
1.4
1.2
1
CV%
0.8
0.6
0.4
0.2
0
C0 C1 C2 C3 C4 C5 C6 P0 P1 P2 P3 P4 P5 P6 N0 N1 N2 N3 N4 N5 N6
Figure 25: CV% of cotton, polyester, and nylon.

It was found that tenacity increased from 16.69 cN/tex to 17.44 cN/tex with increased graphene
percentage in the case of cotton yarns while in the case of nylon and polyester yarns, it was
reduced from 34.92 cN/tex to 30.49 cN/tex and 34.89 cN/tex to 30.67 cN/tex respectively. This
30
was due to the better reactivity of graphene oxide with cotton as compared to nylon and
polyester during the reduction process. Secondly, due to an increase in the number of treatment
cycles, nylon and polyester filament strength was reduced. Figure 26 shows an increasing trend
of tenacity for cotton and a decreasing trend for polyester and nylon. Cotton and GO developed
strong molecular bonds during the reduction of the GO-Coated cotton samples. The behavior
was different in the case of polyester and nylon, and it was due to less reactivity/bonding of
GO with the substrate materials. A decreasing trend of tenacity was found for polyester and
nylon.
40
35
30
Tenacity (cN/tex)
25
20
15
10
0
Figure 26: Tenacity for cotton samples and a decreasing trend for polyester and nylon
samples.
3.3.2. Ultraviolet protection factor (UPF)
Ultraviolet Protection Factor (UPF) is an indication of blocking of UV (UVA & UVB) rays to
the human skin. UPF value of 50 represents maximum blocking. UV rays are dangerous for
human skin and cause multiple damages. UVA can cause sunburn but UVB is most dangerous
as it can cause skin cancer. It was noted that UPF values were increased by increasing the
graphene oxide percentage. in the case of cotton, with an increase in concentration and the
number of coating cycles of graphene oxide, UPF values were tremendously enhanced. A
similar trend was observed in UPF blocking, while UPF transmittance was greatly reduced
with increasing GO coating. UPF value of graphene-coated polyester was highest while
graphene-coated nylon stood at the second number and graphene-coated cotton was with least
values.
31
UPF values of all reduced graphene oxide coated samples were compared with untreated
cotton, nylon, and polyester respectively. Figure 27 shows the impact of reduced graphene
oxide on UPF values of cotton, nylon and polyester. An increasing trend in UPF values was
observed. On average, UPF values of cotton, nylon, and polyester were increased from 97.94
to 1772, 177 to 1971, and 107 to 1991 respectively. If we compare cotton, nylon and polyester,
the highest UPF values were observed in polyester. Based on this comparison, we can use these
graphene coated materials in smart textiles.
2000
1800
1600
1400
1200
UPF
1000
800
600
400
200
0
Figure 27: Ultraviolet protection factor (UPF) of cotton, nylon, and polyester.
UVA blocking values of cotton, nylon and, polyester were observed. Figure 28 shows the UVA
blocking values of cotton, nylon and polyester. UVA blocking of cotton was increased from
96.90% to 99.87%, UVA of nylon was increased from 94.82% to 99.91% and UVA of
Polyester was increased from 93.07% to 99.98%. Although all three materials showed
excellent UVA values with an increase in graphene concentration and coating cycles however
Polyester was best among all. The results show that Polyester was at the top of the list when
coated with graphene oxide.
32
100.00%
98.00%
96.00%
%age UVA Blocking
94.00%
92.00%
90.00%
88.00%
Figure 28: UVA blocking of reduced GO coated fabrics.

UVB values of cotton, nylon, and polyester were increased from 96.89% to 99.97%, 97.46%
to 99.98%, and 98.10% to 99.98% respectively. Figure 29 shows UVB blocking values and
the comparison of uncoated cotton, nylon, and polyester with coated materials. Although all
three materials showed excellent UVA values with an increase in Graphene concentration and
coating cycles, however, nylon and polyester both showed almost similar results. The results
show that Nylon and Polyester were excellent in terms of UVB blocking when coated with
graphene oxide.
33
100.00%
99.50%
99.00%
98.50%
%age UVB blocking
98.00%
97.50%
97.00%
96.50%
96.00%
95.50%
95.00%
Figure 29: UVB blocking values.

