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Investigation of the flammability properties of

a cotton and elastane blend denim fabric in the
presence of boric acid, borax, and nano-SiO2

Nilgün Becenen & Gökhan Eyi

To cite this article: Nilgün Becenen & Gökhan Eyi (2020): Investigation of the flammability
properties of a cotton and elastane blend denim fabric in the presence of boric acid, borax, and
nano-SiO2 , The Journal of The Textile Institute, DOI: 10.1080/00405000.2020.1800974

To link to this article: https://doi.org/10.1080/00405000.2020.1800974

Published online: 10 Aug 2020.

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THE JOURNAL OF THE TEXTILE INSTITUTE
https://doi.org/10.1080/00405000.2020.1800974

RESEARCH ARTICLE

Investigation of the flammability properties of a cotton and elastane blend

denim fabric in the presence of boric acid, borax, and nano-SiO2
€khan Eyib
€n Becenena and Go
Nilgu
a
Vocational College of Technical Sciences, Trakya University, Edirne, Turkey; bInstitute of Natural Science, Trakya University, Edirne, Turkey

ABSTRACT ARTICLE HISTORY

This study contributes to the field of flammable resistant textiles. Boric acid, borax, and nano SiO2 Received 5 August 2019
were added to a commercial finishing solution, separate solutions were prepared for each. The differ- Accepted 19 July 2020
ence in this study is to improve the functional finishing processes of denim fabrics consisting of 99%
KEYWORDS
cotton and 1% elastane. The aim is to draw attention to the flame-retardant performance improve-
Denim fabric; boric acid;
ments that can be created by a synergistic mechanism for textiles. Using TGA, LOI and vertical com- flame retardant;
bustion tests for determining flame retardant effect were sufficient to achieve meaningful and precise combustion tests
results. Each chemical added to increase the flammability performance effect of the commercial finish
solution entered the fabric surface structure, and the flammability performance of the commercial fin-
ish solution was improved by a simple and feasible method. Denim fabric can be made suitable for
industrial textiles by flame retardant finishing process.

Introduction and fabric structure have an important effect on the level of

Cotton fabrics are environmentally friendly, biodegradable,
soft, moisture wicking and breathable, such as having
important advantages for users but organic materials have a
high carbon and hydrogen content, which makes them eas-
ily flammable. The comfort of stretch denim garments
causes to be preferred more in daily and work clothes
(Kaynak, 2017; Varghese & Thilagavathi, 2015). Denim fab-
rics have been known for their durability and comfort in
the past, nowadays they stand out with their functional and
innovative aspects. In literature, there have been some stud-
ies on the comfort properties of denim fabrics containing
cotton and elastane yarn blend (stretch), but there are no
studies to increase their flammability performance despite
the increase in their use depending on the comfort factor in
work clothes. Clothing made from traditionally used fibers
is flammable when exposed to sources of fire such as open
fire, stove fire and cigarettes, flames can spread rapidly, and
the user may experience skin burns of up to 70% of the
body’s surface within seconds (Chivas et al., 2009;
Forouharshad et al., 2011; Horrocks & Anand, 2000).
Therefore, in recent years, the production of protective
clothing has gained importance for fire safety in the textile
industry (Weil & Levchik, 2008). Flame resistant textiles
developed (World Fire Statistics, 2017) for this purpose
have a wide range of uses (Horrocks et al., 2004; Kamath
et al., 2009; Stegmaier et al., 2005). The term flame retardant
textile refers to the textile product made fire-resistant with
suitable flame retardant chemicals (Neisius et al., 2014). It is
concluded that in textile materials selected for the produc-
tion of protective clothing, parameters such as fiber content
clothing protection (Dipietro et al., 1971; Nawaz et al.,
2011). In addition to the advantages of denim fabrics made
entirely of cotton, their low flexibility can be seen as a dis-
advantage that reduces comfort features. Therefore, it is
planned to provide ease of movement and wearing to the
user by using denim fabric containing 1% elastane. It is
believed that the denim fabric with 1% elastane and 99%
cotton as a protective clothing will increase the flame resist-
ance and contribute to the production of denim with
improved comfort and functionality.
Brominated flame retardants accounted for about 21% of
the total flame-retardant production in the world in 2004,
they were very effective in low amounts compared to other
flame retardants (Birnbaum & Staskal, 2004; Wimmer et al.,
2004). However, many brominated flame retardants have
unintended negative effects on the environment and human
health (Meerts et al., 2001; Waaijers et al., 2013; Xie et al.,
2013). Halogen containing retardants such as chlorine,
bromine, and derivatives have been widely applied to cotton
fabrics, suppressing oxygen and heat transfer and delaying
the spread of fire. Due to the toxic and corrosive effects of
gases released during combustion, limitations have been
placed on their use (Levchik & Weil, 2008). Flame retard-
ants which can pose risks to the environment and human
health are subject to different levels of restrictions in differ-
ent countries and are banned in some. Flame retardants
containing boron, phosphorus, nitrogen and silicon draw
attention with their being excellent flame resistance and
environmental friendliness (Zhao, 2010).

