textila nr1_2013.pdf

IndustriaTextilaISSN 12225347 (156)

1/2013

Recunoscut n Romnia, n domeniul tiinelor inginereti, de ctre Consiliul Naional al Cercetrii tiinifice din nvmntul Superior

(C.N.C.S.I.S.), n grupa A /Aknowledged in Romania, in the engineering sciences domain,

by the National Council of the Scientific Research from the Higher Education (CNCSIS), in group A

COLEGIULDE REDACTIE:

Dr. ing. EMILIA VISILEANUcerc. t. pr. gr. I EDITOR EF

Institutul Naional de Cercetare-Dezvoltare pentru Textile i Pielrie Bucureti

Dr. ing. CARMEN GHIULEASAcerc. t. pr. II

Institutul Naional de Cercetare-Dezvoltare pentru Textile i Pielrie Bucureti

Prof. dr. GELU ONOSEcerc. t. pr. gr. I

Universitatea de Medicin i FarmacieCarol Davila Bucureti

Prof. dr. GEBHARDT RAINERSaxon Textile Research Institute Germania

Prof. dr. ing. CRIAN POPESCUInstitutul German de Cercetare a Lnii Aachen

Prof. dr. ing. PADMA S. VANKARFacility for Ecological and Analytical Testing

Indian Institute of Technology IndiaProf. dr. SEYED A. HOSSEINI RAVANDIIsfahan University of Technology Iran

Prof. dr. FRANK MEISTERTITK Germania

Prof. dr. ing. ERHAN NERMarmara University Istanbul

Dr. ing. FAMING WANGLund University Sweden

Conf. univ. dr. ing. CARMEN LOGHINUniversitatea Tehnic Ghe. Asachi Iai

Ing. MARIANA VOICUMinisterul Economiei, Comerului

i Mediului de AfaceriConf. univ. dr. ing.

LUCIAN CONSTANTIN HANGANUUniversitatea Tehnic Ghe. Asachi Iai

Prof. ing. ARISTIDE DODUcerc. t. pr. gr. I

Membru de onoare al Academiei de tiineTehnice din Romnia

Conf. univ. dr. Doina I. PopescuAcademia de Studii Economice Bucureti

GULSAH PAMUK, FATMA CEKENComparaie ntre comportamentul mecanic al tricoturilor din bumbacconturate spaial i cel al compozitelor ranforsate cu esturi din in 37

AMINODDIN HAJI, HOSSEIN BARANI, SAYYED SADRODDIN QAVAMNIAAnaliza in situ i impregnarea cu nanoparticule de argint a esturilor din bumbac 812

MENGMENG ZHAO, JUN LI, YUNYI WANGProprietile de performan ale materialelor textile din bumbac,tratate cu microcapsule ce conin materiale cu schimbare de faz 1319

ONUR BALCI, UUR GENERAplicarea enzimelor celulazice pe esturile din bumbacPartea I. Determinarea efectului enzimelor asupraperformanei esturii 2026

GULZAR A. BAIGVopsirea prin epuizare a fibrelor acrilice cu colorani de cad 2733

MIRELA IORGOAEA - GUIGNARD, DANIELA FARM, LUMINIA CIOBANU, MIHAI CIOCOIU, STEPHANE GIRAUD, CHRISTINE CAMPAGNE, GIANINA BROASC - ASAVEIProprietile de confort ale tricoturilor cu efect de masaj 3439

FLOAREA PRICOP, RZVAN SCARLAT, CARMEN GHIULEASA, ALINA POPESCU, MARIUS IORDNESCU, IOANA CORINA MOGASisteme integrate pentru controlul i monitorizarea calitii apelor uzate 4045

DOINA I. POPESCUGreen fashion un eventual nou stil de via pentru romni 4654

DOCUMENTARE 33, 39,45, 54-55

INDEX DE AUTORI pe anul 2012 56

Editat n 6 nr./an, indexat i recenzat n:Edited in 6 issues per year, indexed and abstracted in:

Science Citation Index Expanded (SciSearch), Materials ScienceCitation Index, Journal Citation Reports/Science Edition, World Textile

Abstracts, Chemical Abstracts, VINITI, Scopus

Revist cotat ISI i inclus n Master Journal List a Institutului pentrutiina Informrii din Philadelphia S.U.A., ncepnd cu vol. 58, nr. 1/2007/ISI rated magazine, included in the ISI Master Journal List of the Instituteof Science Information, Philadelphia, USA, starting with vol. 58, no. 1/2007

1industria textila 2013, vol. 64, nr. 1


GULSAH PAMUKFATMA CEKEN

AMINODDIN HAJIHOSSEIN BARANISAYYED SADRODDIN QAVAMNIA

MENGMENG ZHAOJUN LIYUNYI WANG

ONUR BALCIUUR GENER

GULZAR A. BAIG

MIRELA IORGOAEA - GUIGNARDDANIELA FARMLUMINIA CIOBANUMIHAI CIOCOIUSTEPHANE GIRAUDCHRISTINE CAMPAGNEGIANINA BROASC - ASAVEI

FLOAREA PRICOPRZVAN SCARLATCARMEN GHIULEASAALINA POPESCUMARIUS IORDNESCUIOANA CORINA MOGA

DOINA I. POPESCU

DOCUMENTARE

INDEX DE AUTORI PE ANUL 2012

3

8

13

20

27

34

40

46

33, 39,45, 54

56

Comparison of the mechanical behavior spacer knit cotton and flax fabric reinforcedcomposites

In situ synthesis and loading of silver nanoparticles on cotton fabric

Performance properties of cotton fabrics treated with phase change materialmicrocapsules

Cellulase enzyme application for the cotton based woven fabrics Part I. Determination of effect of enzyme on the performance

The exhaust dyeing of acrylic fibers with vat dyes

Comfort properties of knitted fabrics with massaging effects

Integrated systems of monitoring and controlling wastewater quality

Green fashion a new possible lifestyle for Romanians

Documentation

Index of 2012

Revista INDUSTRIA TEXTIL, Institutul Naional de Cercetare-Dezvoltare pentru Textile i Pielrie Bucureti

Redacia (Editura CERTEX), administraia i casieria: Bucureti, str. Lucreiu Ptrcanu nr. 16, sector 3, Tel.: 021-340.42.00, 021-340.02.50/226, e-mail:[email protected]; Fax: +4021-340.55.15. Pentru abonamente, contactai redacia revistei. Instituiile pot achita abonamentele n contul nostru devirament: RO25RNCB0074029214420001 B.C.R. sector 3, Bucureti.

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Referenii articolelor publicate n acest numr al revistei INDUSTRIA TEXTIL/Scientific reviewers for the papers published in this number:

Cerc. t. gr. II dr. ing./Senior researcher dr. eng. IULIANA DUMITRESCUCerc. t. gr. III dr. ing./Senior researcher dr. eng. ALINA POPESCU

Cerc. t. dr. ing./Senior researcher dr. eng. SABINA OLARUCerc. t. ing./Senior researcher eng. LILIOARA SURDUCerc. t. ing./Senior researcher eng. RZVAN SCARLAT

Contents

industria textila 2013, vol. 64, nr. 1

The advantages of using natural fibers as rein-forcement material in composites include lowcost, high toughness, low density, good specificstrength, reduced tool wear, reduction in CO2 emis-

sions and biodegradability [1]. For instance, glassfibers have a density of 2.6 g/cm3, and cost between$ 1.30 and $ 2.00/kg as being a conventional rein-forcement material [2]. The energy consumption toproduce a glass fiber mat is 54.7 MJ/kg [3]. However,a natural fiber like flax, have a density of 1.5 g/cm3. Itcosts $ 0.22 $ 1.10/kg [2] and the energy con-sumption to produce a flax-fiber mat is 9.55 MJ/kg(including cultivation, harvesting, and fiber separa-tion) [3]. The lower density of natural fibers is a bigadvantage in the application areas where even asmall amount of weight reduction is significant. Sucha case stands out especially for automotive sectorwhich is a major composite material user. Accordingto an estimate, about 25% reduction in the weight ofa vehicle is equivalent to a saving of 250 million bar-rels of crude oil and reduction in CO2 emissions to

the tune of 220 billion pounds per annum [4]. In addi-tion to the advantages of natural fibers, quantified tar-gets for the reuse and recycling and recovery of endof life vehicles, established by European Union andAsian countries, played an important role for theauto motive sector to become an important area thatmarks out a future in natural fiber usage. TheEuropean Union published a directive in 2000 by the

aim of increasing the rate of re-use and recoveryfrom 75% to 85% in terms of average weight pervehicle/year by 2006, and to 95% by 2015, and toincrease the rate of reuse and recycling over thesame period to at least 80% and, respectively, 85%in terms of average weight per vehicle/year [5].Recently, the potential of natural fiber reinforcedcomposites has been attractive for researchers, andthe researches have widely studied interfacial prop-erties of composites and worked for modifying thenatural fiber for better matrix-fiber adhesion or theresultant performance of the natural fiber reinforcedcomposite [622]. In these studies the natural fiberreinforcements are in the form of random mat, non-woven mat or basic woven fabric. Only Carvalho etal. [12, 15] used jute flat knitted fabrics for the rein-forcement of composites. The objective of the pre-sent work is different from those of the studies givenabove. Our aim is to analyze the difference of flaxand cotton fabric composites in terms of tensile, com-pression and impact strength, also to understand themechanical contribution of fibre and yarn inlay inthese composites.