UVA transmittance values were also investigated and a tremendous effect was achieved when
the concentration/percentage of graphene was enhanced. Figure 30 shows the trends of
decreasing UVA transmittance with increasing percentage and coating cycles of graphene
oxide. UVA transmittance of cotton, nylon, and polyester was effectively reduced from 6.10%
to 0.09%, 5.18% to 0.08% and 4.93% to 0.04% respectively. Polyester was found more
promising when coated with reduced graphene oxide. nylon and cotton also showed excellent
results but polyester was superior because with little increase in graphene oxide coating or with
increasing coating cycles, UVA transmittance was greatly reduced. Although, cotton showed
good results however it took more coating cycles and concentration of graphene oxide to gain
similar results of nylon. Hence, polyester showed better results and it can give better UV
protection.
34
7.00%
6.00%
%age UVA transmittance

5.00%
4.00%
3.00%
2.00%
1.00%
0.00%
Figure 30: UVA transmittance values.

Figure 31 shows the UVB transmittance values. Keeping the previous results in mind, this was
expected that UVB values of polyester should be as good as for as UVA. When we see the
below trends, this is proved that polyester showed the best results in terms of UVA
transmittance. Even when there was just a little increase in the concentration of graphene oxide
i.e. 1% by wt, UVB transmittance of polyester was reduced from 3.45% to 0.09% while with
further increasing the concentration and coating cycles, it was further reduced to 0.04%. UVB
values of cotton and nylon were reduced from 4.58% to 0.06% and 3.8% to 0.07% respectively.
Similarly, if we compare uncoated cotton, nylon, and polyester, we can see that Graphene can
play a vital role in developing smart textiles with better UV protection efficiency.
35
5.00%
4.50%
4.00%
%age UVB transmittance

3.50%
3.00%
2.50%
2.00%
1.50%
1.00%
0.50%
0.00%
Figure 31: UVB transmittance values.

3.3.3. Measurement of surface resistivity and vertical resistance
Electrical conductivity is dependent on the consistent coating of GO and its reduction. Figure
32 shows the decreasing trend in surface resistivity and vertical resistance in cotton samples.
When we compare the surface resistivity and vertical resistance of all the samples, we see an
extraordinary decrease in both of these values in R-GO-Coated samples. The untreated sample
of cotton had 76.8×E7 Ω surface resistivity and 34.8×E5 Ω vertical resistance. After coating
and reduction treatment of cotton, surface resistivity, and vertical resistance values dropped
to 4.32 ×E7 Ω and 5.85 ×E5 Ω respectively. C6 exhibited far less surface resistivity and vertical
resistance than C1. The reason for this trend was due to the increased concentration of GO and
increased number of coating cycles. Further, cotton has better bonding with GO during
reduction leading to better performance with respect to the surface and vertical resistance.
36
90
80
70
60
50
(Ω)
40
30
20
10
0
C0 C1 C2 C3 C4 C5 C6
Surface Resistivity (Ω) 100v (xE7) Vertical Resistance (Ω) 10v (xE5)
Figure 32: Surface resistivity and vertical resistance of cotton.
Polyester also showed similar behavior leading to excellent performance with respect to
surface resistivity and vertical resistance. Figure 33 shows the decreasing trend in surface
resistivity and vertical resistance in polyester samples. The untreated polyester samples had
1365×E9 Ω surface resistivity and 2532×E6 Ω vertical resistance. P1 samples, with minimum
GO concentration, showed 108.4×E9 Ω and 350.5×E6 Ω respectively. There was a continuous
decrease in these values leading to the P6 with the least resistance vales.
2500
2000
1500
Ω
1000
500
0
P0 P1 P2 P3 P4 P5 P6
Figure 33: Surface resistivity and vertical resistance of polyester.
37
Nylon samples showed a similar behavior like cotton and polyester with a decreasing trend in
surface resistivity and vertical resistance values. Figure 34 shows the decreasing trend in
surface resistivity and vertical resistance in nylon samples. Untreated nylon samples displayed
surface resistivity and vertical resistance values as 610×E10 Ω and 224×E8 Ω respectively.
Surface resistivity values of N1 to N6 increased from 808×E10 Ω to 1422×E10 Ω while vertical
resistance values were increased from 243×E8 Ω to 251.8×E8 Ω.
700
600
500
400
Ω
300
200
100
0
N0 N1 N2 N3 N4 N5 N6
Figure 34: Surface resistivity and vertical resistance in nylon samples.
3.3.4. Thermal resistance and thermal conductivity