CONTACT Nilg€un Becenen nilgunbecenen@trakya.edu.tr Vocational College of Technical Sciences, Trakya University, 22030 Edirne, Turkey
ß 2020 The Textile Institute
2 N. BECENEN AND G. EYİ
Boric acid and borax remove water molecules involved in
the cellulose structure before the ignition temperature and
prevent combustion progression by forming a glassy pro-
tective layer on the cellulose surface. In the decomposition
of boric acid as a result of an endothermic reaction, water is
observed due to increase of temperature and a glassy pro-
tective layer occurs. The glassy protective layer cuts off con-
tact between the polymer surface and oxygen and protects
the surface from heat (Troitzsch, 1998). Nanocomposite
coatings are reported to represent a promising system that
protects the oxidation of the char structure after it is
installed, there by strengthening the flame-resistant proper-
ties of coatings (Wang et al., 2007).
Many of the nitrogen based compounds used as flame
retardants are melamine derivatives, with both gas and con-
densed phases also exhibiting flame inhibition (Laoutid
et al., 2009). Interest in the development of environmen-
tally-friendly flame-retardant technology has led researchers
to develop coatings with an advanced fire-retardant effect by
combining plasma and nanotechnology (Quede et al., 2004).
Nano TiO2 and SiO2 have been extensively used.
The flame resistance of fabric depends on fabric proper-
ties (weight, type of fiber, mixture ratio of fibers, fabric
structure, etc.), chemicals and methods used in the finishing
processes, the point where the flame touches, the flame
intensity and fabric position. A large number of test meth-
ods, developed depending on variables are included in the
standards (Horrocks, 2008). Many researchers have used
LOI value in determining fabric flame retardant effective-
ness. Since the closest position to the daily use of clothing is
vertical, the vertical combustion test was also preferred in
terms of getting the closest result from combustion tests
(Morgan, 2019; Shete et al., 2004). This study is about
improving the flame retardant feature in denim fabrics
made of cellulose and elastane fiber combination and
increasing performance of commercial flame retardant used
in textile production with adding boric acid, borax and
nano-SiO2 compounds. The objectives of the study are
1. To improve the flame retardant performance of the
commercial finishing solution with the synergistic effect
mechanism by adding boric acid, borax and nano-SiO2
compounds to the commercial finishing chemical with
flame retardant effect for textile materials,
2. To increase the use of denim fabrics in daily and work
clothes thanks to the increased comfort and functional-
ity by adding 1% elastane to the fabric structure in
denim fabrics and improving their flame retardancy
performances.
Experimental
Materials
Denim fabric is blue dyed, made from 99% cotton and 1%
elastane yarns, 3/1 twill weaving. Chemicals (all 99.9% pur-
ity) are boric acid, borax (Na2B4O7.10H2O), nano SiO2 and
commercial finishing solution. Commercial finishing
solution is a commercially sold flame retardant that affects
cellulose fiber textiles. It can create a smooth film layer on
fabric surfaces. It is a halogen and antimony-free finishing
solution composed of organic and inorganic nitrogen salts.
Method
Preparing the finishing solution
Process solutions prepared with different chemicals in the
same prescription values were used. Loading rates were
taken the same for each solution, the solids added to the
solutions were changed. Process solutions were considered
as below:
1. Only commercial finishing solution
2. 50% commercial solution þ 50% water þ boric acid (5%
by weight)
3. 50% commercial solution þ 50% water þ borax (5%
by weight)
4. 50% commercial solution þ 50% water þ nano SiO2
(5% by weight).
Solutions were obtained by stirring samples magnetically
at 30  C at 800 rpm. Fabric samples with the same properties
were processed separately with prepared solutions.
Pad-dry-cure covering method
Firstly, fabric samples were impregnated with process solu-
tions and 70% tightening in a laboratory foulard machine,
then dried at 100  C thermostat dryer, and fixated at 120  C
in the same dryer for 2 s (Figure 1).
Sample characterization
SEM (Scanning electron microscopy) Zeiss Levo LS 10
brand SEM microscope) and EDX (Energy dispersive X-ray
analysis) were used for the surface analysis.
Performance features
The tensile strength (ISO 13934-1) and tear strength (TS
EN ISO 13937-1) and tensile properties (ASTM D2594-04)
of the treated and untreated denim fabrics are determined
according to international standards.
TS EN ISO 13937-1: This standard describes to deter-
mine fabric tear force known as ballistic pendulum
(Elmendorf) method. Tear strength is the resistance force
required to initiate and maintain a tear under specified con-
ditions in a fabric. In this method, the sample prepared in a
rectangular shape with a notch on it is subjected to tearing
force by a pendulum. In the test device, the fixed jaw is
attached to the base of the device and the movable jaw is
attached to a pendulum capable of free swinging downwards
with the effect of gravity. Tear strength is calculated in both
warp and weft direction. During tearing, the threads break
off individually or in groups. For this reason, the strength
of single threads is important in tearing. Since the denim