EXPERIMENTAL PART

Preform manufacturingThe flax yarn used in the present work is 49.56 2 tex and has 0.029 kgF/tex specific strength whilecotton yarn is 49.7 2 tex and 0.017 kgF/tex specific

REZUMAT ABSTRACT

Comparaie ntre comportamentul mecanic al tricoturilor din bumbac conturate spaial i cel al compozitelor ranforsate cu esturi din in

Fibrele naturale ofer multe avantaje pentru compozitele textile ranforsate. Principalele obiective ale acestui studiu con-stau n transformarea fibrelor din bumbac i in n preforme tricotate i utilizarea lor ulterioar n calitate de ranforsripentru compozite, precum i analiza avantajelor ecologice i de mediu ale acestora. Scopul lucrrii l constituie studiereadiferenei dintre compozitele din in i cele din bumbac, n ceea ce privete rezistena la traciune, compresie i impact,i evidenierea comportamentului mecanic al acestora, n urma inserrii de fibre i fire naturale n aceste compozite.

Cuvinte-cheie: compozite, ranforsri textile, proprieti mecanice, preforme tricotate, fir de bumbac, fir de in

Comparison of the mechanical behavior spacer knit cotton and flax fabric reinforced composites

Natural fibers offer many advantages in textile reinforced composites. The main purpose of this study was to turn cot-ton and flax fibers into knitted preforms, then to use these preforms as reinforcement to examine their ecological andenvironmental advantages that they provided to the knitted preforms. Our aim was to analyze the difference of flax andcotton fabric composites in terms of tensile, compression and impact strength, also to understand the mechanical con-tribution of fibre and yarn inlay in these composites.

Key-words: composites, textile reinforced, mechanical properties, knitted preforms, cotton yarn, flax yarn

Comparison of the mechanical behavior spacer knit cotton and flax fabricreinforced composites

GULSAH PAMUK FATMA CEKEN


strength. Two types of spacer fabrics were knitted inorder to produce preform on 7E Stoll CMS 440 elec-tronic knitting machine. To improve the fibre weightfraction in the preform, weft insertion was madebetween two spacer fabric layers. Also we managedto insert fibre inlay between two fabric layers of spac-er fabrics. This way we were able to examine theeffects of fibre inlay. As can be seen from figure 1 the knitting report of thefirst type spacer fabric is composed of four courses.In the first course the yarn knits on front, in the sec-ond course yarn knit on the rear, in the third courseyarn or fibre inlay is inserted and the two layers offabric is connected by tuck stitches in the fourthcourse. In figure 2, knitting report of the second type of spac-er fabric is displayed. It consists of eight courses, andmaking the knitting action both on short and longneedles is the difference of this spacer fabric from thefirst one. By using the second type of spacer fabricpreform we aimed to improve the stability of the pre-form and consequently to make the resultant strengthperformance of the composite better. The knittingparameters of preforms and properties of ultimatecomposites are given in table 1.

Composite manufacturingThe thermoset composites were manufactured fromthe preforms mentioned above. Epoxy resin wasused as matrix material. Four layers of preforms andepoxy resin were transformed into composites via thehand laying up method. They were cured at 120C forthree hours under a pressure of 250 kPa.

Material testingTensile tests were performed according to ASTM D3039-76, and were conducted in both course andwale directions under displacement control at a rateof 1 mm/minute. The dimensions of tensile test spec-imens are depicted in figure 3. Specimens were mea-sured 230 mm in length and 12 mm in width for thecourse wise tests and 25 mm in width for the wale

wise tests [23]. The tensile testing machine was oper-ated at a crosshead speed of 1 mm/minute and fivespecimens from each composite were tested.


Table 1

PRODUCTION PARAMETERS OF THE SPACER FABRIC PERFORMS AND PROPERTIES OF THE ULTIMATE COMPOSITES

Comp-ositetype

Preformtype

Knittingyarn

Weftin-lay

Knitting speed, m/s Yarn tension, cN

Stitch cam setting Fibreweightfractionof com-

posite, %

Knittingyarn

Weftinsertion

yarn

Knittingyarn

Weftinsertion

yarn

Knitting Tucking

F1 Type I Flax yarn Flax yarn 0.75 0.40 1.5 11.0 11.6 9.6 48.00F2 Type II Flax yarn Flax yarn 0.75 0.40 3.5 8.0 11.8 9.8 52.00

C1 Type ICottonyarn

Cottonyarn

0.75 0.40 1.0 5.5 11.3 9.3 37.30

C2 Type ICottonyarn

Cottonfibre

0.75 0.40 1.0 12.5 11.3 9.3 42.25

C3 Type IICottonyarn

Cottonyarn

0.75 0.40 2.5 7.0 11.8 9.8 51.80

Fig. 2. The knitting report of the second type spacerfabric preform

Fig. 1. The knitting report of the first type spacerfabric preform

Compression tests were conducted by using a modi-

fied IITRI test rig according to ASTM D 3410. The

dimensions of compression test specimens are shown

in figure 4 [24]. Compressive loads were applied at a

nominal displacement rate of 1 mm/minute, and each

of the five specimens was tested for course-wise and

wale-wise directions.

The impact resistance of composites was determined

on unnotched Charpy specimens by a procedure out-

lined in ASTM standard D 5942-96 and using a test

machine with a pendulum of 4J impact or potential

energy [25]. The testing machine is a pendulum type,

has a rigid construction, and is capable of measuring

the absorbed energy of a test specimen. The value of

this energy is defined as the difference between the

initial potential energy of the pendulum and the ener-

gy remaining in the pendulum after breaking the test

specimen. A total of five samples from each compos-

ite were tested to determine the mean impact resis-

tance.

RESULTS AND DISCUSSIONS

In this study, the composites showed better tensile

strength values in course wise tensile direction

(fig. 5), although it is well known that the wale wise

tensile strength is higher than the course wise tensile

strength in weft knitted fabric reinforced composites.

This means that weft inlay made contribution to the

strength in course wise tensile direction as we

expected.

As highlighted in Section 2.1, type II preform made

better contribution to the tensile strengths of com-

posites in both directions then type I preform.

If the cotton composites, that contain type I preforms

(C1, C2), are compared each other, C2 has the high-est course wise tensile strength value. During knitting

the preforms yarn inlays and fibre inlays were made

in C1 and C2, respectively. Although fibre has actual-ly poorer performance than yarn, in our composite it

performed better than yarn since it is more difficult for

the resin to penetrate into yarn because of the twist.

This fact is also supported by the higher wale wise

tensile strength of C1.Figure 6 shows the measured tensile modulus of the

composites. As can be seen in this figure, C1 and F1has lower course wise tensile modulus than C3 andF2 both of which were registered 12 GPa in coursewise direction. However, an increase was observed

in course wise tensile modulus with the increment of

fiber weight fraction (table 1).

Based on the results of the current study, flax com-

posite containing type I preform F1 showed inferiorcompression strength compared to cotton composite

including type I preform C1 and C2 while flax com-posite containing type II preform F2 showed inferior


Fig. 3. The dimensions of tensile test specimens:

a - tensile strength specimen in course wise(parallel to yarn inlay) direction;

b - tensile strength specimen in wale wise(vertical to yarn inlay) direction;

c - side view of tensile specimens

Fig. 4. The dimensions of compression test specimens:

a - compression strength specimen in course wise(parallel to yarn inlay) direction;

b - compression strength specimen in wale wise(vertical to yarn inlay) direction

Fig. 5. Tensile and compression strengths of composites

Fig. 6. Youngs modulus of composites

a

b

a

b

c

compression strength compared to cotton compositeinvolving type II preform C3. In this study, all type of composites showed highercompression strengths in course wise direction. Thisresult is in accordance with those obtained by tensilestrength tests. If we also compare compressionstrengths of the preforms, it is seen that type II pre-forms give better values than type I preforms. On theother hand, although C2 has better course wise ten-sile performance than C1, yarn inlay provided advan-tage to C1 in terms of compression.Impact strengths of the composites are given in fig-ure 7. This figure exhibits that impact strengths of theflax composites are superior than cotton ones.Parallel with the results obtained by compressiontests, composites that contain type II preforms, F2and C3, which have the highest fiber weight fractions(table 1), showed the highest impact strength values.

