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Keywords: In the present work, a pigment-binder recipe was created by adding micro/nano-sized Molybdenum disulfide
MoS2 (MoS2) particles in two distinct concentrations of 10% and 5% to an adhesive binder and water mixture. Spray
Cotton coating was used to apply the mixture directly to the cotton cloth. The modified cotton demonstrated excellent
Antibacterial
bacterial reduction against E. coli and S. aureus. The 10% MoS2 coated fabric reduced E. coli and S. aureus by
Photocatalytic
about 98%, while the 5% MoS2 coated fabric reduced E. coli and S. aureus by 96 and 98%, respectively, during a
Coating
2 h bacterial contact period. The fabric’s antibacterial function showed impressive laundry endurance, with
bacterial reduction of more than 89% after 20 washing cycles. The fabric’s natural properties, such as water
vapor permeability, tensile strength, and abrasion resistance remained unaffected due to the loading of MoS2 on
the cotton surface. The photocatalyst MoS2 coated cotton could be used as a viable treatment against bacterial
infections and holds great promise for usage in medical textiles and everyday clothing.
1. Introduction This results in unpleasant smells, skin allergies, and other illnesses.
Thus, the finishing of cotton textile products with antibacterial protec
Cotton accounts for a substantial portion of natural textiles. Fabrics tion properties has become crucial in the textile industry. Antibacterial
made of cotton are a common choice in modern society. Cotton is known fabrics can prevent the growth and propagation of microbes like bacteria
for its comfort, smoothness, hydrophilicity, biocompatibility, and opti and fungus. These functional fabrics have garnered considerable atten
mum mechanical strength [1]. Cotton is more susceptible to microbial tion in terms of human health protection and medical treatment, with
attacks due to its higher moisture retentive capacity and porosity [2]. the intent of reducing the spread of infectious diseases [3]. According to
* Corresponding author. School of Engineering, Indian Institute of Technology Mandi, Mandi, Himachal Pradesh, 175005, India.
E-mail address: ptd1901@students.iitmandi.ac.in (A. Kumar).
https://doi.org/10.1016/j.matchemphys.2022.126658
Received 27 May 2022; Received in revised form 13 August 2022; Accepted 13 August 2022
Available online 19 August 2022
0254-0584/© 2022 Elsevier B.V. All rights reserved.
A. Kumar et al. Materials Chemistry and Physics 290 (2022) 126658
reported literature, surface antibacterial modification of cotton fabric supercapacitor electrodes while Wang et al. (2020) devised a unique
has been widely performed by embedding antimicrobial chemicals onto photo-responsive hybrid system for bacteria-killing by doping MoS2
the fabric surface. Coating, impregnation, soaking, electrospinning, nanosheets with Cu ions [27,28]. Zhu et al. (2020) loaded chito
grafting, and pad-cure techniques are widely used to provide antibac san-MoS2 with Ag-NPs on the Ti surface for bacteria killing. The coating
terial finishes to textiles [4]. The different agents including metal showed a high antibacterial reduction of more than 98.6% for both E.
nanoparticles (NPs) like silver (Ag), zinc (Zn), copper (Cu), titanium coli and S. aureus [29]. M. Li et al. (2019) prepared a MoS2-based pho
(Ti), gold (Au) and their oxides; quaternary ammonium salts like poly totherapeutic system for eliminating S. aureus bacteria biofilm from the
siloxane based, halogens like N-Halamine and chitosan are used to medical implant [30]. Based on Zn–MoS2 nanosheets, Wang et al. (2022)
enhance the antibacterial activity of textile [5,6]. He et al. (2022) pre created a biodegradable metal-organic framework that kills a significant
pared an antibacterial face mask by combining cotton with Ag/Zn amount of bacteria and speeds up the healing of bacteria-infected
coatings and electro-spun poly (vinylidene fluoride)/polystyrene nano wounds.
fibers while Cao et al. (2021) coated cotton gauze with photothermal MoS2, being photocatalytic, can produce reactive oxygen species
Au-NPs for producing the antibacterial effect [7,8]. According to Ran (ROS), which are lethal to bacteria [31,32]. The potential usage of MoS2
et al. (2020), fabrication of zeolitic imidazole frameworks skeleton-8 on in textiles has yet to be fully researched. The incorporation of these MoS2
poly-dopamine coated cotton showed effective inhibition toward E. coli particles into textile fabric could aid in the creation of smart,
[9]. Rehan et al. (2019) coated cotton gauze fabric with guava leaf self-cleaning textiles. Spray coating is an easy, quick, non-contact, and
extract mixed with sodium alginate/starch matrix. The modified cotton affordable technique that can be employed for coating textile substrate
gauze showed significant antibacterial, antioxidant, UV protection, and with minimal agglomeration. Khattab et al. (2019) prepared
wound healing characteristics [10]. water-repellent viscose fibers by spray-coating lanolin-silicon rubber
Textile bacterial reduction modes can be categorized into two with negligible agglomeration [33].