Figure 1. (a) Preparation of finishing solutions, (b) foulard, (c) dryer and (d) treated denim.
fabric used in the study consists of elastane and cotton, it
has been examined considering that it may have an impact
on tear strength values. In addition, the finishing processes
applied to the fabric is another factor affecting the tear
strength. If chemical finishing is applied to the fabric, this
often increases friction between the yarns and reduces free-
dom of movement. Thus, it causes a decrease in tear
strength. For this reason, in order to determine the effect of
process solutions applied on denim fabric tear strength, tear
strength tests were applied (https://www.iso.org/standard/
23369.html).
Breaking strength ISO 13934-1: This European Standard
specifies a procedure to determine the maximum force and
elongation at maximum force of textile fabrics using a strip
method. The dimensions of the sample to be tested are
50 mm wide and 150 mm long. The tensile strength of the
fabric was determined in conjunction with the standard test
procedure ISO 13934-1 (1999) (ISO 13934-1:1999, 1st
Edition, pp. 12). The standard consists of stretching the fab-
ric sample until it breaks. The forces that separate the sam-
ple during stretching and breaking are measured (https://
www.iso.org/standard/60676.html).
Stretching properties were determined according to
ASTM D2594-04 (https://www.astm.org/Standards/D2594.
htm). This test method includes procedures for fabric
growth and stretching and can be used individually when
individual specifications are required. A tensile testing
instrument, consisting of a frame with separate clamps fixed
at the top and at the bottom, was implemented to determine
the stretch properties of the fabrics. Sample strips from weft
direction were hung on the apparatus after marking a
250 mm index in the central part of each specimen. A 1.8 kg
load, which was hung according to the fabric weight in the
bottom hanger, was applied to the sample three times and
after the fourth application; the marked distance was meas-
ured. The samples were hung for 30 min, and the distance
was measured once again. After that fabric samples were
THE JOURNAL OF THE TEXTILE INSTITUTE 3
removed from the tensile testing apparatus and let to be
relaxed for one hour. Fabric growth, maximum stretching
and elastic recovery values were calculated from these meas-
ured outcomes, as follows:
Stretch ð%Þ ¼ ðB  AÞ=A  100
Growthð%Þ ¼ ðC  AÞ=A  100
where, A: The distance marked between the upper and bot-
tom parts of the fabric (250 mm), B: The distance between
the marked points after hanging the sample for 30 min with
the load (mm), C: The distance between the marked points
after 1 h relaxation.
Thermal characterization
Thermogravimetric analysis (TGA)
Measures mass continuously while the temperature of the
sample changes over time (Liu & Yu, 2006). In a controlled
atmosphere (oxygen-nitrogen) weight changes that occur
during the change in substance temperature are determined
quantitatively. Thermo gravimetric data collected from a
thermal reaction is compiled in a graph with the percen-
tages of mass change on the Y-axis against temperature or
time on the X-axis. When material undergoes thermal deg-
radation, it determines the behavior of the material and the
amount of ash that occurs. The amount of ash is indirectly
used in determining the flame resistant. In this study, for
treated and untreated denim fabrics, in a nitrogen-oxygen
atmosphere, in the 25–900  C temperature range, mass
losses, residue formation and degradation temperatures were
determined by TGA analysis. The synergistic effects of solid
boric acid, borax and nano SiO2 chemicals added to the
commercial solution and the degree of flame retardant effect
on the fabric were determined by comparing the TGA ana-
lysis results of the fabrics treated with these solutions.
4 N. BECENEN AND G. EYİ
Determination of flame resistant properties for
denim fabrics
Flame retardancy of the untreated and treated denim fabrics
were examined by vertical burning test and LOI measure-
ment. These tests were chosen because they were very simi-
lar to the actual fabric combustion behavior. Samples were
conditioned 20 ± 2  C and 65 ± 4% RH conditions.
Vertical combustion tests (TS EN ISO 15025: in protect-
ive clothing)
Test parameters are 23  C and 30% RH. It was ignited with
propane gas for 10 s perpendicular to the fabric surface
placed in the test device. At the end of the period, flame
burning, flameless burning, spillage (dripping) formation
and hole formation were observed (www.iso.org).
LOI test
Shows the minimum concentration of oxygen a material
must have in the atmosphere to continue burning. It does
not specify exactly what would happen in the event of a
fire, but it is used in comparing flame retardants (BS EN
ISO 4589-2, 2017). The sample was placed on (Prowhite
brand) test equipment vertically in the chimney where
nitrogen and oxygen gases pass in the determined propor-
tions. Using an igniter fired by propane gas, a flame is
applied to the top surface of the sample for a maximum of
30 s by entering through the hole in the chimney cap and
coming from top to bottom. With a series of experiments at
different oxygen concentrations, the lowest oxygen concen-
tration required for the material to continue burning
is calculated.
Results and discussion
Surface properties of fabrics
SEM analysis
For untreated denim fabric, surface coating layer was not
visible (Figure 2a), transparent and thin chemical layer coat-
ing fibers were seen on the surface of the fabric treated with
a commercial finisher (Figure 2b), porous structure was
seen on the fabric surface that was treated with finishing
solution containing boric acid. This structure filled all the
gaps (Figure 2c). Finish layer containing Borax was distrib-
uted well over fabric (Figure 2d). Nano SiO2 particles
appeared prominently on coated fabric surface (Figure 2e).
It was concluded that prepared solutions could be adhered
to the surface using the pad-dry-cure technique.
EDX analysis
When the EDX results were evaluated, phosphorus and
nitrogen were observed in the chemical structure of all fab-
ric samples treated as due to the content of the commercial
finishing solution. Boron was found in the chemical struc-
tures of fabric treated with solutions containing borax and
boric acid. The presence of Si was detected in those contain-
ing nano SiO2 (Figure 3–7).
Thermal characterization
TGA analyses
When data was examined, the residue mass at 900  C was
0.3627% in untreated fabric. This suggests that untreated
fabric was completely burnt. Residue mass increased with
the additions made. The percentage of the residuemass with
the addition of boric acid was 15.43%, borax was 6.91% and
nano SiO2 was 12.71% (Figures 8–10).
Untreated denim fabric results
When TGA thermal diagrams untreated denim fabrics were
examined, there was no residue at the end of the test period,
and it was completely burnt (Figure 8). The deterioration took
place in three stages due to increase of temperature. The first
stage was from 23.08–129.65  C. The weight reduction at this
stage is 5.35%. The second stage was from 220.62–597.16  C
and the weight reduction was 80.01%. The final stage termi-
nated at 597  C and left no residue. The pyrolysis start and
ignition temperature was 350  C for untreated cotton fabric.
However, the thermal degradation of untreated fabric continued
until 597  C. This is because fabric properties helped the flam-
mability properties feature of the untreated fabric by delaying
thermal degradation (Horrocks, 2011).
Results for treated denim fabric
The first stage of deterioration due to temperature increase
in fabrics processed only with commercial finishing was at
28.54–139.93  C. and weight reduction 5.122%. The second
was from 139.93–223, 37  C and weight reduction 2.877%.
The third was from 223.37– 604.56  C. the weight reduction
52.40%. The final stage resulted in a weight reduction of
10.53% at 604.560  C. Theres idual mass was 6.392%
(Figure 9).
As separate solutions to a commercial finishing solution,
a decrease in the lost fabric mass compared to the commer-
cial solution by adding boric acid, borax and nano SiO 2
components (Figure 10) was observed. The deterioration
due to increase of temperature in all treated denim fabrics
occurred in four stages but untreated fabric took place in
three stages. When the mass losses of combustion are com-
pared for untreated and treated denim fabric, the loss rates
are as follows: in untreated denim 80%, 52.40% in only
commercial solution fabric, 40.39% in boric acid fabric,
49.70% in borax fabric, 41.75% in nano SiO2 fabric. These
results confirm the idea that by adding boric acid or nano
SiO2 into the commercial finishing solution used in the
study; the commercial finishing solution can increase the
thermal degradation effect of denim fabric at pyrolysis tem-
perature (Zhang et al., 2015). It was observed that the
amount of residue in the commercial finishing fabric, where
the untreated fabric burned completely without leaving any-
residue, can be increased by adding chemicals to the

