Maintaining hand and improving fire resistance of cotton fabric through ultrasonication rinsing of multilayer nanocoating

Thin films of environmentally benign polyelectrolytes, cationic chitosan (CH) and anionic poly(sodium phosphate) (PSP), were deposited on cotton fabric via layer-by-layer (LbL) assembly to reduce flammability. This CH–PSP nanocoating promotes charring of the cotton, rendering the fabric self-extinguishing. The coated fabric was rinsed in an ultrasonication bath between deposition steps to improve the softness (i.e., hand) of the coated fabric. Ultrasonication is believed to remove weakly adhered polyelectrolyte, preventing the fabric from becoming stiff, while improving anti-flammable behavior at a given coating weight. At 17 bilayers, only 9.1 wt% was added to the cotton, yet the coated cotton consistently passed vertical flame testing. Electron microscopy provides evidence of intumescence and confirms the cleaner deposition afforded by ultrasonication. The reduction in peak heat release rate and total heat release, as measured by micro cone calorimetry, were 73 and 81 % respectively, which is a new benchmark in LbL flame retardant coating on cotton. The mechanical properties of the fabric were measured using the Kawabata evaluation system, which showed that ultrasonication rinsing significantly improved the hand. The ability to render cotton fabric self-extinguishing, while maintaining a soft hand, marks a major milestone in the development of these environmentally-benign nanocoatings.     

Investigation on the Enhancement of Antimicrobial Activity of Neem Leaf Extract Treated Cotton Fabric Using Air and Oxygen DC Plasma

The enhancement of hydrophilicity of DC air and oxygen plasma treated cotton fabric and its effect on the antimicrobial efficacy when treated with neem leaf extract is reported in this paper. The axial and radial ion density distribution between the electrodes was studied using Langmuir probe to place the fabric between the electrodes for effective plasma treatment. The effect of system parameters viz., process gas pressure, DC power density and plasma exposure time on the hydrophilicity and hence the antimicrobial efficacy after the neem leaf extract treatment was analysed and optimised. The functional group present in the cellulose units of the cotton fabric before and after plasma treatment was identified and estimated using standard tests and analysed using ATR–FTIR spectra. The surface morphology of untreated and plasma treated cotton fabric was analyzed with the help of SEM micrograph. The mean pore diameter of the fabric matrix was calculated and air permeability was measured before and after plasma treatment to account for the improved capillarity due to plasma treatment. The formation of functional groups with increased polarity and improved capillary action of the plasma treated fabric enhances its hydrophilicity which in turn improves the sorption of neem leaf extract and hence the antimicrobial activity.     

阻燃超疏水棉纤维的制备及性能

将氢氧化镁(Mg(OH)₂)凝胶沉积到棉纤维上,以提高棉纤维表面粗糙度和阻燃性能,随后将含有Mg(OH)₂的棉纤维浸渍到聚二甲基硅氧烷(PDMS)溶液,获得阻燃超疏水棉织物。 并对棉纤维进行了傅里叶变换红外光谱仪(FTIR)、扫描电子显微镜(SEM)、疏水性、热稳定性、阻燃性能和耐久性测试。 结果表明,Mg(OH)₂负载到织物上,使得织物表面具有一定的微/纳米结构,形成了粗糙涂层。 当Mg(OH)₂浓度为1.0 mol/L时,Mg(OH)₂/PDMS改性的织物接触角(CA)可达158°,极限氧指数(LOI)提升至24.5%,导热系数为0.0525 W/(m·K), 具有超疏水和阻燃性能。 整理后织物经过20次洗涤,100次磨擦,极端条件处理后,CA仍大于150°,LOI值高于23%,显示了较好的耐久性。     

Surface Characterization and Antimicrobial Activity of Chitosan-Deposited DBD Plasma-Modified Woven PET Surface