CONCLUSIONS

Cotton and flax fibers are widely used natural fibersin textile industry. The main purpose of this study was

to turn these fibers into knitted preforms, then to usethese preforms as reinforcement to examine theirecological and environmental advantages that theyprovided to the knitted preforms, because due to ourcomprehensive literature review, there seems therewerent any studies examining these advantages onthe knitted preforms. Based on the results of the cur-rent study we conclude that: Fiber inlays can be made during preform knitting; If the weft inlays were made into preforms, better

tensile, compression and impact properties areobtained in course wise direction;

The fiber inlay, made into cotton preform, is moreeffective in terms of strength than yarn inlay;

Composites which contain spacer preform that isboth knitted on short and long needles showedbetter performance than composites containingspacer preforms that is knitted with needle cancel;

Cotton composites may be preferred for treat-ments that need high tensile and compressionstrengths, but flax composites may be consideredif high impact strength is required.

It must be noted that tensile, compression and impactfailure mechanisms in composites that are producedfrom natural fiber knitted preform are rather compli-cated and call for further investigation. This investi-gation should include different knitted fabric types,natural fibers and several matrix combinations. Moreknowledge on these parameters will allow us design-ing composites with better performance.

Acknowledgements

This study was granted by Dokuz Eylul University ScientificResearch Center. The composites were produced atIzoreel Composite Insulating Materials Company. The testswere conducted at Dokuz Eylul University MechanicalEngineering Laboratories. The authors thank these compa-nies for their valuable support.


Fig. 7. Impact strengths of composites

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Authors:

GULSAH PAMUKEge University

Emel Akin Vocation SchoolTextile Department

FATMA CEKENDokuz Eylul University

Textile Engineering Department

Corresponding author:GULSAH PAMUK

e-mail: [email protected]

Fabrication of functionalized textiles by applyingnanoparticles is an interesting approach for sur-face modification of textiles [15]. As means of creat-ing new properties a considerable amount ofresearch has been carried out for immobilization ofvarious nanoparticles on textile materials, while eachof these nanomaterials are able to provide specialeffects. Among of them, silver nanoparticles (AgNPs)are widely used to create antibacterial propertiesbecause of their wide-spectrum antibacterial activity[611]. Especially, Ag exhibits non-toxicity to humancells when it is used in a reasonable amount [12]. Several methods have been applied for synthesizingsilver nanoparticles [13]. The synthesis methods ofnanosilver must correspond to its application in orderto obtain antimicrobial fabric with a broad antibacteri-al spectrum, strong antibacterial activity, short actiontime, and good washing fastness [14]. Silver nano -particles can be deposited on the textile surface sub-strate by various coating methods or can beabsorbed by exhaustion method. In addition, it is pos-sible to synthesize silver nanoparticles on textile sub-

strate by in situ method [6, 12, 1517]. Cotton fibercontains hydroxyl groups on its molecular structurewhich is able bind to positive charged species oforganic or inorganic materials. The presence of thesecharacteristic groups makes them ideal for the selec-tive binding of metal ions. Therefore, the cottonfibers' hydroxyl groups can be a suitable template togrow metal nanoparticles.The aim of this study was to synthesize silver nano -particles inside the cotton fibers obtaining durablenanosilver loaded substrate. In this case, cotton fibercan act as a template for synthesizing and growingthe silver nanoparticles. Sodium hypophosphite(SHP) (NaPO2H2), which is often applied as a reduc-

tant in nonelectrical deposition, was used as a reduc-ing agent. In addition, TiO2 nanoparticle was loaded

to cotton fabric before synthesizing silver nanoparti-cles to enhance the antibacterial effect of silvernanoparticles and reduce the yellow color appeareddue to presence of silver nanoparticles. The cottonfabrics loaded with Ag/TiO2 nanocomposite at different


AMINODDIN HAJI SAYYED SADRODDIN QAVAMNIAHOSSEIN BARANI

REZUMAT ABSTRACT

Analiza in situ i impregnarea cu nanoparticule de argint a esturilor din bumbac

Nanoparticulele de argint sunt tot mai mult folosite n diferite aplicaii, datorit proprietilor lor antibacteriene. Fibrele debumbac pot aciona ca matrice pentru stabilizarea i controlul generrii de nanoparticule de argint. Nanoparticulele deargint au fost ncorporate n fibrele de bumbac prin metoda in situ, n prezena nanoparticulelor de TiO2. Ca agentreductor a fost utilizat hipofosfitul de sodiu. Ca tehnici de analiz a caracteristicilor suprafaei esturii de bumbac tra-tate, s-au folosit microscopia electronic de baleiaj la tensiune sczut i spectrometria de absorbie n infrarou cutransformat Fourier i nregistrarea spectrelor prin atenuarea reflexiei totale. esturile din bumbac impregnate cunanocompozite pe baz de Ag/TiO2, la diferite concentraii ale nanoparticulelor de TiO2, au fost analizate prin metodaanalizei termogravimetrice (TGA) i prin metoda spectrometriei de absorbie atomic (AAS). Prezena nanoparticulelorde TiO2 alb a mbuntit proprietile esturii de bumbac impregnate i a redus indicele de nglbenire a esturii debumbac impregnat cu nanoparticule de argint.

Cuvinte-cheie: in situ, impregnare, nanoparticule, TiO2, bumbac


Silver nanoparticles are being used increasingly in various applications due to their antibacterial properties. Cotton fibercan act as a template to stabilize and control the growth of silver nanoparticles. Silver nanoparticles were synthesizedon cotton fibers by in situ method in presence of TiO2 nanoparticles. Sodium Hypophosphite (SHP) (NaPO2H2) wasused as a reducing agent. The surface of loaded cotton fabric was characterized by low voltage scanning electronmicroscopy, and attenuated total reflection-Fourier transform infrared spectrometry. The cotton fabrics loaded withAg/TiO2 nanocomposite at different TiO2 nanoparticles concentrations were examined by thermo gravimetric analysis(TGA), and atomic absorption spectrometer. The presence of white TiO2 nanoparticles enhanced the properties of load-ed cotton fabric and reduced the yellowness index of cotton fabrics loaded with silver nanoparticles.

Key-words: in situ, loading, silver nanoparticle, TiO2, cotton



TiO2 nanoparticles concentrations were examined by

thermogravimetric analysis (TGA) and attenuatedtotal reflectance infrared Fourier transform (ATR-FTIR) spectroscopy. In addition, the effect of Ag/TiO2nanocomposite concentration on yellowness Index ofloaded cotton fabrics was studied by measuringreflectance spectra. Furthermore, the water contactangle of loaded samples was examined.

EXPERIMENTAL PART

Materials usedAll chemicals used in this study were of analyticalgrade and distilled water was used throughout thework. Silver nitrate (AgNO3 extra pure, > 99.8%),

sodium hypophosphite (NaPO2H2), and citric acid

(C6H8O7) were purchased from Merck Company

(Germany). TiO2 nanopowder (Degussa P-25) was

provided by SigmaAldrich.

Fabric sample A plain woven, 100% cotton fabric with an area weightof 240 g/m2 was used in this study. In order to cleanthe fabrics from the impurities, all samples wereimmersed in a solution containing a nonionic deter-gent (1 g/l) for 30 minutes at 60C (L:G = 40:1), thenrinsed with tap water and dried at room temperature.