All the samples, cotton, polyester, and nylon showed excellent improvement in thermal
conductivities. Figure 35 shows the thermal resistance and thermal conductivity values of
cotton. The thermal resistance of untreated cotton was 0.065 m2K/W and R-GO-Cotton
samples (C1 to C6) showed a reduction from 0.052 m2K/W to 0.045 m2K/W respectively. In
the case of thermal conductivity, cotton showed an increasing trend with an increase in GO
concentration & number of coating cycles. R-GO-cotton (C6) sample exhibited an excellent
thermal conductivity value of 0.216 W.m-1.K-1 while the untreated sample displayed 0.0185
W.m-1.K-1. The impact of GO coating and reduction on cotton was comparatively better than
nylon while polyester exhibited the best results.
38
0.08
0.07
Thermal Conductivity (W.m-1.K-1)

Thermal Resistance (m2K/W)
0.06
0.05
0.04
0.03
0.02
0.01
0
C0 C1 C2 C3 C4 C5 C6
Thermal Resistance (m2K/W) Thermal Conductivity (W.m-1.K-1)
Figure 35: Thermal resistance and thermal conductivity values of cotton.
The thermal conductivity response of GO coated polyester was best among all samples. Figure
36 shows the thermal resistance and thermal conductivity values of polyester. Thermal
resistance showed reduced redults by increasing the GO concentration. The untreated polyester
samples showed maximum thermal resistance i.e. 0.029 m2K/W and minimum thermal
conductivity of 0.0317 W.m-1.K-1 while the P6 exhibited minimum thermal resistance of 0.021
m2K/W and maximum thermal conductivity of 0.0424 W.m-1.K-1.
0.08
0.07
0.06
0.05
0.04
0.03
0.02
0.01
0
P0 P1 P2 P3 P4 P5 P6
Thermal resistance (m2K/W) Thermal Conductivity (W.m-1.K-1)
Figure 36: Thermal resistance and thermal conductivity values of polyester.

39
The thermal resistance of the untreated nylon samples was also very high that reduced with the
application of GO and its reduction in later stages. Figure 37 shows the thermal resistance and
thermal conductivity values of nylon. When GO-Coated nylon samples were reduced, N1
displayed thermal resistance and thermal conductivity values of 0.064 (m2K/W) and 0.0145
(W.m-1.K-1) respectively. N6 was best among nylon samples with thermal resistance and
thermal conductivity of 0.055 (m2K/W) and 0.0167 (W.m-1.K-1) respectively.
0.08
0.07
0.06
0.05
0.04
0.03
0.02
0.01
0
N0 N1 N2 N3 N4 N5 N6
Thermal resistance (m2K/W) Thermal Conductivity (W.m-1.K-1)
Figure 37: Thermal resistance and thermal conductivity values of nylon.
3.3.5. Liquid moisture management properties (OMMC)