In this work, a woven PET with an antimicrobial activity was prepared by depositing chitosan on its surface. Firstly, the hydrophilic property of the PET surface was achieved by a plasma treatment using dielectric barrier discharge (DBD). The hydrophilic property of the PET surface was characterized by wickability and contact angle measurements. The XPS analysis revealed an increment of oxygen-containing polar groups, such as C–O and O–C=O, on the PET surface after the plasma treatment, resulting in an enhanced hydrophilic property. The plasma-treated PET specimen was further deposited with chitosan by immersing in a chitosan acetate aqueous solution. The effects of temperature, chitosan concentration, and number of rinses on the amount of deposited chitosan on the PET surface were investigated. The disappearance of the above-mentioned polar groups from the PET surface was clearly observed after the chitosan deposition, indicating the involvement of these functional groups in interacting with the chitosan. The chitosan-deposited plasma-treated woven PET possessed an exceptionally high antimicrobial activity against both E. coli (gram-negative bacteria) and S. aureus (gram-positive bacteria).     

Layer-by-layer assembled thin films based on fully biobased polysaccharides: chitosan and phosphorylated cellulose for flame-retardant cotton fabric

Polyelectrolytes multilayer (PEM) films based on fully biobased polysaccharides, chitosan and phosphorylated cellulose (PCL) were deposited on the surface of cotton fabric by the layer-by-layer assembly method. Altering the concentration of PCL could modify the final loading on the surface of cotton fabrics. A higher PCL concentration (2 wt%) could result in more loading. Attenuated total reflection Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and energy-dispersive X-ray analysis directly showed that chitosan and PCL were successfully deposited onto the surface of cotton fabric. In the vertical flame test, the cotton fabric with 20 bilayers at the higher PCL concentration (2 wt%) could extinguish the flame. Microcombustion calorimetry results showed that all coated cotton fabrics reduced the peak heat release rate (HRR) and total heat release (THR) relative to the pure one, especially for (CH0.5/PCL2)₂₀, which showed the greatest reduction in peak HRR and THR. Thermogravimetric analysis results showed that the char residue at temperatures ranging from 400 to 700 °C was enhanced compared to that in the pure cotton fabric, especially in the case of higher PCL concentration (2 wt%). The work first provided a PEM film based on fully biobased polysaccharide, chitosan and PCL on cotton fabric to enhance its flame retardancy and thermal stability via the layer-by-layer assembly method.     

Synthesis of gold nanoparticles using herbal Acorus calamus rhizome extract and coating on cotton fabric for antibacterial and UV blocking applications

Gold nanoparticles (AuNPs) have been synthesized by greener method using chloroauric acid as precursor and extract of Acorus calamus rhizome as reducing agent. Formation of AuNP was confirmed by the presence of Surface Plasmon Resonance (SPR) peak in UV–Visible spectral analysis. XRD and FT-IR spectral analyses were performed for characterization. SEM images show spherical morphology and HR-TEM images reveal nanosize of AuNPs. The AuNPs were then coated on cotton fabric by pad-dry-cure method and characterized by SEM with EDAX technique. The results reveal the deposition of AuNPs on the surface of cotton fabric. Uncoated cotton, neat extract coated cotton and extract containing AuNPs coated cotton fabrics were then tested for antibacterial activity against Gram positive (Staphylococcus aureus) and Gram negative (Escherichia coli) bacterial strains by AATCC 100 test method. It showed that the extract containing AuNPs coated cotton fabric had higher antibacterial activity than other test samples against E. coli. UV-DRS analysis performed on extract containing AuNPs coated cotton fabric showed improved UV-blocking property than uncoated cotton fabric and neat extract coated cotton fabric.     