Figure 2. SEM Images of denim (a) untreated, (b) treated with commercial finishing solution only, (c) containing boric acid, (d) containing borax, (e) containing
nano-SiO2.
Figure 3. Untreated denim.
commercial finishing solution. The results are consistent
with previous studies (Mettler et al., 2012) and show reli-
ability of tests. Mass loss was observed in all denim fabric
samples in range of approximately 28–110  C. This is
thought to be caused by water loss (Mettler et al., 2012). To
see the effect of additives the mass losses of fabrics treated
with finishing solutions containing boric acid, borax, and
nano SiO2 were compared within themselves; the greatest
mass loss was in samples treated with finishing solution
containing borax.
The temperature at which the polymeric structure begins
to deteriorate was fixed at the highest value (233  C) in
THE JOURNAL OF THE TEXTILE INSTITUTE 5
fabric samples treated with finishing solution containing
boric acid. In organic boron compounds form a glassy pro-
tective layer on the fabric surface and this layer act as pro-
tection against the oxygen and heat required for
combustion. Therefore, in these samples the degradation
temperature of the polymeric structure also increased in dir-
ect proportion to the amount of inorganic matter (Table 1).
Pyrolysis percentages of fabrics were taken as 15% in
untreated fabrics, 33% in the commercial finishing solution
treated samples, with boric acid addition 32%, with borax
addition 35%, and with nano-SiO2 addition 34%. Due to the
absence of inorganic matter in the untreated fabric the
6 N. BECENEN AND G. EYİ
Figure 4. Treated denim with only the commercial finishing solution.
Figure 5. Treated denim with finishing solution containing borax.
Figure 6. Treated denim with finishing solution conaining boric acid.
amount of pyrolysis, which is 15%, was deducted as the
amount of flammable, igniting gases. With commercial fin-
ishing solution treated and untreated fabrics, the tempera-
ture at which the polymeric structure begins to deteriorate
is the same and is 221  C. This is an expected result. This
can be explained by the flame retardant mechanism. During
the combustion process, although no inorganic matter was
formed in the untreated fabric, 6.5% inorganic matter was
formed in only commercial finishing fabric. Untreated fabric
has a high deteriorate temperature due to its structural
properties such as density and weight however, since no
inorganic substance was formed, it could not be prevented
from burning. The mechanism of action of commercial
flammability chemical has proceeded to reduce the release
of volatile degradation products that create fuel for the
flame (Table 1). Commercial finish is thought to change
pyrolysis mechanism of fabrics to create less flammable
volatile more ash. Results are consistent with the literature

Figure 7. Treated denim with finishing solution containing nano SiO2.
Figure 8. TGA diagram for untreated denim.
Figure 9. TGA diagramfor treated denimby only commercial finishing solution.
(Schindler & Hauser, 2004). The boric acid and nano SiO2
additions had effect on increasing the percentage of inor-
ganic substance of the commercial finishing solution. The
reason for the increase in organic matter is prevention of
evaporation and the formation of non-volatile coal products.
THE JOURNAL OF THE TEXTILE INSTITUTE 7
Inorganic matter percentages were also consistent with EDX
data. In treated fabrics containing boric acid and nano SiO2
the amount of inorganic matter was also high. The resulting
acids and hydroxyl groups in the fabric structure form are
non-volatile esters, which support the formation of coaling.
8 N. BECENEN AND G. EYİ

Figure 10. TGA diagram for treated denim with (a) containing boric acid, (b) containing borax, (c) containing nano SiO2.

Table 1. Total TGA test results.