Methods usedSynthesis of Ag/TiO2 nanocomposite: The scoured

cotton fabric was immersed in the silver nitrate solu-tion with liquor-to-goods ratio of 1:50 for 30 minutesat room temperature. Silver ion concentration wasadjusted at 400 ppm, while the TiO2 concentration

was varied from 0 to 1.5% owf (on weight of fabric).After that, the wet fabric was dried in oven at 100Cfor 20 minutes. Reducing agent concentration wasadjusted more than the silver ions concentration onthe cotton fabrics. So, its guaranteed that the totalabsorbed Ag+ in to cotton fabric was reduced to Ag.Moreover, the higher reducing agent concentrationscreate higher nuclei which lead to smaller Ag nano -particles. The cotton fabrics impregnated with silvernanoparticles and Sodium Hypophosphite werecured at 130C for 10 minutes. This is lead to reduceAg+ to Ag atom and to the synthesis of silver nano -particles. Synthesizing silver nanoparticles on cottonfabric changes the color of cotton fabric to brownishyellow.The surface of loaded cotton fabric was character-ized with low voltage scanning electron microscopy(PHENOM SEM, FEI Company, Eindhoven, TheNetherlands). This guarantees the uncharged imag-ing of non conductive materials without sputter coat-ing.Silver loading efficiency on cotton fabric was de -termined by an atomic absorption spectrometer(Unicam 939). Approximately 1 g of each sample wasput in a porcelain crucible and burned. Temperaturewas increased from room temperature to 650C in an

hour and burning was continued for two hours. Afterthat, the burnt samples were cooled in the desicca-tors and ash weight was recorded. Then, 1 ml of hotconcentrated Nitric Acid was added to the porcelaincrucibles to dissolve all the silver content. Finally, theconcentration of each solution sample was deter-mined with the atomic absorption spectrometer.Thermo gravimetric analysis (TGA) of treated anduntreated cotton fabrics was performed with Perkin-Elmer 7 thermal analyzer. Approximately, 7 mg ofpieces of fabric was placed on the plate and heatedfrom 25C to 650C by heating rate of 10C/minuteswith nitrogen purging. The surface of all cotton samples were analyzed bythe Attenuated total reflection-Fourier transformsinfrared spectrometer (ATR-FTIR, Perkin ElmerSpectrum 100 series). ATR-FTIR spectra wererecorded at a resolution of 1 cm1 and the scanningrange was 6504 000 cm1 and an average of 20scans was recorded.The reflectance spectra of the treated and untreatedcotton fabrics were measured in the range of400700 nm with 10 nm intervals (Color Eye 7000 A,Gretag-Macbeth). The CIE terms namely, L*, a*, b*and C* color coordinates under illuminant D65 and10 standard observer were measured for evaluatingthe color of samples. The change in color of a loadedsample from untreated cotton to yellow brownish canbe described by yellowness Index which was calcu-lated from the spectrophotometer data. The yellow-ness index of the loaded fabric was determinedaccording to the ASTM E313 by equation (1) underilluminant D65 and 10 standard observer:

YI = 100(1.3013 X 1.1498 Z)/Y (1)


Synthesis of silver nanoparticles

Most textile fibers as well as cotton fiber have a neg-ative zeta potential in neutral and alkali aqueoussolutions [18]. Cotton fibers have a negative zetapotential due to acidic groups in their chemical struc-ture such as carboxyl or hydroxyl groups [19]. Silverions with positive charges can adsorb and diffuse intothe cotton fiber due to the electrostatic interaction ofnegative charge groups and positive charge of silverions (2). Silver ions can be converted to silver atomsand nanoparticles in presence of sodium hypophos-phite as a reducing agent and cotton fiber acts as atemplate and controls the growth of silver nano -particles [12].

Cotton OH Cotton Oaq

Cotton O + Ag+ Cotton O Ag+ (2)

Cotton O Ag+ + NaPO2H2 Cotton O Ag


Low voltage scanning electron microscopy(LVSEM)The morphological changes of cotton fibers surfacescaused by synthesizing Ag and Ag/TiO2 nanocom-posites were followed by LVSEM. Images of cottonfibers loaded with silver nanoparticles and Ag/TiO2nanocomposites are presented in figure1. These fab-rics were immersed in a solution containing 400 ppmsilver nitrate in presence of sodium hypophosphite. Itcan be seen obviously that the formation of nano -composites on the surface of cotton fibers has led tochange the uniform and homogeneous cotton sur-face to a rough surface [16]. In addition, the silvernanoparticles were well-dispersed on fiber surfaces.LVSEM image of loaded cotton fiber by in situmethod with silver nanoparticles and the loadedfibers with Ag/TiO2 nanocomposites are presented infigure 1a. However, the surface morphology and the Ag nano -particles density on cotton fabrics varied with theconcentration of the TiO2 in the solution (fig. 1b). Thepresence of TiO2 nanoparticles in loading solution ledto increasing of the Ag/TiO2 nanocomposite densityon the surface of cotton fabrics. In addition, increas-ing the TiO2 concentration enhanced the density ofAg/TiO2 nanocomposites on the surface of cottonfabrics (fig. 1c).

Silver content of loaded cotton fabricThe amount of the loaded silver on the cotton fabricsis presented in table 1. The obtained results showedthat the amount of silver nanoparticles on the fabricsin the presence of TiO2 is much greater than the load-ed sample without TiO2 (AT0). It is obvious that thehigher concentration of TiO2 in the recipe of immers-ing solution results to greater silver content and thesilver content of fabrics increased from 3.67 g kg1 forwithout TiO2 sample (AT0) to 12.98 g/kg

1 for the fab-ric treated with 1.5% owf of TiO2 (AT1.5).It has been reported that the colloidal solution of TiO2(1 wt%) has a negative zeta potential ( 35.5 mV)[20] and it has a negative surface charge even at

weak acidic media [21, 22]. So, the electrostatic inter-action of Ag+ to the negative surface charge of TiO2resulted to the higher silver content in presence ofTiO2. It can be assumed that loading cotton fiber withhigher TiO2 concentrations caused the formation ofmore negative sites on the surface of cotton fibersand is suggested a more hydrophilic fiber surface[23], facilitating the subsequent interaction andadsorp tion of Ag+. Consequently, the amount of syn-thesized silver nanoparticles on the cotton fabricsincreased. This result was confirmed with SEMimages that presence TiO2 lead to formation of high-er nanocomposites density on the surface of loadedcotton.

Thermogravimetric analysisThe thermal properties of the loaded cotton fabricswere analyzed and compared to untreated sample asmeans to estimate the amount of Ag/TiO2 nanocom-posites on the loaded samples. The TGA curves ofuntreated and treated cotton fabrics with Ag andAg/TiO2 nanocomposites are presented in figure 2. Itcan be seen that sample loaded with Ag/TiO2 (AT1.5)presented a more weight loss at the initial tempera-ture range compared to the other sample which cor-responds to the vaporization of H2O adsorbed physi-cally on the surface of loaded fabric [23] due to more

Table 1

Fig. 1. LVSEM image of loaded cotton fiber by in situ method with: a - silver nanoparticles and the loaded fibers with Ag/TiO2 nanocomposites; b - at different concentrations of TiO2;

c - 0,51% on weight of fabric

a b c

THE SILVER NANOPARTICLES CONTENTOF LOADED COTTON FABRICS DETERMINEDBY ATOMIC ABSORPTION SPECTROMETER

Samplecode

Recipe componentconcentration Silver

content,gkg1Ag,

ppmTiO2,

% (owf)AT0 400 0 3.67

AT0.5 400 0.5 7.42

AT1 400 1 9.12

AT1.5 400 1.5 12.98

hydrophilic surface of treated cotton fiber [24]. It canbe seen that a sharp weight loss begins at about350C, and continues till 700C, which can beattributed to a significant thermal decomposition ofcotton fiber. However, the weight loss of sampletreated with Ag/TiO2 (86%) is lower than the sampletreated with Ag nanoparticles (AT0, 89%) anduntreated sample (92%).

ATR-FTIR analysisFourier transform infrared with attenuated total inter-nal reflectance (ATR-FTIR) mode analysis wasemployed to examine the chemical composition ofcotton fiber surface until the depth of 500 nm [25]. So,in order to investigate the loading mechanism, ATR-FTIR measurements were carried out on the samplesover 1 800 4 000 cm1, as shown in figure 3. Thespectra of the Ag (AT0) and Ag/TiO2 (AT1.5) nano -

composite loaded cotton fabric presented a highertransmittance intensity compared to untreated cottonfabric, due to deposition of nanoparticles on the sur-face of cotton fibers. The peak at 3 300 cm1, asso-ciated with the OH groups located on the surface ofthe fabrics, got weaker, suggesting the mount of OHgroups became less. Generally, Ag and TiO2 have

high affinity toward hydroxyl groups. Therefore theOH groups take part in the loading process and con-sequently to be consumed by loading procedure [26].

Color measurementThe yellowness indexes of the untreated and treatedcotton fabrics with different concentrations of TiO2are presented in figure 4. The yellowness indexes aremeasured primarily to study the yellowing effect ofthe processing. The yellowness index measurementsshow that loading of Ag nanoparticles on cotton fab-ric leads to increase in yellowness. Higher TiO2 con-

centration led to lower yellowness indexes [27]. Thepresence of white TiO2 nanoparticles which are

attached on the cotton fabric surface resulted inincreasing of the fabric whiteness. Therefore, thehigher applied concentration of TiO2 nanoparticles on

the loaded cotton fabrics led to appear whiter.