Oxidative stress induced antimicrobial efficacy of chitosan and silver nanoparticles coated Gutta-percha for endodontic applications

Root canal treatment is the most effective treatment for irreversible pulpal damage. However, it suffers the risk of failure due to micro-leakage at the Gutta-percha-sealer-tooth interface. Concerning the issue, it is important to enhance the antimicrobial properties of Gutta-percha. The current study describes a novel coating of the Gutta-percha with chitosan and silver nanoparticles to increase their antimicrobial efficacy. They were coated with chitosan and silver nanoparticles with concentrations of 1%, 2% using chemical methodology. Coated Gutta-percha were evaluated for their antimicrobial efficacy against E. faecalis, which is frequently isolated microorganism in failed endodontic cases using standard microbiological methods like growth curve analysis. Detailed analysis of the antimicrobial activity was performed by live-dead analysis with the help of flow cytometry and fluorescent microscopy. Although, the experimental analysis showed concentration-dependent antibacterial activity by both chitosan and silver NP coated Gutta-percha, the silver NP coating exhibited higher antibacterial activity compared to the Gutta percha coated with chitosan nanoparticles. Mechanistic evaluation unveiled the cause of antibacterial activates due to action of induced oxidative stress and membrane damage to the bacteria by coated nanoparticles. The information will be useful for the endodontist to have an alternative filling material with higher antibacterial potency for higher success rate of root canal therapies in clinical procedures.     

In situ production of silver nanoparticle on cotton fabric and its antimicrobial evaluation

An ecological and viable approach for the in situ forming silver nanoparticles (AgNPs) on cotton fabrics has been used. Silver nanocoated fabric of brownish yellow color (AgNPs, plasmon color) was characterized by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) and Fourier transform infrared spectroscopy (FTIR). SEM images revealed that the surface of the modified cotton was rougher than that of normal cotton. In addition, SEM images showed the presence of AgNPs on the surface of the treated fabric. Silver mapping and elemental analysis of the silver nanocoated cotton fabric using EDS confirmed the presence of AgNPs in a homogeneous distribution. Also, FTIR spectra of silver nanocoated sample showed more intense and broad peaks with a slight red shift if compared with those of blank sample indicating the binding of AgNPs with cellulose macromolecules. Different coating levels and the impact of repeated washings have been evaluated against different microbial strains by growth inhibition zone. The results of antimicrobial studies reveal that the presence of a low coating level of nanosilver is enough for producing an excellent and durable antimicrobial cotton fabrics.     

Antibacterial cotton fabric prepared by a “grafting to” strategy using a QAC copolymer

Quaternary ammonium compounds (QACs) have outstanding antimicrobial effect, but covalent immobilization of plentiful QAC onto cotton fiber surface to realize a durable function remains a challenge. Herein, a quaternary ammonium monomer, [2-(methacryloyloxy) ethyl] trimethylammonium chloride (DMC) was co-polymerized with methyl acrylate (MA) to prepare an antibacterial copolymer, poly(DMC-co-MA). To graft the copolymer with an improved grafting efficiency, cotton fabric was treated using carboxymethyl chitosan (CMC) to establish an amino-functionalized fiber surface first. This treatment allows the amidation reactions between the amino groups and the pendant ester groups in the poly(DMC-co-MA) to take place, achieving a durable anionic polymer coating onto the fiber surfaces with remarkably antibacterial effect. Characterization results indicated that when DMC/MA monomer ratio was 100:1, the resulting copolymer endows the modified cotton fabric with antibacterial capability that inactivates all Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). Even after 50 laundering cycles, more than 98.0% of the antibacterial rate could still be retained. Moreover, the wearing comfort properties such as softness, water absorption and air permeability of the finishing cotton fabrics have been insignificantly changed by comparing to the untreated cotton fabric.