Fabric type Untreated Only commercial solution Containing boric acid Containing borax Containing nano-SiO2
Organic matter (Water) (%) 5 5 4 4 4
Organic matter (other) (%) – 5 8 4.5 8
Polymer matter (%) 80 46 40.5 49.5 41.5
Pyrolysis (%) 15 33 32 35 34
Inorganic matter (%) – 6.5 15.5 7 12.5
Beginnings of polymeric structure degradation ( C) 221 221 233 225 232.5
End of polymeric structure degradation ( C) 597 601 599 606 597

The change in degradation temperature with the addition of
nano structured SiO2 was an expected result, because nano-
particles have a larger surface area per unit mass and unit
volume than the conventional surface. Nanoparticles are
12 nm in size and have a surface area of 175–225 m2/g
(www.sigma aldrich.com). The SEM images clearly show
that nano SiO2 is distributed over entire fabric surface
(Figure 2). Nano SiO2 has low expansion coefficient and is
heat resistant material due to its high melting temperature.
With these features, nano SiO2 on the fabric surface form a
physical flame barrier by forming a nano layer. This barrier
that located between fabric surface and flame is provides
high resistance to the rapid spread of the flame (Gbewonyo
et al., 2017). Therefore, a higher degree of deterioration
occurred in nano loading. The initial temperature of poly-
meric structure degradation in commercially treated fabrics
was 221  C, while it was 232.5  C in fabrics treated with
nano SiO2.
Flame retardant performance test results
LOI test results
The LOI value gave sufficient results for the determination
of flame resistant properties for denim fabrics. By adding
borax, boric acid and nano SiO2 to the commercial finishing
solution, an increase in LOI values, that is, provided an
improvement in the flammability properties of denim fab-
rics (Table 2).
Untreated fabrics had 20.1% LOI, which is lower than
the oxygen ratio in air (21%) under normal conditions;
untreated denim fabric continues to burn after the flame is
removed. With 20.1% LOI is defined as flammable

Table 2. LOI test results.
Fabric type Untreated Only commercial solution
% LOI 20.1 73.9
Standard Deviation % d 0.2 0.4
Sequential O kons. the difference 0.3 0.5
Figure 11. LOI test application for untreated denim fabric: (a) image of the LOI tester, (b) sample section of tester, (c) appearance of fabric at the start of test and
(d) the end of test.
according to the standards. The 73.9% LOI value for fabrics
treated with commercial finishing solutions increased by
over 80% with the addition of boric acid, borax, and nano
SiO2. Highest LOI value was observed in boric acid added
finish solution (Table 2). The high LOI value suggests that,
in standard atmospheric environments, that material has
more difficult combustion characteristic. Because the LOI
value for treated denim samples is higher than oxygen ratio
(21%), these fabrics are non flammable after the flame is
removed. In order to be safe in fire danger in real life, the
use of clothes made from high LOI value fabrics will be
very helpful. In stretch denim clothes treated with flame
retardant, flame spread and skin burns on the garment can
be prevented. The LOI results can also be verified by the
mass profile in TGA. Inorganic matter was not formed in
untreated fabric and inorganic matter formation was
detected in other finish solutions. Inorganic substances pre-
vented the formation of flammable volatile substances and
the power igniting performance of denim fabrics
was improved.
Combustion mechanisms of textile fibers depend on
chemical structure of the fiber and the coatings applied on
the fiber (Didane et al., 2012). Connection between the LOI
value of the fabrics and degradation temperature is related
to the combustion mechanisms of the fibers used and the
flame regardants. Although the polymeric structure deterior-
ation of untreated and commercial finishing solution treated
denim fabrics is the same as the initial temperatures but
THE JOURNAL OF THE TEXTILE INSTITUTE 9
Containing boric acid Containing borax Containing nano SiO2
89.4 82.4 86.3
0.6 0.6 0.6
0.8 0.8 0.8
LOI values are different. It is seen that borax or boric acid
or nanoSiO2, which are added to the commercial finishing
solution, change the combustion mechanism of denim fabric
with synergistic effect and increase the pyrolysis temperature
in comparison to the commercial finishing (Tabuani et al.,
2012). They have also been shown to affect the pyrolysis
reaction to produce less flammable volatiles and more
residual coal, thereby achieving a better flame retardant
effect than a commercial finish. With this mechanism, resi-
due formation and LOI value can be increased at the end of
combustion compared to commercial finishing. The results
in Table 2 are consistent with those in Table 1. In both
tables, it confirms the statement that the addition of boric
acid or borax or nano SiO2 may increase the flame retardant
effect of commercial finishing solution on denim fabric.
Mineral-based flame retardant chemicals increase the
thermal degradation temperature and LOI value of the fiber
by providing cooling during condensation with the power
ignition mechanism that provides cooling mechanism with
endothermic reactions (Liang et al., 2013). Some images
were given in Figure 11.
Results of vertical combustion test
According to the test results, adding boric acid, borax, or
nano SiO2 to commercial finishing solution provided signifi-
cant suppression of fire and heat release, while creating an
anti-burn layer. No progress of combustion was observed
10 N. BECENEN AND G. EYİ

Table 3. Results of vertical combustion test.

