- Open Access
Copper nano-sol loaded woven fabrics: structure and color characterization
© The Author(s) 2017
- Received: 11 August 2016
- Accepted: 5 January 2017
- Published: 28 May 2017
Nano technology is an upcoming branch where lot of research work is being done with the intention of improving/changing properties of the materials. In this study polyester, cotton and polyester-cotton blended fabrics were coated with copper nano particles by pad-dry-cure technique. The morphology of nano-composite fabrics characterized using scanning electron microscope reveals that nanoparticles were dispersed on the fabric samples. The elemental analysis for confirming the presence of copper in the fabric samples was done using the Fourier transform infrared spectroscopy and energy dispersive X-ray spectroscopy techniques. The X-ray diffraction analysis of the fabric samples helped to unveil that incorporation of copper nano particles increased the d-spacing value in polyester fabric to a greater extent in comparison to the cotton and polyester-cotton blended fabrics. The nano treated woven fabric samples were dyed using myrobolan; a natural dye. The samples were evaluated in terms of colourimetric parameters and colour fastness. The copper nano-sol treatment was found to improve both K/S and colour fastness.
- Copper nano
- Natural dye
- Polymer structure
Nano particles have at least one dimension as 100 nm or less. Owing to higher surface areas nano materials can be highly reactive; hence find their application in variety of fields like medicine, electronics, food, fuel cells, batteries, water treatment, chemical sensors, pharmaceuticals, dairy industry, textiles etc. Its application is sought in textiles, to achieve improvement or change in property of the raw material or improvement in its functional properties (Chattopadhyay and Patel 2009, 2010; Patel and Chattopadhyay 2007; Patel and Patel 2012). Currently nano technology is used in textiles with the aim of furthering functional properties like dyeing, resistance to shrinkage, wrinkling, staining and flammability.
Nano application is also opted for improving the ultra violet (UV) protection, water repellency, and in odor and moisture management. They have capability to provide self cleaning and anti-bacterial properties making them popular for intimate as well as non intimate applications. In short the type of effect achieved like self cleaning/antibacterial/UV resistant and so on, is greatly dependent on the choice of nano material selected and its inherent characteristics (Patel et al. 2014; Bhattacharya and Chaudhari 2014; Shaikh et al. 2015; Chattopadhyay and Patel 2012).
Besides the nano material (filler) chosen, its degree of dispersion greatly influences the enhancement efficiency. To attain excellent properties, it is however very important that the average size of fillers present must be in the nano-meter size along with fine particle distribution in the polymer matrix after its application. Copper nanoparticles have shown a great potential as the nano-filler for hygiene application and in making textiles electrically conductive (Chattopadhyay and Patel 2011, 2012, 2013, 2014a, b).
The present study reports observations when 100% polyester (‘p’), 100% cotton (‘c’) and polyester–cotton blended (p–c; 50:50) fabric samples were treated with copper nano sol. The properties of nano-composite fabrics were evaluated in terms of morphological and chemical changes. The surface morphology has been observed using scanning electron microscopy (SEM). The chemical transformation has been analyzed using Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD) technique (http://www.intechopen.com/books/fourier-transforms-new-analyticalapproaches-and-ftir-strategies/applications-offourier-transform-infrared-spectroscopy-to-study-cotton-fibers).
Polyester, cotton and polyester–cotton fabric specifications
Fabric weight g/sq.mt
Dyes and chemicals
Myrobolan (C.I. Natural brown 6) was used as received for this study without further purification. Copper sulphate, sodium borohydride and tri-sodium citrate of analytical grade purity were procured from Sd Fine Chemicals, India.
Preparation of copper nano sol
Copper nano colloidal sol was prepared from copper salt by chemical reduction technique (Chattopadhyay and Patel 2010). “0.3 g CuSO4 was dissolved in 100 ml of distilled water. It was then kept in the reaction chamber and was slowly reduced by drop wise addition of very dilute chilled solution of sodium borohydride (NaBH4, 0.1 g dissolved in 50 ml distilled water) in nitrogen atmosphere. During the entire reaction process, the solution mixture was stirred vigorously. As the color of the solution turned to light yellow; 5 ml of trisodium citrate (C6H5Na3O7.2H2O, 0.1 g dissolved in 100 ml distilled water), was added drop by drop with vigorous stirring” (Patel and Chattopadhyay 2007). 5 g Lissapol L as surfactant was added to 100 ml of copper nano sol coating solution. The mixture was then stirred using magnetic stirrer at 250 rpm for 30 min at 60 °C temperature.