     

Using graphene/TiO2 nanocomposite as a new route for preparation of electroconductive,self-cleaning,antibacterial and antifungal cotton fabric without toxicity

A novel and efficient process is reported for fabrication of electroconductive, self-cleaning, antibacterial and antifungal cellulose textiles using a graphene/titanium dioxide nanocomposite. Cotton fabric was loaded with graphene oxide using a simple dipping coating method. The graphene oxide-coated cotton fabrics were then immersed in TiCl₃ aqueous solution as both a reducing agent and a precursor to yield a fabric coated with graphene/titanium dioxide nanocomposite. The crystal phase, morphology, microstructure and other physicochemical properties of the as-prepared samples were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and UV-Vis reflectance spectroscopy. Electrical resistance, self-cleaning performance, antimicrobial activity and cytotoxicity of treated fabrics were also assessed. The electrical conductivity of the graphene/titanium dioxide nanocomposite-coated fabrics was improved significantly by the presence of graphene on the surface of cotton fabrics. The self-cleaning efficiency of the treated fabrics was tested by degradation of methylene blue in aqueous solution under UV and sunlight irradiations. The results indicated that the decomposition rates of methylene blue were improved by the addition of graphene to the TiO₂ treatment on fabrics. Moreover, the graphene/titanium dioxide nanocomposite-coated cotton samples had negligible toxicity and possessed excellent antimicrobial activity.     

Functionalization of cotton fabrics with rutile TiO<Subscript>2</Subscript> nanoparticles: Applications for superhydrophobic,UV-shielding and self-cleaning properties

The superhydrophobic cotton fabrics were prepared by combining the coating of titanium dioxide (TiO₂) with the subsequent dodecafluoroheptyl-propyl-trimethoxysilane (DFTMS) modification. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) measurements revealed that the nanosized TiO₂ sphere consisted of granular rutile. The TiO₂ layer coated on the cotton altered both the surface roughness for enhancing the hydrophobicity and UV-shielding property. The cotton fabric samples showed excellent water repellency with a water contact angle as high as 162°. The UV-shielding was characterized by UV-vis spectrophotometry, and the results indicated that the fabrics could dramatically reduce the UV radiation. The photocatalytic progress showed that organic stains were successfully degraded by exposure of the stained fabric to UV radiation. Such multifunctional cotton fabrics may have potentials for commercial applications.     

WPU/Cu2-XSe coated cotton fabrics for photothermal conversion and photochromic applications

Cellulose - Multifunctional cotton fabrics were fabricated by coating of anionic waterborne polyurethane (WPU)/Cu2-XSe. The surface morphology of WPU/Cu2-XSe coated cotton fabric was characterized...     

Improved UV stability of antibacterial coatings with N-halamine/TiO2

The outstanding advantages of N-halamine materials over other antimicrobial materials are their durable and rechargeable antimicrobial properties, as well as their efficacies in inactivating a broad spectrum of pathogens. Theoretically, the oxidative chlorine of antimicrobial cotton coated with N-halamine hydantoin diol can be restored upon loss of its biocidal efficacy after exposure to ultraviolet light. In this work nano-titania particles were added into the coating solutions containing N-halamine diol and 1,2,3,4-butanetetracarboxylic acid (BTCA), and the coatings were applied to produce antimicrobial cellulose with improved UV stability. The treated cotton fabrics were characterized by FT-IR, SEM, XRD, and XPS. The effects of the coatings on tensile strength and wrinkle recovery angle were investigated. Biocidal efficacies of fabrics coated with hydantoin diol and diol/TiO₂ against Staphylococcus aureus (ATCC 6538) and Escherichia coli O157:H7 (ATCC 43895) were determined using a modified AATCC 100-1999 method and showed excellent antimicrobial properties against these two bacterial species within a brief contact times. It was found that the addition of Nano-TiO₂ in the antimicrobial coatings, especially rutile titanium dioxide, could improve the UV light stability of the chlorinated fabrics coated with hydantoin diol significantly. The UV light stability of N-halamine coatings were enhanced with increasing amounts of rutile TiO₂.     

自支撑柔性氮掺杂碳织物电极的制备与性能研究

本文以纯棉织物为基底,吡咯单体为氮源,采用简单的原位聚合-高温煅烧的方法制备了自支撑柔性氮掺杂织物（N-CT）. 利用傅立叶红外技术、X射线光电子能谱、比表面积测试、扫描电子显微镜对所得产物进行结构与形貌表征. 结果表明,碳化后聚吡咯主要以纳米碳球包覆在碳织物表面,N-CT电极的比表面积为495.0 m²·g^-1,其含氮量为2.26%. 电化学测试表明,在0.5 A·g^-1的电流密度下N-CT电极的比电容器为256.2 F·g^-1,经过5000次的恒流充放电循环后电容保持率为98.3%,库伦效率保持率在98.8%左右,具有良好的柔性和机械性能.     