Graphene coated materials have excellent moisture management properties. Figure 38 shows
liquid moisture management properties of cotton (OMMC). Moisture management properties
of cotton were analyzed, and an increasing trend was found. In the case of cotton, the untreated
sample showed a value of 0.5, while C1 showed improvement and had a 0.72 value. C6
exhibited maximum among all cotton with 0.84 value. That took cotton to second after
polyester due to better moisture management properties than nylon. Graphene oxide when
coated and reduced on cotton, showed better results among all cotton samples.
40
1
0.9
0.8
OMMC Index 0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
C0 C1 C2 C3 C4 C5 C6
Figure38 Liquid moisture management properties of cotton (OMMC).
When moisture management values of polyester were analyzed, the increasing trend was
found. Figure 39 shows the liquid moisture management properties of polyester (OMMC). In
the case of polyester, the untreated sample showed a value of 0.71, while the P1 sample showed
improvement and had a 0.78 value. P6 exhibited maximum among all samples with 0.88 value.
Graphene oxide when coated and reduced on polyester, showed the best results among all
samples leading to the best performer. The reason behind this highest value of moisture
management was the better moisture management properties of polyester in addition to the R-
GO.
1
0.9
0.8
0.7
OMMC Index
0.6
0.5
0.4
0.3
0.2
0.1
0
P0 P1 P2 P3 P4 P5 P6
Figure 39: Liquid moisture management properties of polyester (ommc).

41
Although OMMC values of untreated and treated nylon samples were not as good as polyester
or cotton, however, it also showed an increasing trend. Figure 40 shows liquid moisture
management properties of nylon (OMMC). The untreated nylon samples showed a value of
0.65 while N1 showed improvement and had a 0.69 value. N6 exhibited maximum among all
nylon samples with 0.77 value.
1
0.9
0.8
0.7
OMMC Index
0.6
0.5
0.4
0.3
0.2
0.1
0
N0 N1 N2 N3 N4 N5 N6
Figure 40: Liquid moisture management properties of nylon (OMMC).
3.4 Analytical testing
3.4.1. Fourier transform infrared spectrometer (FTIR) analysis