CONCLUSIONS

Negative surface charge of cotton fibers can absorbsilver ion with positive charge due to the electrostaticinteraction. Sodium hypophosphite reduced theabsorbed silver ions to silver atom and formed Agnanoparticles. Ag/TiO2 nanocomposites formation on

the surface of cotton fibers changed the uniform andhomogeneous cotton surface to a rough surface,while well-dispersed on the surface of cotton fiber.Presence of TiO2 in loading solution resulted in the

formation of more negative site charge on the surfaceof cotton fiber and led to higher loading efficiency ofsilver nanoparticles. However, higher loading effi-ciency led to enhance the thermal properties of load-ed fabric with e intensity of the hydroxyl group was

reduced due to absorption of Ag/TiO2 on the surface

of cotton fiber and the OH groups took part in theloading process. Synthesizing silver nanoparticles oncotton fabric led to change the color of cotton fabricto be brownish yellow. But, the presence of whiteTiO2 nanoparticles on the cotton fabric surface

reduced the yellowness index of treated cotton fabric.

Acknowledgments

Authors would like to thank Islamic Azad University, BirjandBranch for financial support of the research project.


Fig. 2. TGA curves of the untreated and treated cottonfabric with Ag and Ag/TiO2 nanocomposites

Fig. 3. ATR-IR spectra of untreated and loadedcotton fabric

Fig. 4. Yellowness index of the untreated and treatedcotton fabric with Ag/TiO2 nanocomposites

at different TiO2 concentrations


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Autori:

AMINODDIN HAJISAYYED SADRODDIN QAVAMNIA

Textile Engineering Department, Birjand Branch Islamic Azad University

Birjand, Irane-mail: [email protected]

HOSSEIN BARANIUniversity of Birjand

Birjand, Iran

Phase change materials (PCM) are latent heatstorage materials. Unlike sensible heat storagematerials, they have much higher heat storage den-sity with a narrow temperature difference betweenstoring and releasing heat [1]. They absorb heat inthe heating process as they change phase from solidto liquid (melting process) and release heat in thecooling process as they undergo a reverse phasechange (crystalizing process). During the melting andcrystalizing process, the temperature of the materialsremains constant [2]. Based on these merits ofPCMs, they have been applied to develop smarttextiles and clothes to improve thermal comfort forhuman bodies. Because in the melting process theywill change from a solid phase to a liquid phase,these materials have to be encapsulated as PCMmicrocapsules [36] or encapsulated as PCM packs[710] before they are used in textile and clothing. There are many kinds of PCMs, like hydrated salt,fatty acids, and mixed compounds of organic andinorganic [12, 1112]. The most well-known PCMs

for textile and clothing oriented microcapsules areparaffin wax based materials, like n-octadecane andn-eicosane etc. They have high latent heat and theyare non-toxic and non-corrosive. Furthermore, theirphase change temperatures are in the temperaturerange (about 18 to 35C) in which human bodies canremain thermally comfort [5]. The diameters of PCMmicrocapsules are only a few micrometers. Hence,they can be incorporated into fibers or textiles.Incorporating PCM microcapsules into fibers can beachieved by wet spinning or melt spinning [13, 14].Whereas the modified fibers are confined to a limitedheat capacity with low PCM microcapsule loadingcontent. Another way to incorporate PCMs into tex-tiles is achieved by coating process. This finishingprocess includes knife over roll, screen printing, paddry cure, etc. Polymer binders, like polyurethane, arerequired to link the microcapsules permanently onthe fabric substrate. A high loading content can begained by a coating process [5, 11, 15].

Performance properties of cotton fabrics treated with phase changematerial microcapsules

MENGMENG ZHAO JUN LIYUNYI WANG

REZUMAT ABSTRACT

Proprietile de performan ale materialelor textile din bumbac, tratate cu microcapsule ce conin materiale cu schimbare de faz

n ultimele decenii, n scopul mbuntiriii proprietilor de confort termic ale corpului omenesc, n textile i confecii aufost ncorporate microcapsule PCM. n cadrul acestui studiu, pentru tratarea unor materiale textile din 100% bumbacs-au utilizat dou tipuri de microcapsule ce conin materiale cu schimbare de faz, pe baz de n-alcani, folosind raclucontra rol. Morfologia suprafeei materialelor textile astfel tratate difer n funcie de adaosul de microcapsule PCM. Deasemenea, capacitatea de stocare a cldurii de ctre aceste materialele textile crete odat cu creterea cantitii demicrocapsule PCM. Pe de alt parte, permeabilitatea la aer i la vaporii de ap scade odat cu creterea adaosului demicrocapsule PCM. Pe msur ce cldura latent a materialelor textile astfel tratate crete, vor crete i coeficienii detransfer termic, ns rezistena termic va scdea. Rezultatele obinute au indicat faptul c materialele textile astfeltratate au o bun capacitate de reglare termic.

Cuvinte-cheie: microcapsule PCM, materiale textile din bumbac, morfologia suprafeei, permeabilitate la aer, rezistentermic, coeficient termic, reglare termic

Performance properties of cotton fabrics treated with phase change material microcapsules

PCM microcapsules have been applied in textile and clothing in the past decades to improve thermal performance prop-erties for human bodies. In the research we used two types of n-alkane based phase change material (PCM) micro-capsules to treat 100% cotton fabrics, by a knife over roll method. The surface morphologies of the treated fabrics weredifferent under different add-on levels. Heat storage capacities of the treated fabrics increased as the add-on of PCMmicrocapsules increased. Both air and water vapour permeability became lower as the add-on increased. Heat transfercoefficients of the treated fabrics became higher as the latent heat of the treated fabrics increased, whereas heat resis-tances of the treated fabrics changed in a reverse direction. The results indicated that the treated fabrics had the abili-ty to regulate thermal effect.

Key-words: PCM microcapsules, cotton fabric, surface morphology, air permeability, water permeability, heat resis-tance, heat coefficient, thermal regulate effect


The technology of incorporating PCM microcapsulesinto clothing was developed in the early 1980s undera NASA program. The purpose of the program was toimprove the thermal performance of astronautsspace suits in extreme conditions [2]. Later on, PCMmicrocapsules were employed in textiles and clothingfor ordinary people. In the same time, related research-es in material science, textile and clothing sciencehave been conducted. Sarier and Onder [6] estab-lished a manufacturing technique to accomplish PCMmicrocapsules that could be applied to different tex-tiles. Shin et al. [15] reported that the add on of poly-mer binders and PCM microcapsules on fabric struc-ture could lead to a change of fabrics tensilestrength, drape and hand, as well as air and watervapour permeability. Kim and Cho [16] used PCMmicrocapsules containing octadecane to treat poly -ester fabrics by a knife over roll method. They foundthat the durability of microcapsules lasted for aboutten launderings. The mean skin temperature andmicroclimate temperature with the treated garmentwere less compared with the untreated garment.Bendkowska et al. [7, 11] used a TRF (temperatureregulating factor) index defined by Hittle and Andre[17] to evaluate thermal performance of fabrics treat-ed with PCMs. Ying et al. [18] used the indices ofthermal regulating capacity to describe thermal regu-lating performance of textiles incorporated with PCMmicrocapsules and found that they were stronglydependent on the amount of PCM add-ons. After a literature review, the authors find that the typeof PCM microcapsules, i.e. the phase change tem-perature, the latent heat of the PCM and the add-onlevels, together with the fishing process have greateffect on performance properties of the treated fab-rics. Hence, in the study two types of PCM microcap-sules are utilized and they are treated on cotton fab-rics at different add-on levels. The surface morphology,air and water vapour permeability and thermal regu-lating ability of the treated fabrics were investigatedto give a better understanding of this technology.

EXPERIMENTAL PART

Materials used Two types of PCM microcapsules were supplied byBeijing Julong Bofang Science and TechnologyInstitute. The cores of the two types of PCM micro-capsules were paraffin based materials. For technol-ogy right, we just knew that the core materials weren-alkane materials. The shells of the PCM microcap-sules were mainly melamine-formaldehyde poly-mers. The average diameters of the microcapsuleswere less than 3 ms (fig. 1).Figure 1 shows the surface morphology of the PCMmicrocapsules. The photographs were taken byscanning electron microscope (S-3000N, Hitachi Japan). Their heat characteristics were tested by dif-ferential scanning calorimeter (204F1, Netzsch Germany). The melting temperatures of PCM Type Iand Type II are 33.9C and 27.2C, respectively.