groups: release-killing and contact-killing. Antibacterial activity gets In this work, antibacterial cotton fabric was prepared by spray
reduced with the release of antibacterial agents in release-killing anti coating micro/nano-sized MoS2 onto the fabric surface. The pigment-
bacterial situations; however, the bacterial resistance will not be pre binder spray-coating process is an easy-to-manage technology for pro
vented [11,12]. Ag and other metals perform as release-killing ducing antibacterial-active coated fabric. ATR-FTIR, XRD, XPS, FE-SEM,
antibacterial agents on the textile surface. Ag-NPs coatings cannot form and TEM were utilized to characterize the prepared samples. The anti
covalent linkages with the surface of cotton fabrics, their antibacterial bacterial durability of the modified fabric, as well as its water vapor
effect’s stability and sustainability have always remained an issue. They permeability, tensile strength, and abrasion resistance, were assessed. It
agglomerate in colloidal solutions because of their high surface energy, was observed that the MoS2 coating provided remarkable bacterial ac
making it difficult to apply them to textile substrates. Further, due to the tivity reduction without affecting fabric breathability and comfort.
reactive surface of Ag, their toxicity has also become a concern [13,14].
On the other hand, a contact-killing antibacterial surface shows good 2. Experimental
biocompatibility, higher antibacterial activity, and lesser side effects.
The quaternary ammonium salts-loaded textile works on the 2.1. Materials
contact-killing principle, however, it increases the hygroscopicity of the
textile, thus providing a platform for bio-fouling [15]. A simple and The micro/nano-sized MoS2, liquid ammonia, and urea were ob
universal coating technique is required to suit the textile substrate. The tained from Sigma Aldrich, India. Cotton fabric (100% cotton, and 138
coating applied should be efficient and durable and should not affect the gsm) was provided by Vardhman Unit India. CHT India Pvt. Ltd. pro
fabric’s native properties such as water vapor permeability and me vided cross-linkable acrylate-based binder TUBVINYL ASN, and anti
chanical characteristics. In the present scenario, photocatalysis-based foaming agent KOLLASOL OCE, emulsifier TUBIGAT WAF 200,
products are appreciated over other antibacterial agents because of thickener TUBIVIS DL 600, silicone-based softener TUBISOFT PS and
their high efficiency, low cost, and non-toxicity. TiO2 has excellent fixing agent TUBIFIX HF.
photocatalytic properties and offers advantages like effective antimi
crobial properties, durability, non-toxicity, and relatively inexpensive 2.2. Stock-pigment paste preparation
[16]. However, TiO2 has a limited absorption of visible light and can
only respond to UV radiation below 387 nm [17]. Thus, the efficacy of The stock paste was initially prepared by mixing liquid ammonia
photocatalytic reduction of TiO2 is limited. (1.3%), urea (4%), antifoam agent (0.5%), emulsifier (0.5%), softener
Molybdenum disulfide (MoS2), a two-dimensional material, has (0.7%), and fixing agent with thermally cross-linkable acrylate binder
received a lot of attention among newly produced photocatalytic ma (22%) and water (67%) in a controlled fashion, accompanied by
terials because of its comprehensive surface area, open morphology, continuous mixing. The mixture was then constantly stirred for 15–20
flexible interlayer spacing, conductivity, and chemical stability [18,19]. min at room temperature. To attain the appropriate viscosity level, the
MoS2 can respond to mid-Infrared (IR) light and thus possess high thickening (4%) was incorporated into the mixture and stirred
photocatalytic reduction efficiency. Due to distinct electrical and optical constantly at 60 ◦ C for the next 10 min to achieve a homogenous stock
characteristics, MoS2 is widely used in biosensors, photodetectors, bat paste. Thereafter, micro/nano MoS2 pigment in two different weight
teries, super-capacitors, and transistors [20–23]. In addition, re concentrations of 5% and 10% were added to the stock paste and both
searchers have explored the use of MoS2 in biological applications such mixtures were stirred continuously for the next 10 min to prevent ag
as radiation protection, cancer treatment, and antibacterial agent due to gregation. The anti-foaming reduced the formation of foam in the so
its easy fabrication, relatively inexpensive, low toxicity, and good lution by lowering the surface tension. The emulsifier improved paste
biodegradability. Zhang et al. (2016) reported that cysteine-protected flow qualities and coated fabric’s soft handle, luster, and rubbing fast
MoS2 dots might be employed as radioprotectants and can be utilized ness. The thicker improved the flow of the pigment paste and gave the
in ionizing radiation protection. He suggested the use of MoS2 dots in the coating a pronounced edge and sheen.