The level of reduction of graphene-oxide on cotton, polyester, and nylon was analyzed through
FTIR spectroscopy by comparing the spectra of untreated cotton, polyester, and nylon with
their respective GO-coated and reduced-GO-coated spectra.
In Figure 41, the broad peak of the hydroxyl group (OH) in cotton and GO-coated cotton was
observed in the range of 3300 cm-1. Still, the intensity of this broad peak was much lowered in
the case of reduced-GO-cotton spectra that might be due to the boding of GO with cotton after
the reduction of coated GO. Whereas, the peaks at 2918 cm-1 and 2845 cm-1 are attributed to
vibration of C-H stretching and HO-C=O traces respectively which were also minimized in
case of reduced-GO-cotton. But a slight absorption was noticed in the range of 2300 cm-1 only
in GO-coated cotton spectra which might be due to the result of weak bonding of GO with
cotton as vibration mode of O-H stretching [29].
42
Besides this, the difference in peaks (in range of 1200 ~ 1750 cm-1) was also noticed for these
three spectra. The new peak at 1744 cm-1 was noticed in GO-coated cotton which was moved
at 1708 cm-1 after reduction of GO attributes to the presence of methyl group in GO. While the
OH deformation peak at 1629 cm-1 and C-C stretching peak at 1424 cm-1 [30] was observed in
both cotton and GO-coated cotton, but after the reduction of GO, this both of these peaks were
disappeared that might be due to minimum active sites of GO and cotton after reduction.
Figure 41: FTIR analysis of cotton, GO-coated cotton, and reduced-GO-coated cotton.
In Figure 42, during the analysis of untreated polyester samples with GO-coated and reduced-
GO-coated polyester, a peak of OH group at 3434 cm-1 was observed in GO-coated and
reduced-GO-coated. While, the C-H stretching was prominent at 2925 cm-1 and 2849 cm-1 in
the case of reduced-GO-coated polyester and the intensity of these peaks was higher as
compared to the untreated polyester. The reason of higher intensity of GO-coated polyester
peak was due to the strong bonding of GO with polyester in result of reduction of GO. The
peaks observed at 1712 cm-1, 1408 cm-1 and 1339 cm-1 are usually attributed to the presence
of C=O stretching of carboxylic acid, C-O stretching and CH2 of glycol moiety in polyester
chains [31]. But the peak at 1454 cm-1 attributed to stretching of the C-O group deformation
43
of the O-H group was disappeared in untreated polyester and GO-coated polyester. The reason
behind this behavior was the presence of untreated particles of GO on polyester fabric. This
might be due to presence of some traces, although the fabric was intensively washed in hot
water. Besides this, the peaks of the terephthalate group (OOCC6H4-COO) at 1237 cm-1 and
1124 cm-1 were revealed [32, 33].
Figure 42: FTIR analysis of untreated polyester with GO-coated and reduced-GO-coated
polyester.
In Figure 43, nylon fiber showed a generic peak at 3292 cm-1 and an overlapping peak appeared
at 3080 cm-1 (clearer in GO-coated nylon) due to a strong hydrogen bond linking with N-H
bending. Presence of symmetrical and asymmetrical CH2 bond stretch in the polymer chain
was observed at 2923 and 2857 cm-1 [33, 34]. The band is associated with the C=O stretching
was noticed at 1634 cm-1 (in all spectra) but at 1713 cm-1 the peak was disappeared in untreated
nylon. Whereas, at 1533 cm-1 a peak was observed due to the bending N–H band and the
stretching of the C–N [33].
44
Figure 43: FTIR analysis of untreated nylon, GO-coated nylon, and reduced-GO-coated
nylon.
3.4.2. Scanning electron microscope (SEM) analysis
The surface morphology of coated yarn samples was studied and analyzed using FEI Quanta-
250 scanning electron microscope (SEM) at magnification 2000X and voltage; HV 5.00 kV.
Two samples of polyester, nylon, and cotton were selected respectively in order to analyze the
level of coating. In the case of cotton, an untreated sample can be seen in Figure 44. The
topographic analysis shows that GO was present on cotton fiber (C6) and coated material could
be traced in Figure 45. This analysis concluded that cotton samples were successfully treated
with GO. With increasing concentration of GO and the number of treatment cycles, the coating
was enhanced. After the reduction of GO, it made permanent bonding with cotton. Cotton
sample (C6) with 2 wt% concentration and three treatment cycles exhibited a maximum level
of coating.
45
Figure 44: SEM images of untreated cotton, polyester, and nylon yarns.
SEM images of untreated polyester can be seen in Figure 44 while the reduced graphene oxide
coated polyester sample (P6) can be seen in Figure 45. The topographic analysis shows that
GO was present on polyester fiber. This analysis concluded that overall polyester samples were
successfully treated with GO. With increasing concentration of GO and number of treatment
cycles, the quantity of GO coating was increased. After the reduction of GO, it made permanent
bonding with polyester.
In the case of nylon SEM analysis, GO coating was more prominent as compared to polyester.
SEM image of the untreated nylon sample can be seen in Figure 44. GO deposits on reduced
graphene oxide nylon yarn (N6) can be seen in Figure 45. The topographic analysis shows that