Their melting enthalpies were 139.5 J/g and 160.3 J/g,respectively.A 100% cotton fabric (plain weave, 118 g/m2, thick-ness of 0.24 mm) was used as the substrate. PCMmicrocapsules were first dispersed in aqueous solu-tion of surfactant, dispersant. In a research conduct-ed by Salaun et al. [4], they report that a poly -urethane based binder is the most suitable to linkmelamine-formaldehyde microcapsules. Thus we chose a polyurethane binder (PU3630,Hefei Anke China) to link the microcapsules on thecotton fabrics surface. The composition of the PCMmicrocapsules and the binder were churned up even-ly to treat the cotton fabrics by a knife over rollmethod. The treated fabrics were then dried in roomtemperature.In this research different amount of PCM microcap-sules were used to treat the cotton fabrics. The add-ons of the microcapsules are presented in table 1. Inthe table, the treated fabrics area weight included thePCM microcapsules weight and the polyurethanebinders weight. The add-on is calculated by equation(1) [5]:

add-on = 100% (1)

where:a is the cotton fabrics weight after coating; b the cottons fabrics weight before coating.

Testing methodsScanning electron microscope (S-3000N, Hitachi Japan) was used to observe the surface morphologyof the coated fabrics. The coated fabrics latent heat characteristics weretested by differential scanning calorimeter (204F1,Netzsch Germany). The heating and cooling ratewas 10C/minute under N2 atmosphere. The heating

and cooling temperature range was from minus 50Cto 100C.Air permeability of the coated fabrics was measuredby an apparatus (YG461E, China). The testingmethod was in equivalent to ISO 9237-1995. Air per-meability was determined by measuring the flow rateof the air passing through the tested fabric area at apressure difference of 100 Pa. A water vapour permeability tester (M261, SDL Atlas USA) was applied to test the coated fabrics water


a ba

Fig. 1. PCM microcapsules with core material of type 1taken by SEM:

a - magnification 3 000x, 10.0 kV; b - magnification 10 000x,10.0 kV, the average diameter was less than 3 ms

a b

vapour permeability. The testing method was in accor -dance with ASTM E96 in a temperature of 20C,65% RH. The water vapour permeability (WVP) ing/m2/day is calculated by equation (2).

WVP = (2)

where:M1, M2 are the mass of the testing assembly before

and after the specimens exposed period; A is the area of the exposed specimen, m2; t the exposed time, h;M1, M2 are measured with an electrical balance capa-

ble of weighing to an accuracy of 0.001 g. A guarded hot plate apparatus (YG606E, China) wasemployed to test the coated fabrics thermal regulat-ing effect. The apparatus consist of three hot plates,namely the testing plate, the bottom plate and theguard plate. The latter two plates prevent heat leak-age and guarantee that heat loss is toward the verti-cal direction. The fabric samples were conditioned inroom temperature (20C, 65% RH) for 24 hoursbefore tested. The fabric side without PCM micro-capsules was toward the test plate (fig. 2). The tem-peratures of these plates were maintained at 35C.The test was conducted in a temperature of 20C,65% RH. Heat resistances and heat transfer coeffi-cients of the treated fabrics were measured. Theheat resistances (Rct) of the samples are calculated

by equation (3). Each fabric sample was tested forthree times.

Rct = Ro (3)

where:Rct, Ro are the heat resistance of the tested fabric

and the boundary air layer respectively,m2 C/W;

A is the specimens area, m2; Q the electrical power, W.


The treated fabrics surface morphology Figure 3 and figure 4 show the surface morphologiesof two pieces of the treated fabrics taken by SEM.Figure 3 is a coated fabric with a 28.2% add-on. Fromfigure 3, we can see that PCM microcapsules wereembedded on the surface of the cotton fibers and inthe pores between the fibers. They were linked to thefabric substrate with the help of the polymer binder.Because the add-on was not too high, the surfacetexture of the fabric substrate could still be seen. Figure 4 is a coated fabric with a higher add-on levelof 35.1%. As shown in the figure, PCM microcap-sules and the polymer binder covered all the surfacearea of the fabric substrate. The substrates surfacetexture could not be seen any more. Thus the add-onsof PCM microcapsules changed the cotton fabrics


Note: Fab-I symbolizes the fabrics coated with PCM microcapsules of Type I and Fab-II symbolizes the fabrics coated with PCM Type 2. No. 1 to 6 means the different add-on levels.

Table 1

A(Ts Ta)Q

24(M1 M2)At

DIFFERENT ADD-ONS OF THE COATED FABRICS

Fabriccode

Thickness,mm

Area weight,g/m2

Ratio of mass PCM microto mass binder

Add-on,%

Fab-substrate 0.24 118 - 0

Fab-I/1 0.25 174 1:4 28.2

Fab-I/2 0.26 181 1:4 35.1

Fab-I/3 0.27 203 1:4 41.9

Fab-II/4 0.25 153 1:4 23.1

Fab-II/5 0.26 169 1:4 30.2

Fab-II/6 0.27 190 1:4 37.9

Fig. 2. The schematic diagram for thermalregulate effect test

a bFig. 3. The surface morphology of cotton fabric treated

with PCM microcapsules with a 28.2% add-on: a - magnification 1 000x, 10.0 kV; b - magnification

3 000x, 10.0 kV

surface morphology greatly. The change of the sur-face morphology will bring changes in fabrics tensilestrength, hand and other surface physical properties[15, 16], which will change clothing wearing properties.

Heat storage capacity of the treated fabrics The heat storage capacity of the treated fabrics test-ed by DSC is listed in table 2. In the last column heatstorage was expressed in kJ/m2 by multiplying heatstorage in J/g with the area weight in g/m2 [11]. In thisway the heat storage capacity per area could beachieved, which was more suitable for clothing usage. As shown in table 2, with a higher add-on level theheat storage capacity became higher. This was inaccordance with other researches [15, 16]. In theresearch conducted by Shin et al. [15], n-eicosane isused as the core material of PCM microcapsules. The latent heat of fusion of their PCM microcapsulesis 134.3 J/g. The treated fabric with a 22.9% add-onis capable to absorb 4.44 J/g heat when it undergoesphase change. In our research, the latent heat offusion of PCM microcapsules was higher than that inShin et. al. research. Therefore, the heat storagecapacity of the coated fabrics was higher. The treat-ed fabric with a 23.1% add-on of PCM Type II wascapable to absorb 12.62 J/g heat. Furthermore, thefabrics treated with PCM Type II had a higher heatstorage capacity than the fabrics treated with PCMType I, because PCM Type II had a higher latentheat.From table 2 it can also be seen that the melting tem-peratures of phase change are decreased comparedwith the melting temperature before coated (33.9C

and 27.2C, respectively). The melting temperaturesof phase change treated by PCM Type I decreasedby 5 to 5.4C. The other ones treated by PCM TypeII decreased by 3.2 to 4C. This phenomenon wasalso seen in the researches of Shin et al. [15] andKim et al. [16]. The reason was not clear. It might bethat in the coating process the PCM microcapsuleswere affected to some extent either by the knife overroll process or by the polymer binder.

Air and water vapour permeabilityof the treated fabricsThe performance properties of the treated fabrics,including air and water vapour permeability and ther-mal regulating capacity are listed in table 3. It can beseen from table 3 that after coating the air perme-ability of the treated fabrics decreased dramatically.The air permeability of the cotton fabric before coat-ed was 1083.35 cm3/cm2/min, but after being coatedit decreased to very low levels. When the add-on was 28.2%, the air permeabilitywas only 25.32 cm3/cm2/minute.Figure 5 shows the change of air permeability oftreated fabrics under different add-ons. We can seethat under a higher add-on level the treated fabricsair permeability became lower. The reason might bethat PCM microcapsules and the polymer binderwere embedded in the pores of the cotton fibers andyarns. They blocked the passing channel of the airand they made the fabrics thicker. This might be good


Fig. 4. The surface morphology of cotton fabric treatedwith PCM microcapsules with a 35.1% add-on:

a - 1 000x, 10.0 kV; b - magnification 3 000x, 10.0 kV

Fig. 5. Air permeability of the treated fabricswith different add-ons

a b

Table 2

THE HEAT STORAGE CAPACITY OF THE COATED FABRICS

Fabriccode

Thickness,mm

Tm,g/m2

Heat storage,Hm, J/g

Heat storage,Hm, KJ/m2

Fab-substrate 0 - - -

Fab-I/1 28.2 28.5 9.49 1.65

Fab-I/2 35.1 28.8 11.69 2.12

Fab-I/3 41.9 28.9 15.3 3.10

Fab-II/4 23.1 24 12.62 1.93

Fab-II/5 30.2 23.2 19.02 3.21

Fab-II/6 37.9 23.9 21.60 4.09

in the winter situation. The coated fabrics could beused as outer wears to keep cold wind out andrelease heat to keep the body warm.Like air permeability, water vapour permeability of thecoated fabrics also decreased after being treated byPCM microcapsules. But compared with air perme-ability, water vapour permeability was decreased notas much as air permeability (table 3). The watervapour permeability of the cotton fabric before coatedwas 815.774 g/m2/day. When the add-on was 41.9%of the highest among the add-ons, water vapour per-meability was decreased by 52.2% compared withthe one before coated. Figure 6 shows the trend of water vapour permeabil-ity of the treated fabrics under different add-ons. Asshown in the figure, with a higher add-on of PCMmicrocapsules, water vapour permeability of thecoated fabrics became lower. Water vapour perme-ability determines how much sweat vapour can betransferred to the ambient environment. The higherwater vapour permeability the more sweat vapourcan be transmitted to the outside environment.Therefore, it relates greatly to human body comfort[1921]. The purpose of coating PCM microcapsulesis to improve clothing thermal regulating capability,but it should not reduce other clothing performanceproperties. Therefore, in the near future a better

method that can improve water vapour permeabilityof the treated fabrics should be developed.