body to remove accumulated free radicals, repair DNA, and recuperate
all key chemical and biological markers [24]. Liu et al. (2014) explored 2.3. Fabric coating process
the use of lipoic acid-modified PEG-MoS2 nanosheets as a drug carrier
for cancer treatment [25]. Xu et al. (2020) synthesized antibacterial The pristine cloth fabric was cleaned with deionized water and air
nano-structured MoS2-nanoflowers by utilizing galvanostatic electrol dried for 24 h. The coating of both prepared compositions on pristine
ysis [26]. Ali et al. (2019) explored the application of MoS2 in cotton samples (25 cm * 25 cm) was performed using automatic
2
A. Kumar et al. Materials Chemistry and Physics 290 (2022) 126658
2.4. Characterization where α is the absorption coefficient, A is a constant and υ is the tran
sition frequency.
SEM, UV–visible spectroscopy, and XRD were used to characterize Thus, the optical band gap lies well within the visible region. SEM of
MoS2 particles and pristine cotton. Perkin Elmer spectrometer-2 with pristine cotton, Fig. 1(e), showed a rough and uneven appearance of
ATR accessory was used for FTIR measurements within the spectrum fibers, with a twisted ribbon-like surface. The diffraction peaks, Fig. 1(f),
range 4000-400 cm− 1 (100 scans per sample). On a powder X-ray noticed in pristine cotton at 2θ = 15.06◦ , 16.82◦ , 22.81◦ , and 34.31◦
diffractometer (Rigaku Corporation), XRD experiments were carried correlate to cellulose 110, 110, 200, and 004 crystallographic planes
out. XPS tests were carried out using a Thermofisher scientific X-ray [39,40].
photoelectron spectrometer. The pristine and coated cotton morphology The ATR-FTIR spectrum of pristine cotton and MoS2 particles coated
was examined on Field Emission-Scanning Electron Microscope (JFEI cotton fabric is shown in Fig. 2 (a). In pristine cotton, a broad spectrum
SEM-450) with an energy dispersive X-ray spectrometer ((EDS). A high- band from 3271 to 3224 cm− 1 is related to the cellulose and water OH
resolution transmission electron microscope (HR-TEM; FP 5022/22-Tec group. The vibration of the C–H molecule is represented by the bands at
nai G2 20 S-TWIN) was used for MoS2 particle size analysis. 2977 cm− 1 and 2927 cm− 1. The band at 1626 cm− 1 corresponds to OH
Antibacterial activity was investigated by a drop cast of gram-positive bending vibration of water absorbed in cotton. The cellulose C–H
bacteria, Staphylococcus aureus (S. aureus), and gram-negative bacteria, bending was seen at 1464 cm− 1 while the peak at 1259 cm− 1 correlates
Escherichia coli (E. coli) on cotton fabric surface under visible light and in a to C–O stretching vibrations. The C–O–C asymmetric stretching of
dark atmosphere. The control sample was pristine cotton cloth. Autoclaving β-glycoside linkage was seen at 1154 cm− 1 while the band 1055 cm− 1 is
was done on 1 cm × 1 cm square test cloth specimens. The swatches were associated with C–O stretching of C-6 in cotton [41]. In MoS2 coated
then placed in a cell cultured dish under visible light. The 100 μL of the cotton, the sharp band observed from 3433 cm− 1 is associated with the
bacterial solution, both S. aureus and E. coli, were added to the swatches. A OH groups forming intra-molecular hydrogen while the band noticed at
900 μL of physiological saline solution was added to control and bacterial- 3342 cm− 1 relates to N–H stretching vibrations of the urea molecule. A
treated fabric swatches after 30 min, 1 h, 90 min, and 2 h respectively, band at 1729 cm− 1 is related to C– – O stretching while the band at 1677
− 1
followed by four serial dilutions. Agar plates were inoculated with 100 μL of cm is assigned to the C– C bond of the acrylate-based binder. The
–
the formulated bacterial solution and then maintained in an incubator at weak band generated at 467 cm− 1 is attributed to Mo–S vibration [42,
37 ◦ C for 24 h. After 24 h, the following equation was used to estimate the 43]. The FTIR spectrum authenticates that the MoS2 particles were
percentage of bacterial reduction (R %): successfully lodged on the cotton surface.