GO was present on nylon fiber, but the coating was not consistent. This analysis concluded
that nylon samples were successfully treated with GO. With increasing concentration of GO
and the number of treatment cycles, coating was enhanced.
Figure 45: SEM images of reduced GO treated/coated cotton (C6), polyester (P6) and, nylon
(N6) yarn.
46
3.5. Analysis of variance: ANOVA and main effect plots
Analysis of variance (ANOVA) was done in order to understand the impact of input variables
i.e. main yarn (cotton, polyester & nylon), concentration and number of coating cycles of GO
on output variables in the form of fabric properties (ultraviolet protection factor (UPF), surface
resistivity, vertical resistance, thermal resistance, thermal conductivity and OMMC). P-value
of less than 0.05 for output variables (fabric properties) indicates that any of these three input
variables has a statistically significant effect on that property, with a 95% confidence level. P-
value indicates the change in fabric properties by the change in the GO concentration, no. of
coating cycles, and type of substrate i.e. cotton, polyester, and nylon. The lower the value of a
P i.e. less than 0.05, significant is the impact of input variables on output variables.
3.5.1 Analysis of variance of ultraviolet protection factor (UPF)
The impact of cotton, polyester, and nylon main yarns had a significant effect on UPF with a
P-value of 0.023 which is significant as it had a confidence level of more than 95%. Table 10
shows the analysis of variance (ANOVA) of UPF. UPF was also significantly dependent on
the concentration of GO with a P-value of 0.002. An increase in GO concentration played a
vital role in the enhanced UPF. Similarly, the number of coating cycles was also a leading
factor in the change in UPF with a significance of more than 95%. All the input factors had a
significant effect on UPF. Figure 46 shows the main effects plot for the ultraviolet protection
factor in which polyester showed the best results in terms of UPF.
Table 10. A general linear model for ultraviolet protection factor (UPF) versus main yarn
(Tex), concentration, no. coating cycles).
Source DF Adj SS Adj MS F-Value P-Value
Main Yarn (Tex) 2 967882 483941 11.12 0.023
Concentration (Wt% GO) 1 2065013 2065013 47.43 0.002
No. coating cycles 2 1437356 718678 16.51 0.012
Error 4 174147 43537
Total 17 4644398
47
Figure 46: Main effects plot for the ultraviolet protection factor.
3.5.2. Analysis of variance of surface resistivity
The variance of analysis concludes that main yarns; cotton, polyester and nylon had a
significant impact on surface resistivity. Table 11 showed a general linear model of surface
resistivity versus main yarn (Tex), concentration, no. coating cycles. The concentration of GO
also had a significant effect on surface resistivity where the P-value is less than 0.05 leading a
confidence level of more than 95%. However, in the case of number of coatings, there was no
major impact on surface resistivity leading to the fact that the main yarn after reduced GO
coating has the best results in terms of surface resistivity. Nylon had the maximum surface
resistivity as shown in Figure 47. With increasing concentration, surface resistivity was
reduced while a similar trend was observed with the number of coating cycles but the impact
was not significant.
Table 11. General linear model: surface resistivity versus main yarn (Tex), concentration, no.
coating cycles).
Main Yarn (Tex) 2 468187 234093 5147.74 0
No. coating cycles 2 339 170 3.73 0.122
Error 4 182 45
Total 17 470723
48
Figure 47. Main effects plot for surface resistivity (Ω).
3.5.3 Analysis of variance of vertical resistance
Table 12. General linear model: vertical resistance versus main yarn (Tex), concentration, no.
coating cycles)
Main Yarn (Tex) 2 81395.6 40697.8 592.27 0
No. coating cycles 2 732.3 366.1 5.33 0.074
Error 4 274.9 68.7
83327.8
Total 17
49
Figure 48: Main effects plot for vertical resistance (Ω).
3.5.3 Analysis of variance of thermal resistance
P-values values from ANOVA of thermal resistance of reduced GO coated cotton, polyester,
and nylon main yarns, concentration, and no of coating cycles are given in the Table 13. The
effect of main yarns i.e. cotton, polyester, and nylon on the thermal resistance had significant
impact with P-value less than 0.05 leading to the confidence level of more than 95%. Lower
P-value showed that thermal resistance is significantly dependent on the type of main yarn.
Analysis further explained that the impact of GO concentration was also significant with P-
value less than 0.05 and the confidence level of more than 95% as shown in Table 13. However,
number of coating cycles played less significant role in varying thermal resistance with P-value
more than 0.05 leading to the significance less than 95%. Main effects plot of thermal
resistance depicts the maximum values of thermal resistance of polyester in Figure 49.
Concentration of GO played a vital role to increase thermal resistance.
Table 13. General linear model: thermal resistance versus main yarn (Tex), concentration, no.
coating cycles.
Main yarn (Tex) 2 0.004066 0.002033 1742.48 0
Concentration (Wt.% GO) 1 0.000098 0.000098 84 0.001
50
Error 4 0.000005 0.000001
Total 17 0.004194
Figure 49: Main effects plot for thermal resistance (m2K/W).