Thermal regulating effect of the treated fabrics

When the fabrics were tested on the hot plate, thesurface temperature of the hot plate was controlled at35C to simulate body skin temperature at a comfortrange. The ambient temperature was controlled at20C, so temperature gradient appeared and heatfrom the hot plate was lost to the environment.Because there were fabrics between the hot plateand the ambient environment, heat loss was blocked.This is how heat resistance happens. Different fab-rics have different heat resistance ability, dependingon the fabrics thickness and structure [22, 23]. Whennormal cotton fabrics are used as heat regulatingmaterials, their performance properties are limited.But when PCM microcapsules were used to treat thefabric substrate, this problem could be quite different,as show in table 3 of the changed heat resistancesand heat transfer coefficients. When the relationship of the heat transfer coefficientwith the heat storage capacity of the treated fabricsis plotted, we can see that the higher heat storagecapacity (also latent heat) the higher heat transfercoefficients of the coated fabrics were (fig. 7).


Table 3

THERMAL AND MOISTURE PROPERTIES OF THE COTTON FABRICS BEFORE AND AFTER COATING

Fabriccode

Add-on,%

Airpermeability,cm3/cm2/min.

Water vapourpermeability,

WVP,g/m2/day

Heatrezistence,

Rct,m2 C/W

Heat transfercoefficient,W/m2 C

Fab-substrate 0 1083.35 815.774 0.0177 0.0572

Fab-I/1 28.2 25.32 561.787 0.0234 0.0429

Fab-I/2 35.1 21.61 456.230 0.0246 0.0409

Fab-I/3 41.9 16.01 389.703 0.0189 0.0537

Fab-II/4 23.1 25.70 549.073 0.0137 0.0734

Fab-II/5 30.2 24.47 527.489 0.0186 0.0540

Fab-II/6 37.9 18.91 421.045 0.0190 0.0528

Fig. 6. Water vapour permeability of the treated fabricswith different add-ons

Fig. 7. The relationship of heat transfer coefficient withheat storage capacity of the treated fabrics

However, heat resistances of the treated fabrics werein the opposite situation (fig. 8). In the test, the sub-strate side without PCM microcapsules was in con-tact with the testing plate ((fig. 2). When heat lossfrom the hot plate passed through the fabric sub-strate and reached the PCM membrane, the micro-capsules began to absorb heat and stored it as thetesting plates temperature was higher than the PCMmicrocapsules phase change temperature. When thePCMs melted completely, heat storage was finishedand gradually a steady thermal state was reached.The higher heat storage capacity of the treated fab-rics, the more heat was absorbed and stored. Hence,more heat from the hot plate was transferred to thePCM microcapsules. Figure 9 shows the comparison of the fabrics heatresistances treated by the two types of PCM micro-capsules. From figure 9 we can see that fabrics treat-ed by PCM Type I had higher heat resistance com-pared with fabrics treated by PCM Type II. This canbe explained by the findings of Gao et al. [8]. In theresearch the authors find out that the higher of thetemperature gradient between the thermal manikinssurface temperature and PCMs melting temperaturethe more heat is lost from the manikin to the environ-ment. Fabrics treated by PCM Type I had higher melt-ing temperature. Their temperature gradient betweenthe hot plate and the PCM membrane was lowercompared with that of fabrics treated by PCM Type II.Moreover, fabrics treated by PCM Type I had lowerheat storage capacity than fabrics treated by PCMType II. Thus less heat was absorbed and lost fromthe fabrics coated by PCM Type I.Besides, as can be seen from figure 9 that heat resis-tances of the treated fabrics had no clear relationshipwith the different add-on levels. Fabric treated byPCM Type I with a 35.1% add-on level had the high-est heat resistance. While the fabric treated by PCM

Type II with a 23.1% add-on level had the lowest heatresistance. And fabrics treated by PCM Type II with30.2% and 37.9% add-on levels had almost the sameheat resistances with the fabric treated by PCM TypeI of 41.9 % add-on. In a research conducted by Yinget al. [18], the authors also find that static heat resis-tances of fabrics treated by PCM microcapsules haveno clear linear relationship with PCM load content.They are independent on PCM load content. Theauthors did not explain the reason. In our view, thereason might be complicated. Many factors affectfabrics heat resistance, like the fabrics thicknessand structure, e.g. air in the fiber and yarns [22, 23].Although fabrics after being treated by PCMs had thecapability to absorb heat from the hot plate whichcould decrease heat resistances to some extent, theybecame thicker and they blocked heat loss to theenvironment. Furthermore, after being treated thepores of the fabrics were embedded with PCM micro-capsules, so less air was trapped in the fabrics [11].

CONCLUSIONS

Two types of paraffin based PCM microcapsuleswere applied to treat cotton fabrics by a knife over rollmethod. The PCM microcapsules were embedded onthe surface of the fabrics and changed the fabricssurface morphology, air and water vapour permeabil-ity, as well as thermal regulating capacity. Still furtherresearches on subject wear trials should be carriedout to further validate the thermal regulate effect ofthe treated fabrics.

Acknowledgements

The authors would like to thank the financial support ofDissertation Innovation of Donghua University for Doctoralstudents (BC201116), National Natural Science Foundation(51106022) and Doctoral Program of Higher Education ofChina.


Fig. 8. The relationship of heat resistance with heatstorage capacity of the treated fabrics

Fig. 9. Comparison of the heat resistances of fabricstreated with the different types of PCM and add-ons

BIBLIOGRAPHY

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[2] Mondal , S. Phase change materials for smart textiles An overview. In: Applied Thermal Engineering, 2008,vol. 28, p. 1 536


[3] J in , Z. , Wang, Y. , L iu , J . e t a l . Synthesis and properties of paraffin capsules as phase change materials. In:Polymer, 2008, vol. 49, p. 2 903

[4] Salan, F. , Devaux, E. , Bourb igot , S. e t a l . Application of contact angle measurement to the manufac-ture of textiles containing microcapsules. In: Textile Research Journal, 2009, vol. 79, p. 1 202

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[6] Sar ier, N. , Onder, E. The manufacture of microencapsulated phase change materials suitable for the designof thermally enhanced fabrics. In: Thermochimica Acta, 2007, vol. 452, p. 149

[7] Bendkowska, W. , K lonowska, M. , Kopias, K. e t a l . Thermal manikin evaluation of PCM cooling vests.In: Fibres and Textiles in Eastern Europe, 2010, vol. 18, p. 70

[8] Gao, C. S. , Kuk lane, K. , Holmr, I . Cooling vests with phase change material packs: The effects of tem-perature gradient, mass and covering area. In: Ergonomics, 2010, vol. 53, p. 716

[9] Gao, C. S. , Kuk lane, K. , Holmr, I . Cooling vests with phase change materials: The effects of melting tem-perature on heat strain alleviation in an extremely hot environment. In: European Journal of Applied Physiology,2011, vol. 111, p. 1 207

[10] Reiner tsen, R. E. F. H. Optimizing the performance of phase-change materials in personal protective cloth-ing systems. In: International Journal of Occupational Safety and Ergonomics, 2008, vol. 14, p. 43

[11] Bendkowska, W. , Wrzosek, H. Experimental study of the thermoregulating properties of nonwovens treatedwith microencapsulated PCM. In: Fibres and Textiles in Eastern Europe, 2009, vol. 76, p. 87

[12] Za lba, B. , Mar n , J . M. , Cabeza, L . F. e t a l . Review on thermal energy storage with phase change:Materials, heat transfer analysis and applications. In: Applied Thermal Engineering, 2003, vol. 23, p. 251