Fig. 3 shows the XRD plot of MoS2 particles coated on cotton fabric.
Y− X
R %= ∗100 (1) The MoS2 particles embedded on the cotton fabric by spray coating were
Y
identified by the diffraction peaks at 29.08◦ (004), 32.74◦ (100), 33.55◦
where X and Y, respectively represent coated and control samples bac (101), 35.98◦ (102), 39.62◦ (103), 44.28◦ (006), 49.94◦ (105), 56.14◦
terium colony forming units (CFU) [34]. (018) and 58.43◦ (110) [42,44].
The cytotoxic potential of MoS2 coated cotton against the HeLa cells Fig. 4 (a) illustrates the XPS analysis of the pristine cotton and MoS2-
was examined by a 3-[4, 5-dimethylthiazol-2-yl]-2, 5-diphenyl tetrazo loaded cotton fabric. The C 1s and O 1s binding energy signals of carbon
lium bromide (MTT) assay. The pristine cotton and coated cotton sam and oxygen present in cellulose were found to be 284.8 and 532 eV,
ples were cut into 7 mm * 7 mm pieces. After autoclaving and exposure respectively, in both samples. In the MoS2 loaded cotton, Mo (3d5/2) and
to UV light for 30 min, they were loaded in a 24-well plate. Thereafter, 1 Mo (3d3/2) binding energies, Fig. 4 (b), were found to be 228.5 and
mL of HeLa cell suspension (1 * 105 cells per mL) was seeded in each well 231.7 eV, respectively. Furthermore, the binding energies of S (2p3/2)
and cultured at 37 ◦ C in 5% CO2 for 1, 3, and 7 days. Then, the cell and S (2p1/2), Fig. 4 (c), were found to be 161.4 and 162.5 eV, respec
culture medium was replaced with 200 μL of 0.5 g/L MTT solution, and tively [45,46].
further incubated for 4 h. The culture medium was removed and 200 μL Therefore, the XRD and XPS plots validate that MoS2 particles were
dimethyl sulfoxide (DMSO) was added to dissolve the crystals. Finally, productively coated on the surface of cotton.
the optical density (OD) of the liquid was determined by measuring it The surface morphology of coated cotton was examined by FESEM,
with a microplate reader at 570 nm wavelength. The cells without cotton as presented in Fig. 5. The SEM images demonstrate that the cotton
samples were used as the control samples. Using the following equation, surface was satisfactorily embedded with micro/nano-sized MoS2 par
the relative cell viability (%) was determined: ticles after spray coating with pigment paste for both the 5% and 10%
3
A. Kumar et al. Materials Chemistry and Physics 290 (2022) 126658
Fig. 1. (a) SEM of MoS2 particles, (b–c) TEM of MoS2 particles, (d) Absorption spectrum of MoS2, (e) SEM of pristine cotton, and (f) XRD plot of pristine cotton.
Fig. 2. FTIR of (a) Pristine cotton and MoS2 particles loaded, (b) Magnified MoS2 loaded cotton FTIR curve.
4
A. Kumar et al. Materials Chemistry and Physics 290 (2022) 126658
Fig. 4. XPS spectrum of (a) Pristine cotton and MoS2 loaded cotton, (b) Mo (3d) and (c) S (2p).
Fig. 5. FESEM images of (a) 10% MoS2 coated fabric, (b) 5% MoS2 coated fabric, (c) Washed fabric (10% MoS2), (d) Washed fabric (5% MoS2), and, (e) EDX Analysis
of fabric coated with 10% MoS2 (Washed; 20 cycles).