Preparation of nano copper composite fabrics
The padding liquor was applied to the ‘p’, ‘c’ and p–c fabric samples (size: 40 × 30 cm) by dipping them in the dispersion for 10 min. After which they were padded on an automatic padding mangle machine, operating at 15 rpm and 1.75 kg/cm2 pressure; using 2-dip-2-nip padding sequence at 70% expression. The padded substrates were dried at 80 °C for 5 min and cured in a preheated curing oven. Curing of ‘p’, ‘c’ and p–c fabric samples was done in oven at temperatures of 140, 120 and 130 °C respectively for 3 min.
Characterization of nanoparticles
The morphology and elemental analysis of the synthesized nanoparticles was performed using SEM (Model JSM5610LV, version 1.0, Jeol, Japan) using Oxford-Inca software (U.K.). The copper nanoparticles were examined after depositing on carbon coated aluminum sheet and further coating with gold (Au).
Characterization of fabric samples
The surface morphology of the copper loaded nano ‘p’, ‘c’ and p–c blended fabric was observed on SEM (Model JSM5610LV, version 1.0, Jeol, Japan). The presence of copper in composite fabric was confirmed by elemental analysis using Oxford-Inca software (U.K.) on the same instrument. The chemical composition of the composite material was further analyzed using FT-IR; recorded using KBr wafer on a Bomem MB series. The initial basal spacing in the fiber matrix is an important parameter for the determination of the potential for polymer intercalation. This was determined by X-ray diffractometer for ‘p’, ‘c’ and p–c blended fabrics treated with nano-copper sol. The scans were performed for each sample and the values are reported for the basal spacing. The X-ray diffraction patterns were obtained using diffractometer D8 advance with CuK α radiation (λ = 1.54 Å).
Dyeing of untreated and treated woven fabrics with natural dye
A study on the dyeing behavior using Myrobolan on woven fabrics loaded with copper nano sol was also done, in order to ascertain the change in their dyeing performance. This was executed on laboratory scale instrument, applying exhaust dyeing technique and maintaining constant dye bath temperature (Paramount instruments Pvt. Ltd., India). The dye bath liquor containing natural dye 20% (on weight of fabric-owf) and acetic acid ~2% (owf) was added to maintain dye bath pH of 5.5 in case of ‘p’ fabric whereas 2% (owf) sodium carbonate was added while dyeing ‘c’ fabric; maintaining material-to-liquor ratio of 1:40. Dyeing was started at room temperature and gradually raised to boil within 15 min; continued till 30 min at same temperature. Finally the samples were thoroughly washed and air-dried.
Dyeing of p–c blend fabric was initially started with 20% (owf) natural dye; the temperature was gradually raised to boil within 15 min and continued for 30 min. 2% (owf) sodium carbonate was then added to the dye bath and the dyeing was continued further for 15 more minutes. The samples were thoroughly washed, neutralized, and dried.
The dyed samples were assessed for K/S values using computer colour matching system (Spectra scan 5100 RT Spectrophotometer, Premier Color scan Instrument Pvt. Ltd., Mumbai/India). The light fastness of the dyed samples was tested on Fad-o-meter (FDA-R, Atlas Material Testing Technology LLC, Chicago, Ill/USA) and the wash fastness test of the samples was performed as per ISO-2 test methods in launder-o-meter (Digi.wash, Paramount Scientific Instruments Pvt Ltd., New Delhi/India). The samples were evaluated for the rating in terms of colour change.
Morphological analysis of nanoparticles
Elemental analysis of nanoparticles
Surface morphology of nano copper loaded fabric
Fourier Transform Infrared analysis
Figure 5b shows the FT-IR spectra of the untreated ‘c’ fabric samples. The fabric samples show a strong absorption band between the wavelengths of 3000–3500 cm−1. The vibrations located at 1161 cm−1 can be attributed to the anti symmetric bridge C–O–C stretching vibration, 1105 cm−1 can be attributed to the anti symmetric in-plane ring stretching band and 1056 cm−1 to C–O stretching mode.