Novel UV-protective formulations for cotton, PET fabrics and their blend utilizing irradiation technique

A novel coating formulation to impart ultraviolet (UV) protection property to cotton, Polyethylene trephethalate (PET) and cotton/PET fabrics was prepared and gamma rays as an ionizing radiation was utilized for surface curing. Natural occurring aluminum potassium sulfate (Alum) was used individually and in binary coat with Zinc Oxide (ZnO), to induce the UV-blocking properties. It was found that using Alum (0.3 g/ml) caused a prompt increase in ultraviolet protection factor (UPF) over the uncoated fabrics. Moreover, the incorporated ZnO in the binary coat increased the UPF for two to threefold than the stand-alone Alum coating, specially in case of PET coated fabric. Water absorbance and moisture regain of ZnO and Alum/ZnO coated fabrics showed a decrease over the blank samples, due to the usage of oligomer/monomer combination. On contrary, Alum showed a hydrophilic effect with the increase in its content in the formulation. Surface Electron Microscope showed the homogenous coating of fibers. X-ray diffraction (XRD), energy dispersive X-ray (EDX) and water vapor permeability were also tested for coated samples.     

Multifunctional superhydrophobic/oleophobic and flame-retardant cellulose fibres with improved ice-releasing properties and passive antibacterial activity prepared via the sol–gel method

In this research, a two-component sol–gel inorganic–organic hybrid coating was prepared on a cotton fibre surface. An equimolar sol mixture of the precursors 1H,1H,2H,2H-perfluorooctyltriethoxysilane (SiF) and P,P-diphenyl-N-(3-(trimethoxysilyl)propyl) phosphinic amide (SiP) was applied to cotton fabric samples using the pad-dry-cure method. The surfaces of the untreated and coated cotton fibres were characterised using scanning electron microscopy, Fourier transform-infrared spectroscopy, X-ray photoelectron spectroscopy, and time-of-flight-secondary ion mass spectrometry. The functional properties of the coated cotton fabric samples were investigated using static contact angle measurements with water and n-hexadecane, the ice-releasing test, antibacterial testing against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli, thermogravimetric analysis in an air atmosphere, and vertical flammability tests. The results reveal the formation of a nanocomposite two-component inorganic–organic hybrid polymer network that is homogenously distributed over the cotton fibre surface. The presence of the SiP component in the two-component inorganic–organic hybrid coating did not hinder the functional properties imparted by the presence of the SiF component and vice versa, illustrating their compatibility. The cooperative action of the SiF and SiP components in the two-component coating provided the cotton fabric with exceptional multifunctionality, including simultaneous superhydrophobicity and high oleophobicity, passive antibacterial activity, and improved thermo-oxidative stability.     

Hexamethyldisiloxane‐modified ZnO‐SiO2‐coated superhydrophobic textiles for antibacterial application

A superhydrophobic cotton textile with high antibacterial properties has been fabricated. The cotton textile was coated through the in situ growth of ZnO‐SiO₂ nanoparticles in presence of chitosan as the template agent via a hydrothermal process at 95 °C. This process was followed by the coating of additional layers of hexadecyltrimethoxysilane (HDTMS). The obtained cotton textile showed antibacterial property against Staphylococcus epidermis and Escherichia coli with inhibition zones up to 18.26 and 8.48 mm, respectively. Scanning electron microscopy (SEM) revealed that the coating had a rough surface, which was attributed to the distribution of ZnO‐SiO₂ nanorods of hexagonal shape. This rough surface creates a superhydrophobic layer that repels the bacteria, as proven by the large water contact angle of approximately 150°. Nevertheless, the HDTMS layers prolong the durability of hydrophobicity for up to 3 h.     