Fabric type
Only commercial Containing Containing Containing
Sample Test measurements criteria Uncreated finishing solution boric acid borax Nano SiO2
Whether any flame reaches the upper Occured Occured No occur No occur No occur
edge or one of the vertical edges
Flame burn time after flame 396 s 49 s No occur No occur No occur
Weft towards Cored combusition progression beyond Occured Occured No occur No occur No occur
the flame span (usually carbon area)
Burning with cinder after flames 300 s 86 s No occur No occur No occur
Residue (rash) formation Occured Occured No occur No occur No occur
Of melting the formation No occur No occur No occur No occur No occur
Whether or not hole occurs, the No occur No occur No occur No occur No occur
number of holes and the size of the
largest hole (mm)
Warp towards Whether any flame reaches the upper Occured Occurred No occur No occur No occur
edge of one of the vertical edges
Flame burn time after flame 59 s 52 s No occur No occur No occur
Burning with cinder after flames Occured Occured No occur No occur No occur
Of melting the formation No occur No occur No occur No occur No occur
Whether or not a hole occurs, the No occur No occur No occur No occur No occur
number of holes and the size of the
largest hole (mm)

Figure 12. Application of vertical combustion test for untreated fabric.

after flame was withdrawn from these fabric samples (Table
3). Some images were given in Figures 12 and 13 due to
understanding of the test application for the untreated sample.
Performance and structural features of fabrics
In untreated and with each solution treated fabrics, weights
(in grams per square meter) were measured, and their
warp-weft density were counted as below:
In untreated denim fabrics: Weft density 17, warp density:
28, weight: 405 g/m2, fabrics treated with containing nano
SiO2, weft density: 17, warp density: 27, weight: 408 g/m2,
fabrics treated with containing Boric acid; weft density: 17,
warp density: 27, weight: 455 g/m2, fabrics treated with conta-
ing borax; weft density: 17, warp density: 27, weight: 456 g/
m2. The warp-weft density and tear strength (Table 4) of
denim fabrics treated with finishing solutions containing
boric acid and borax chemicals did not change significantly,
but their weight increased.
When the stretch and growth values of denim fabrics were
measured, the stretch (%) is between 15 and 17% (Table 5).
It is stated that elasticity value above 15% is acceptable
according to usage area (El-Ghezal et al., 2009). The elastane
yarns in fabric structure can affect physical properties such as
weight, weft density, tensile strength, wrinkle resistance,
explosion, air permeability (Ertaş et al., 2016).
The weight change occurring in fabrics was calculated by
the formula 1.
 
Wincrease ð%Þ ¼ ðW2  W1Þ=W1 x 100 (1)
W1: Weight of the denim before coating, W2: Weight of
the denim after coating, Wincrease: Mass increase value
of denim
 THE JOURNAL OF THE TEXTILE INSTITUTE 11

Figure 13. Application of vertical combustion test for treated fabric.

Table 4. Strength results of fabrics.

Tear-strength Tear-strength Break-strength Break-strength
Fabric type (weft-tear) cN (Warp-tear) (weft-break) cN (warp-break) cN
Un treated 3181.3 Not tearing 405.1 2262.0
With boric acid 3048.8 Not tearing 390.0 2144.0
With borax 3059.8 Not tearing 387.2 2115.0
With NanoSiO2 3060.2 Not tearing 391.2 2132.8