3.5.3 Analysis of variance of thermal conductivity
Analysis of variance of thermal conductivity was similar to that of thermal resistance. P-values
of main yarns i.e. reduced GO coated cotton, polyester, and nylon main yarns and
concentration of GO were less than 0.05 leading to the significant impact on thermal
conductivity while no. of coating cycles had a P-value of 0.073 that depicts a less significant
impact on thermal conductivity. GO concentration was statistically significant with 99%
confidence level (P-value < 0.05) for concentrations. P-values are given in Table 14. The main
effects plot, as shown in Figure 50, revealed that the change of main yarn had a major shift in
thermal conductivity values. Similarly, thermal conductivity has significantly enhanced with
increased concentration of GO.
Table 14. General linear model: Thermal conductivity versus main yarn (Tex), concentration,
no. coating cycles.
51
Main Yarn (Tex) 2 0.001753 0.000877 873.85 0
Concentration (Wt% GO) 1 0.00004 0.00004 39.48 0.003
Error 4 0.000004 0.000001
Total 17 0.048025
Figure 50: Main effects plot for thermal conductivity (W.m-1.K-1)

3.5.3 Analysis of variance of liquid moisture management (OMMC)
Overall moisture management capacity (OMMC) had a major impact of main yarns i.e. cotton,
polyester, and nylon and concentration of GO. Tables 15 shows the significance of these two
input variables i.e. main yarn and GO concentration that is more than 95% and P-values is less
than 0.05. No of coating cycles did not show significant effect on OMMC. Figure 51 shows
the main effects plot for liquid moisture management (OMMC) and reveals that there was a
major change when the main yarn changed from cotton to nylon. The graphical representation
shows a major increase in OMMC with an increasing concentration of GO.
Table 15. General linear model: liquid moisture versus main yarn (Tex), concentration, no.
coating cycles.
52
Main Yarn (Tex) 2 0.0244 0.0122 48.8 0.002
Concentration (Wt% GO) 1 0.01445 0.01445 57.8 0.002
Error 4 0.001 0.00025
Total 17 0.04615
Figure 51: Main effects plot for liquid moisture management (OMMC).
53
Chapter 4
Conclusion and Future Recommendations
4.1 Conclusion
There was a significant impact of reduced graphene oxide on the properties of cotton, polyester
and, nylon yarns, and fabrics. Strength and linear densities of textile yarns; cotton, polyester
and nylon were increased with increased GO concentration and coating cycles. Cotton showed
more promising results with respect to increase in tenacity. Ultraviolet protection of reduced
graphene oxide coated fabric samples was increased significantly with increased concentration
and coating cycles. Reduced graphene-oxide coated polyester showed the best results in term
of UV protection while nylon was just behind the polyester. A significant decrease in surface
resistivity and vertical resistance of all the reduced grpahene-oxide coated fabric samples was
concluded with an increase in GO concentration and the number of coating cycles. Polyester
fabric samples showed a significant decrease in surface resistivity and vertical resistance while
cotton was also performed well as compared to polyester with an increase in GO concentration
and coating cycles. The concentration of GO played a vital role in enhancing the thermal
conductivity of all developed samples. The thermal conductivity of GO coated polyester
samples was more significant among all the GO coated samples. Polyester showed a sharp
decrease in thermal resistance leading to an excellent thermal conductivity performance. The
thermal conductivity of cotton was not improved significantly while nylon showed a
significant increase in thermal conductivity with an increase in GO concentration and coating
cycles. It was also concluded that with three coating cycles, the properties of fabric samples
were significantly changed as compared to higher GO concentration and a single coating cycle.
Moisture management (OMMC) of nylon was increased more sharply with increased coating
cycles and concentration of GO. Fourier Transform Infrared Spectrometer (FTIR) analysis
showed that GO was reduced more effectively when coated on cotton yarn samples.
54
4.2 Future Research Recommendations
 The electrical properties of graphene can be utilized to develop smart textiles like
wearable electronic gadgets. Even conventional textiles can be converted to smart
textiles by using graphene-coated yarns in knitted and woven textiles.
 The study of the durability of GO coating after washing can be done with varying
parameters.
 The thermal conductivity and moisture management properties of graphene-coated
textile materials are excellent that can help in improving challenging moisture
management and comfort requirements of brands for their sportswear equipment.
 The ultraviolet protection factor of graphene-coated materials is excellent that can be
utilized to develop cost-effective space suits shielding.
 The study of the durability of GO coating after reduction can help in developing smart
textiles for deep-sea divers.
55
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59