5
A. Kumar et al. Materials Chemistry and Physics 290 (2022) 126658
Table 1 illustrates the results of a study on the MoS2 coated fabric’s By increasing the smoothness of the coated fabric’s surface, the
bacterial reduction against E. coli and S. aureus. After 30 min, 1 h, 90 min, softener aided in achieving coating results with a soft handle. The
and 2 h, the bacterial reduction percentage (R %) of fabric swatches treated measurement of water vapor permeability (breathability) of the coated
with the bacterial solution under visible light and dark atmosphere was cloth is of much importance. The water vapor permeability of pristine
measured. After a 2 h bacterial contact period, the 10% MoS2 coated fabric cotton, 10%, and 5% pigment concentration coated cotton were deter
reduced E. coli and S. aureus by around 98%, while the 5% MoS2 coated mined to be 45.4, 42.9, and 43.3 g/m2/h, respectively. The tensile
fabric reduced E. coli and S. aureus by 96% and 98% respectively. strengths of the three samples (pristine cotton, and MoS2 coated (un
The antibacterial impact of the modified cotton fabric against E. coli washed and washed) were measured as 128 N, 125 N, and 126 N,
and S. aureus is shown in Fig. 6 and 7, respectively. After continuous 20 respectively. Further, the samples showed abrasion resistance of 39000,
washing cycles, the coated cloth exhibited antibacterial reduction 38000, and 38500 rubs, respectively for pristine cotton, and MoS2
greater than 89% for both the pigment paste concentration in visible loaded (unwashed and washed), respectively. These studies reveal that
light. Therefore, from a financial perspective, fabric treated with a 5% spray coating of MoS2 onto a cotton surface does not affect the cotton’s
pigment concentration can offer excellent bacterial reduction. Even in a natural properties.
dark environment, the reduction in both bacteria increases as the bac
terial exposure time increases. 4. Conclusions
The antibacterial property of MoS2 is attributed to its photocatalyst
nature. When a photocatalyst absorbs light, the resultant electrons and Using spray coating, the nano/micro-sized MoS2 particles were
holes interact with water and oxygen forming reactive oxygen species successfully loaded on cotton fabric in varying concentrations. The
(ROS) [48,49]. ROS can destroy pathogens, including both coated fabric demonstrated a bacterial decrease of more than 96% for
gram-negative and gram-positive bacteria, by disrupting biomolecules, both strains of bacteria tested. After 20 washing, the coated MoS2
conflicting with their operation, causing cell wall collapse, and resulting remained strongly attached to the cotton surface and is efficient in
in cell malfunction. We believe an analogous effect is produced from reducing bacteria growth by 89%. The photocatalyst MoS2 loaded on
spray-coated MoS2 in the current study. Thus, the MoS2 can produce a cotton surfaces using a simple and significant spray coating technology
durable, non-toxic antibacterial effect on textile at a low cost. could be employed as possible therapeutics against bacterial infections,
and holds a lot of promise for use in regular clothing as well as medical
3.3. Cytotoxicity evaluation MoS2 coated cotton applications.
Cytotoxicity is another crucial factor affecting the utilization of any CRediT authorship contribution statement
material for industrial and medical applications in addition to antibac
terial activity. Appel et al. (2016) reported low toxicity of MoS2 against Amit Kumar: Writing – original draft, Writing – review & editing,
human epithelial kidney cells while Zhu et al. (2020) developed chito Conceptualization, Methodology, Investigation, Validation. Moolchand
san/MoS2 coating loaded with Ag-NPs on the Ti surface and reported Sharma: Data curation, Characterization, Methodology, Investigation,
that the rough surface of MoS2 facilitated cell adhesion and was Validation. Rahul Vaish: Supervision, Resources, Writing – review &
observed non-toxic to cells [29,50]. In this study, the MTT assay was editing, Formal analysis, Conceptualization, Methodology,
used to examine the prepared sample’s cytotoxicity. The cytotoxicity Investigation.
results (Fig. 8) are expressed in percentage as a reduction of viability of
cells cultured in presence of pristine or MoS2 coated cotton compared to Declaration of competing interest
cells grown in a medium without cotton samples. After 07 days of
treatment, the results presented that both the pristine cotton and MoS2 The authors declare that they have no known competing financial
loaded cotton showed excellent cell viability of more than 97% and had interests or personal relationships that could have appeared to influence
almost no cytotoxicity to cells. the work reported in this paper.
Table 1
The antibacterial effect of coated cotton.
Sr.No Samples Antibacterial Activities
E. coli
30 min 1h 90 min 2h
6
A. Kumar et al. Materials Chemistry and Physics 290 (2022) 126658
Fig. 6. Antibacterial effect of E. Coli on: (a.1-a.4) Pure cotton, (b.1-b.4) Fabric coated with 10% MoS2 (Dark), (c.1-c.4) Fabric coated with 10% MoS2 (Visible light;
Unwashed), and (d) Bacterial reduction with treatment time.
Fig. 7. Antibacterial effect of S. aureus on (a.1-a.4) Pure cotton, (b.1-b.4) Fabric coated with 10% MoS2 (Dark), (c.1-c.4) Fabric coated with 10% MoS2 (Visible light;
Unwashed), and (d) Bacterial reduction with treatment time.
Data availability
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