Table 5. Elasticity values of fabrics. increased the flame resistant effect on denim fabric surfaces.
Fabric type Stretch (%) Growth(%) These compounds impacted the pyrolysis reaction, prevent-
Un treated 17.93 4.88 ing formation of flammable volatile substances and increas-
With boric acid 15.47 4.67
With borax 15.73 5.13
ing formation of residue. The effect of the commercial
With NanoSiO2 17.20 4.87 flame-retardant solution was found to increase the most
with boric acid addition. According to vertical combustion
Table 6. Weight increase after treated. tests, the combustion process continued for a short period
Fabric Mass increase (%) after flame removal in the untreated and with commercial
With only commercial solution 7,29 solution treated fabric. The burn progress was halted in the
With NanoSiO2 8.13 fabrics where boric acid, borax, nano SiO2 were added. We
With boric acid 10,42
With borax 11,37 believe that this study will be helpful for researches in field
of halogen-free flame retardants based on nanotechnology,
environmental approaches, protective clothing designs and
Considering that boric acid and borax collapse on fabric synergistic element combinations.
surface, it is expected that the greatest increase in weight As a result, stress and recovery data, the balance between
will occur in solutions containing boric acid and borax. The flammability performance and physical properties, perform-
least weight gain was obtained with low molecular diameter ance and comfort can be explained as follows:
SiO2 nano powder (Table 6). Fabrics used on the ground provide properties such as
breaking, tearing and elongation in the final product, while
functional properties are obtained with the applied finishing
Conclusion
processes. In the study; the addition of low amounts of
The addition of low amounts of boric acid, borax, and nano boric acid, borax and nano SiO2 into a commercial flame
SiO2 to flame-retardant finish solutions used in denim fabric retardant used in textile production has given promising
production yielded promising results in improving flame results in improving the flame retardant performance of the
retardancy performance of the commercial finish solution. commercial finish. These added compounds have been
By creating a synergistic effect usingdirect substances add- shown to affect the combustion reaction of the fabric, pre-
ition, which is an easy and feasible method, it is possible to venting the formation of flammable volatiles and increasing
increase the flame retardancy performance in known finish- the formation of residues. It has been observed that the fire
ing chemicals and meet increasing consumer expectations. resistance performance of denim fabric can be increased
The presence of boric acid, borax, and nano SiO2 compo- with LOI and TGA data. Adding elastane to denim fabrics
nents in flame-retardant finish solution formulation provided an effect to increase the comfort of clothing.
12 N. BECENEN AND G. EYİ
However, it is thought that the use of higher amounts of
elastane may have a negative effect in terms of tear strength.
The results of the study clearly showed that the elastane in
fabric structure and the finishing processes applied have a
significant effect on the mechanical and thermal comfort
properties of denim fabrics.
Acknowledgements
We thank Trakya University TUBAP-2017/219 for financial support.
We (Assist prof.Dr. Nilg€ un Becenen and G€ okhan Eyi) confirm that
‘Trakya University’ only provided financial support within the scope of
the project for chemicals and tests appliedand we declare that the sup-
port received did not lead to any conflict of interests regarding the
publication of this manuscript. There is no need for Trakya
University’s confirmation to publish this manuscript.
Disclosure statement
No potential conflict of interest was reported by the authors.
References
Birnbaum, L. S., & Staskal, D. F. (2004). Brominated flame retardants:
Cause for concern. Environmental Health Perspectives, 112(1), 9–17.
https://doi.org/10.1289/ehp.6559
Chivas, C., Guillaume, E., Sainrat, A., & Barbosa, V. (2009).
Assessment of risks and benefits in the use of flame retardants in
upholstered furniture in continental Europe. Fire Safety Journal,
44(5), 801–807. https://doi.org/10.1016/j.firesaf.2009.03.009
Didane, N., Giraud, S., Devaux, E., Lemort, G., & Capon, G. (2012).
Thermal and fire resistance of fibrous materials made by PET con-
taining flame retardant agents. Polymer Degradation and Stability,
97(12), 2545–2551. https://doi.org/10.1016/j.polymdegradstab.2012.
07.006
Dipietro, J., Stepniczka, H., & Nametz, R. C. (1971). A study of flamma-
bility of cotton, polyester, and their blends. Textile Research Journal,
41(7), 593–599. https://doi.org/10.1177/004051757104100707
El-Ghezal, S., Babay, A., Dhouib, S., & Cheikhrouhou, M. (2009).
Study of the impact of elastane’s ratio and finishing process on the
mechanical properties of stretch denim. Journal of the Textile
Institute, 100(3), 245–253. https://doi.org/10.1080/
00405000701757925
€
Ertaş, O. G., Zervent Unal, B., & Çelik, N. (2016). Analyzing the effect
of the elastane-containing dual- core weft yarn density on the
denim fabric performance properties. The Journal of the Textile
Institute, 107(1), 116–126. https://doi.org/10.1080/00405000.2015.
1016319
Forouharshad, M., Montazer, M., Moghadam, M. B., & Saligheh, O.
(2011). Flame retardant wool using zirconium oxychloride in vari-
ous acidic media optimized by RSM. Thermochimica Acta, 516(1-2),
29–34. https://doi.org/10.1016/j.tca.2011.01.007
Gbewonyo, S., Carpenter, A. W., Gause, C. B., Mucha, N. R., & Zhang,
L. (2017). Low thermal conductivity carbon fibrous composite nano-
material enabled by multi-scale porous structure. Materials &
Design, 134, 218–225.
Horrocks, A. R. (2008). Flame retardant/resistant textile coatings and
laminates. In A. R. Horrocks and D. Price (Eds.), Advances in fire
retardant materials (pp. 159–187). Woodhead Publishing.
Horrocks, A. R. (2011). Flame retardant challenges for textiles and
fibres: New chemistry versus innovatory solutions. Polymer
Degradation and Stability, 96(3), 377–392. https://doi.org/10.1016/j.
polymdegradstab.2010.03.036
Horrocks, A. R., & Anand, S. C. (2000). Heat and flame production. In
A. Richard Horrocks and Subhash C. Anand (Eds.), Handbook of
Technical Textiles (pp. 223–263). The Textile Institute.
Horrocks, A. R., Nazare, S., & Kandola, B. (2004). The particular flam-
mability hazards of night-wear. Fire Safety Journal, 39(4), 259–276.
https://doi.org/10.1016/j.firesaf.2003.11.005
ISO 13937-1:2000 :Textiles — Tear properties of fabrics — Part 1:
Determination of tear force using ballistic pendulum method
(Elmendorf). https://www.iso.org/standard/23369.html
ISO 13934-1:2013: Textiles — Tensile properties of fabrics — Part 1:
Determination of maximum force and elongation at maximum force
using the strip method. https://www.iso.org/standard/60676.html
ASTM D2594 - 04 :Standard Test Method for Stretch Properties of
Knitted Fabrics Having Low Power. https://www.astm.org/
Standards/D2594.htm
ISO 13934-1,2013: Textiles — Tensile properties of fabrics — Part 1:
Determination of maximum force and elongation at maximum force
using the strip method. https://www.iso.org/standard/61739.html
https://www.sigmaaldrich.com/catalog/product/aldrich
ISO 4589-2: 2017. Plastics- Determination of burning behaviour by oxy-
gen index - annual book of ASTM standards.
Kamath, M. G., Bhat, G. S., Parikh, D. V., & Condon, B. D. (2009).
Processing and characterization of flame retardant cotton blend
nonwovens for soft furnishings to meet federal flammability stand-
ards. Journal of Industrial Textiles, 38(3), 251–262. https://doi.org/
10.1177/1528083708098912
Kaynak, H. K. (2017). Optimization of stretch and recovery properties
of woven stretch fabrics. Textile Research Journal, 87(5), 582–592.
https://doi.org/10.1177/0040517516632480
Laoutid, F., Bonnaud, L., Alexandre, M., Lopez-Cuesta, J. M., &
Dubois, P. (2009). New prospects in flame retardant polymer mate-
rials: From fundamentals to nanocomposites. Materials Science and
Engineering: R: Reports, 63(3), 100–125. https://doi.org/10.1016/j.
mser.2008.09.002
Levchik, S. V., & Weil, E. D. (2008). Developments in phosphorus
flame retardants. In Advances in Fire retardantmaterials (pp. 41–66).
Woodhead Publishing.
Liang, S., Neisius, N. M., & Gaan, S. (2013). Recent developments in
flame retardant polymeric coatings. Progress in Organic Coatings,
76(11), 1642–1665. https://doi.org/10.1016/j.porgcoat.2013.07.014
Liu, X., & Yu, W. (2006). Evaluating the thermal stability of high per-
formance fibers by TGA. Journal of Applied Polymer Science, 99(3),
937–944. https://doi.org/10.1002/app.22305
Meerts, I., Letcher, R. J., Hoving, S., Marsh, G., Bergman, A., Lemmen,
J. G., Burg, B., & Brouwer, A. (2001). In vitro estrogenicity of poly-
brominated diphenyl ethers, hydroxylated PBDEs, and polybromi-
nated bisphenol A compounds. Environmental Health Perspectives,
109(4), 399–407. https://doi.org/10.1289/ehp.01109399
Mettler, M. S., Vlachos, D. G., & Dauenhauer, P. J. (2012). Top ten
fundamental challenges of biomass pyrolysis for biofuels. Energy &
Environmental Science, 5(7), 7797–7809. https://doi.org/10.1039/
c2ee21679e
Morgan, A. B. (2019). The future of flame retardant polymers – unmet
needs and likely new approaches. Polymer Reviews, 59(1), 25–54.
https://doi.org/10.1080/15583724.2018.1454948
Nawaz, N., Troynikov, O., & Watson, C. (2011). Evaluation of surface
characteristics of fabrics suitable for skin layer of firefighters pro-
tective clothing. Physics Procedia, 22, 478–486. https://doi.org/10.
1016/j.phpro.2011.11.074
Neisius, M., Stelzig, T., Liang, S., & Gaan, S. (2014). Flame retardant
finishes for textiles. Functional finishes for textiles: Improving comfort,
performance and protection. Woodhead Publishing.
Quede, A., Mutel, B., Supiot, P., Jama, C., Dessaux, O., & Delobel, R.
(2004). Characterization of organosilicon films synthesized by N2-
PACVD. Application to fire retardant properties of coated polymers.
Surface and Coatings Technology, 180-181, 265–270. https://doi.org/
10.1016/j.surfcoat.2003.10.067
Schindler, W. D., & Hauser, P. J. (2004). Flame-retardant finishes.
Chemical Finishing of Textiles, 98–116.
Shete, A. V., Sawant, S. B., & Pangarkar, V. G. (2004). Kinetics of flu-
id–solid reaction with an insoluble product: Zinc borate by the reac-
tion of boric acid and zinc oxide. Journal of Chemical Technology &
Biotechnology, 79(5), 526–532. https://doi.org/10.1002/jctb.1018