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Graphene coated yarns and their knitted structures for smart textile

In partial fulfillment of the requirements for the degree of

Faculty of Engineering & Technology

National Textile University, Faisalabad

This modest effort is dedicated to my

Internal Examiner External Examiner

Director, Postgraduate Dean, Faculty of Engineering

Figure 1: Working mechanism of smart textiles [2]. ................................................................ 2

Table 1: Specifications of yarns. ............................................................................................. 14

1.1.1. Mechanism of smart textiles

Figure 1: Working mechanism of smart textiles [2].

Graphene is a material with extraordinary strength, stiffness, thermal conductivity, and

1.2. Applications of graphene

1.2.1. Applications of graphene in general

Figure 4: Smart textiles applications in military and defense [7].

Figure 5: Smart textiles applications in fashion, entertainment, and sportswear [7].

1.3. Literature review

1.3.1. Recent trends in smart textiles

(a) (b) (c) (d)

1.3.2. Recent trends in graphene-based textiles

Figure 7 TEM based Illustration of a graphene oxide nano-sheet [16].

1.3.3. Graphene oxide and its reduction

1.4. Research gap

1.5. Research problem

1.5.1. Statement of the research problem

1.6. Research aims & objectives

1.6.1. Overall aim

1.6.4. Scope of the project

Specifications of yarns used are given in in Table 1.

32 Tex textured twisted nylon with 24

35 Tex textured twisted polyester with

Specifications of the chemicals used are given in Table 2.

2.3.1. Equipment for sample development

2.3.2. Equipment for testing

2.4.1. Experimental factors and their levels

2 Concentration (graphene-oxide) Wt% 1 2

3 Number of coating cycles - 1 2 3

2.4.2. Response variables

2.4.3. Design of experiment

1 C1 29 Tex combed ring-spun cotton 1 1

2 C2 29 Tex combed ring-spun cotton 1 2

3 C3 29 Tex combed ring-spun cotton 1 3

4 C4 29 Tex combed ring-spun cotton 2 1

5 C5 29 Tex combed ring-spun cotton 2 2

6 C6 29 Tex combed ring-spun cotton 2 3

7 N1 32 Tex textured twisted nylon 1 1

8 N2 32 Tex textured twisted nylon 1 2

9 N3 32 Tex textured twisted nylon 1 3

10 N4 32 Tex textured twisted nylon 2 1

11 N5 32 Tex textured twisted nylon 2 2

12 N6 32 Tex textured twisted nylon 2 3

13 P1 35 Tex textured twisted polyester 1 1

15 P3 35 Tex textured twisted polyester 1 3

16 P4 35 Tex textured twisted polyester 2 1

17 P5 35 Tex textured twisted polyester 2 2

18 P6 35 Tex textured twisted polyester 2 3

2.5. Sample preparation methods

2.5.1. Preparation of graphene oxide (GO) dispersion

2.5.2. Preparation of GO coated yarn samples

2.5.3. Reduction of GO coated yarn samples

2.5.4. Preparation of fabric samples

Figure 9: Socks knitting machine.

2.6. Testing methods

2.6.1. Particle size analysis