After treatment the absorption band at wavelength of 2918 cm−1 becomes more prominent (Fig. 6b) in case of ‘c’ fabrics. Most of the peaks match each other almost exactly except the peak created at 2918.82 cm−1. It thus confirms the presence of hydrogen bond due to cellulosic nature of the parent fabric. This absorption band can be attributed to the asymmetric vibrations of –CH2 bonds. The broad absorption peak at around 3430 cm−1 is caused by the absorbed water molecules since the nano crystalline material exhibits a high surface to volume ratio and thus absorbs more amount of moisture. It is known that the usual absorption pattern in this region can be attributed to the intermolecular and intra-molecular hydrogen bonds (Ibrahim et al. 2010) of which absorption peak at 3335 cm−1 is due to intermolecular hydrogen bond.
Figure 5c shows the FT-IR spectra of untreated p–c blended fabrics. The OH and C=O absorption band at 3500 and 1600 cm−1 is respectively due to OH bond stretching and anti-symmetric stretching of carbonyl group present; attributed to the presence of cotton component. The anti-symmetric stretching band at 2945 cm−1 is due to CH2 bond, carbonyl bond stretching at 1725 cm−1, the standard stretching bond of OH at 1410 cm−1, O–CH2 stretching at 973 cm−1 and benzenoid group (Das et al. 2009) at 868 cm−1 are present by default. It will be seen that the absorption spectrum of treated p–c blended fabric samples does not show much of change (Fig. 6c). However on treatment with copper nanoparticles, additional absorption bands can be noticed at 2922.50, 1408.84, 1339.09, 894.39 and 871.81 cm−1 while other absorption spectrum remains unchanged. From results obtained for ‘p’ and ‘c’ fabrics, it becomes clear that the copper nano treatment was able to influence the cotton component while the polyester component was least affected. The changes thus observed in the absorption spectrum after treatment for p–c blended fabrics (Fig. 6c) may be due to the changes that the cotton component may have undergone.
Elemental analysis of copper nano coated fabrics
XRD analysis of copper nano loaded fabrics
XRD analysis of Cu loaded polyester, cotton and P–C blend fabric
It has also been observed that the flex width and d-spacing value in polyester-nano copper structure was higher compared to the cotton-nano copper structure or p–c blended-nano copper structure. The d-spacing value of cotton-nano copper structure is lower than polyester- nano copper structure. It may be due to the trapping of copper nanoparticles inside the ‘p’ polymer matrix which results in increased intermolecular spacing while in ‘c’ and p–c blended fabrics, the d-spacing value was found to be comparatively lower. The amorphous nature of cotton makes it incapable of trapping the nano sized copper particles.
Effect of copper nano treatment on dyeing
Colour strength values of woven fabrics dyed with natural colourant
Colour strength (K/S) values
Polyester treated with copper nano
Polyester treated with CuSO4
Cotton treated with copper nano
Cotton treated with CuSO4
Untreated P–C blend
P–C blend treated with copper nano
P–C blend treated with CuSO4
Plain woven ‘p’, ‘c’ and p–c blended fabrics were coated with nano sized copper by pad-dry-cure method. The surface morphology of woven fabrics was characterized by SEM technique and shows uniform distribution of nanoparticles throughout the fabric surface. The coated woven fabrics were further characterized by EDS and FT-IR technique; confirming the presence of copper nanoparticles on/in coated woven fabric samples. The structure of the prepared composite woven fabrics was analyzed by X-ray diffraction technique, which indicates that the d-spacing value of polyester polymeric structure was higher than the highly amorphous structure of cotton and p–c blended fabrics. In case of dyeing the improvement could not exceed that obtained using bulk conventional mordanting agent but introduction of nano copper in the system enhanced the wash fastness of dyed fabric samples. Dyeing of the nano copper loaded woven fabrics with natural dye (Myrobolan) also proved to be beneficial.
PK acquired the fabric samples and carried out the structural and elemental testing of fabric samples. BP gave copper nano treatment to the fabric samples and analysed the test results. The manuscript was jointly drafted by both the authors. Both authors read and approved the final manuscript.
The authors declare that they have no competing interests
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