Stegmaier, T., Mavely, J., & Schneider, P. R. Shishoo (Ed.) (2005).
High-performance and high-functional fibres and textiles. In
Textiles in sport. Woodhead Publishing, 89–119.
Tabuani, D., Bellucci, F., Terenzi, A., & Camino, G. (2012). Flame
retarded Thermoplastic Polyurethane (TPU) for cable jacketing
application. Polymer degradation and stability, 97(12), 2594–2601.
Troitzsch, J. H. (1998). Overview of flame retardants. Chemistry Today, 16.
Varghese, N., & Thilagavathi, G. (2015). Development of woven stretch
fabrics and analysis on handle, stretch, and pressure comfort. The
Journal of the Textile Institute, 106(3), 242–252. https://doi.org/10.
1080/00405000.2014.914652
Waaijers, S. L., Kong, D., Hendriks, H. S., de Wit, C. A., Cousins,
I. T., Westerink, R. H., & Parsons, J. R., David M. Whitacre (Ed.).
(2013). Persistence, bioaccumulation, and toxicity of halogen-free
flame retardants. In Reviews of environmental contamination and
toxicology (pp. 1-71). New York: Springer.
Wang, Z., Han, E., & Liu, F. (2007). Influence of nano-TiO2 in thermal
behavior of fire-resistant coating. Journal of Materials Science and
Technology, 23, 547–550.
THE JOURNAL OF THE TEXTILE INSTITUTE 13
Weil, E. D., & Levchik, S. V. (2008). Flame retardants in commercial
use or development for textiles. Journal of Fire Sciences, 26(3),
243–281. https://doi.org/10.1177/0734904108089485
Wimmer, W., Z€ ust, R., & Lee, K. M. (2004). Ecodesign implementation:
A systematic guidance on integrating environmental considerations
into product development (Vol. 6). Springer Science & Business
Media.
World Fire Statistics. (2017). International Bulletin of the World Fire
Statistics Center.
Xie, K., Gao, A., & Zhang, Y. (2013). Flame retardant finishing of cot-
ton fabric based on synergistic compounds containing boron and
nitrogen. Carbohydrate Polymers, 98(1), 706–710. https://doi.org/10.
1016/j.carbpol.2013.06.014
Zhang, Q., Zhang, W., Huang, J., Lai, Y., Xing, T., Chen, G., Jin, G.,
Liu, H., & Sun, B. (2015). Flame retardance and thermal stability of
wool fabric treated by boron containing silica sols. Materials &
Design, 85, 796–799. https://doi.org/10.1016/j.matdes.2015.07.163
Zhao, X. (2010). Synthesis and application of a durable phosphorus/
silicon flame-retardant for cotton. Journal of the Textile Institute,
101(6), 538–546. https://doi.org/10.1080/00405000802563677