Silver‐Doped TiO2‐Coated Cotton Fabric as an Effective Photocatalytic System for Dye Decolorization in UV and Visible Light

In this study, titanium tetra‐isopropoxide was used as a precursor of TiO₂ for in situ coating on cotton fabric by sol–gel method. Subsequently, silver nitrate was used as doping agent to prepare silver‐doped TiO₂‐coated cotton fabric during hydrothermal treatment. The treated samples were characterized through field‐emission scanning electron microscopy, energy‐dispersive X‐ray analysis, inductively coupled plasma‐mass spectroscopy and UV–visible absorption spectroscopy to study morphology, composition of deposited elements and light absorption behavior of treated samples. X‐ray photoelectron spectroscopy was carried out to analyze the electronic state of silver in TiO₂‐coated fabric after hydrothermal treatment. Doping of silver on TiO₂‐coated fabric and subsequent hydrothermal treatment was found to enhance dye decolorization rate of rhodamine B dye solution in both UV and visible light radiations with respect to undoped TiO₂. The study shows that an optimal level of silver‐doped TiO₂‐coated fabric can be used repeatedly for dye decolorization without significant loss in its photocatalytic activity. The self‐cleaning properties of samples were also studied using methylene blue as a staining agent. It was observed that the presence of 1.8% silver on the weight of titanium in doped samples provides almost 82% of stain degradation.     

Growth and fire resistance of colloidal silica-polyelectrolyte thin film assemblies

Thin films of colloidal silica were deposited on cotton fibers via layer-by-layer (LbL) assembly in an effort to reduce the flammability of cotton fabric. Negatively charged silica nanoparticles of two different sizes (8 and 27 nm) were paired with either positively charged silica (12 nm) or cationic polyethylenimine (PEI). PEI/silica films were thicker due to better (more uniform) deposition of silica particles that contributed to more than 90% of the film weight. Each coating was evaluated at 10 and 20 bilayers (BL). All coated fabrics retained their weave structure after being exposed to a vertical flame test, while uncoated cotton was completely destroyed. Micro combustion calorimetry confirmed that coated fabrics exhibited a reduced peak heat release rate, by as much as 20% relative to the uncoated control. The 10 BL PEI-8 nm silica recipe was the most effective because the coating is relatively thick and uniform relative to the other systems. Soaking cotton in basic water (pH 10) prior to deposition resulted in better assembly adhesion and flame-retardant behavior. These results demonstrate that LbL assembly is a useful technique for imparting flame retardant properties through conformal coating of complex substrates like cotton fabric.     

Using atmospheric pressure plasma for enhancing the deposition of printing paste on cotton fabric for digital ink-jet printing

Atmospheric pressure plasma (APP) treatment was applied as a pretreatment process to enhance the deposition of printing paste in order to improve the final colour properties of digital ink-jet printed cotton fabrics. Three printing pastes containing natural polymers, i.e. (1) sodium alginate, (2) chitosan and (3) sodium alginate-chitosan mixture, were prepared separately. After APP treatment, cotton fabric was padded with different printing pastes prior to digital ink-jet printing. Experimental results showed that APP pretreatment could increase the colour yield of the digital ink-jet printed cotton fabric significantly even after washing. In addition, other properties such as colour fastness to crocking, colour fastness to laundering, outline sharpness and anti-bacterial properties were also improved when compared with those of the control cotton fabric printed without APP pretreatment. However, the influence of printing paste on the colour properties of the digital ink-jet printed cotton fabrics depended very much on the composition of the printing paste. The scanning electron microscope images evidenced that the APP treatment could enhance the deposition of printing paste on the cotton fabric surface as proved qualitatively by both the contact angle and wetting time measurement as well as quantitatively by both the X-ray photoelectron spectroscopy and carboxyl group/nitrogen content analysis.