[13] Gao, X. Y. , Han, N. , Zhang, X. X. e t a l . Melt-processable acrylonitrile-methyl acrylate copolymers andmelt-spun fibers containing micro PCMs. In: Journal of Materials Science, 2009, vol. 44, p. 5 877

[14] Zhang, X. X. , Wang, X. C. , Tao, X. M. e t a l . Energy storage polymer/micro PCMs blended chips and ther-mo-regulated fibers. In: Journal of Materials Science, 2005, vol. 40, p. 3 729

[15] Shin, Y. , Yoo, D. I . , Son, K. Development of thermoregulating textile materials with microencapsulatedphase change materials (PCM). IV. Performance properties and hand of fabrics treated with PCM microcapsules.In: Journal of Applied Polymer Science, 2005, vol. 97, p. 910

[16] K im, J . , Cho, G. Thermal storage/release, durability, and temperature sensing properties of thermostatic fabricstreated with octadecane-containing microcapsules. In: Textile Research Journal, 2002, vol. 72, p. 1 093

[17] Hi t t le , D. C. , Andr, T. L . A new test instrument and procedure for evaluation of fabrics containing phase-change material. In: Atlantic City, NJ, 2002, p. 175

[18] Ying, B. A. , Kwok, Y. L . , L i , Y. e t a l . Assessing the performance of textiles incorporating phase changematerials. In: Polymer Testing, 2004, vol. 23, p. 541

[19] Holmer, I . , E lnas, S. Physiological evaluation of the resistance to evaporative heat transfer by clothing. In:Ergonomics, 1981, vol. 24, p. 63

[20] Haveni th , G. , Heus, R. , Lotens, W. A. Clothing ventilation, vapour resistance and permeability index:changes due to posture, movement and wind. In: Ergonomics, 1990, vol. 33, p. 989

[21] Wang, F. M. , Wang, S. Y. Characterization on pore size of honeycomb-patterned micro-porous PET fibersusing image processing techniques. In: Industria Textil, 2010, vol. 66, p. 66

[22] Frydrych, I . , Dz iworska, G. , B i lska, J . Comparative analysis of the thermal insulation properties of fabricsmade of natural and man-made cellulose fibres. In: Fibres and Textiles in Eastern Europe, 2002, vol. 10, p. 40

[23] Holcombe, B. V. , Hoschke, B. N. Dry heat transfer characteristics of underwear fabrics. In: Textile ResearchJournal, 1983, vol. 53, p. 368

Authors:

MENGMENG ZHAOYUNYI WANG

Protective Clothing Research Centre of Fashion Institute of Donghua University

Shanghai, 200051, China

JUN LIKey Laboratory of Clothing Design & Technology

Ministry of EducationDonghua University

Shanghai, 200051, China

Corresponding author:JUN LI

email: [email protected]

Enzymatic treatment has been a focus of the inter-est for the cotton wet processing with differentexperimental study in the textile literature [110]. Thehistory of the modern enzyme technology reallybegan in 1874 when the Danish chemist ChristianHansen produced the first specimen of the rennet byextracting dried calves stomachs with saline solu-tion. Enzymes have been used for over fifty years toremove starch-based sizes in the textile industry.Over the last decade, the textile wet processing indus -try has become more familiar with the use of the sev-eral enzymes for the different processes [8, 11, 12].Various types of the enzyme can been applied of dif-ferent stages of the woven and knitted fabrics in themanufacturing process to improve the desired prop-erties such as handle, appearance and other surfacecharacteristic. The cellulase enzymes used for the

bio-polishing and the stone washing processes canbe accepted as the one of the most common appli-cations. During the last decade, the enzymes for thecellulose as cellulase, catalase etc. have generallyreplaced the traditional stone-washing of the denimgarments and found applications in the finishing fab-rics and clothing from cotton, linen and regeneratedcellulose [1, 8]. Bio-polishing applied with the cellulase enzymeemploys basically cellulose action to remove the finesurface fuzz and the fibrils from the cotton and theviscose fabrics. The bio-polishing can be used toclean up the fabric surface after the primary fibrilla-tion of a peach skin treatment and prior to a sec-ondary fibrillation process which imparts interestingthe fabric aesthetics [12, 13].The commercial cellulase may contain mixtures ofdifferent cellulases, and the effects on the fabricproperties depend on this composition. For instance,one component may decrease the pilling but reduces

Cellulase enzyme application for the cotton based woven fabrics Part I. Determination of effect of enzyme on the performance*

ONUR BALCI UUR GENER

REZUMAT ABSTRACT

Aplicarea enzimelor celulazice pe esturile din bumbacPartea I. Determinarea efectului enzimelor asupra performanei esturii

S-a studiat procesul de prlire din cadrul tehnologiilor clasice de pretratare a esturilor din bumbac, cu scopul de apreveni formarea pilingului i a pilozitii pe suprafaa esturii. n aplicaiile industriale, n cazul acestui tip de estur,chiar n prezena procesului de prlire, se poate aplica i un tratament cu enzime celulazice, att pentru prevenireaformrii pilingului, ct i pentru mbuntirea tueului i aspectului suprafeei. n lucrare s-a studiat efectul i necesita-tea aplicrii enzimelor celulazice pe esturi din bumbac, alturi de procedeul de prlire aplicat n cadrul procesului depretratare. n plus, a fost investigat aplicarea tratamentului enzimatic n funcie de vopsire. n cadrul primei pri a fostanalizat efectul aplicrii unui surplus de enzime asupra performanei esturii. S-au efectuat determinri ale proprieti-lor fizice, cum ar fi: rezistena, pilingul, rezistena la abraziune, i analiza SEM, n conformitate cu standardele interna-ionale. Potrivit rezultatelor, aplicarea enzimelor a afectat n mod negativ proprietile fizice i chimice ale produsuluifinal.

Cuvinte-cheie: rezisten la abraziune, biolustruire, celulaz, piling, rezisten, estur

Cellulase enzyme application for the cotton based woven fabrics Part I. Determination of effect of enzyme on the performance

There was singeing process in the classic pretreatment processes of the cotton based woven fabric to prevent formingof the pill and hairiness on the surface of the fabric studied. However, in the industrial applications, even though the pres-ence of the singeing process, the cellulase enzyme treatment which was also made for preventing pilling could beapplied to this kind of fabric to improve especially handle properties and view of the surface. In this research, the effectand necessity of the cellulase enzyme processes were investigated for the cotton based woven fabric having singeingprocess in the pretreatment line. In addition, the sequence of the enzyme treatment depending on the dyeing applica-tion was investigated. In this part, the effect of extra enzyme application on the performance of fabric was invesitaged.Some physical tests were implemented to the samples as strength, pilling, abrasion resistance, and SEM analysisaccording to the international standards. According to the results, we found out that enzyme application negativelyaffected the physical and chemical properties of final product.

Key-words: abrasion resistance, bio-polishing, cellulase, pilling, strength, woven fabric


* Part I

the tearing strength. There are three major compo-nents in the cellulases, endo-glucanases (EG), exo-glucaneses (cellobiohydrolases CBH), and B-glu-cosidases (cellobiases). A total and whole cellulasepreparation contains mixtures of these threeenzymes types. These enzymes degrade cellulose tothe glucose by hydrolyzing -1,4-glucosidic bonds inpolysaccharide molecule (fig. 1) [1, 2]. Therefore, theshort fibre ends are hydrolyzed, leaving the surfaceof the fibres free and providing a more even look[1, 13].There are several benefits resulting from the enzy-matic bio-polishing of the cellulosic woven and theknitted fabrics, as smoother surface, more attractiveappearance, better pilling resistance, more gentleand softer feel, improved drape1ability and the use ofenvironment-friendly technology [8].The hairiness and the pilling is one of the major unde-sirable and serious problems in the apparel and tex-tile products obtained both weaving and knittingmethods. As we mentioned before, these kinds ofproblems can be prevented with the help of enzy-matic treatments. However, especially for the woven fabrics, the singe-ing is the first process, and it is obvious that singeing

also reduces the hairiness of the fabric surfaces andconsequently the pilling [8]. In the textile finishing mill, the singeing and the cellu-lase enzyme treatments can find application togetheror individually for the cotton woven fabrics [11, 14]. In Part I of this experimental study, we only investi-gated the physical effect of cellulase enzyme treat-ment on the cotton based woven fabrics. As mentioned before, the main aim of the study wasdetermining of the necessity of the cellulase enzymetreatment applied as an extra process after singeing.However, before discussing of necessity of applica-tions, we must determine the physical performanceof treated specimens. In order to test the physicalperformance, we carried out some tests aboutstrength and surface character according to the inter-national standard.

EXPERIMENTAL PART

In this experimental study, 54 processed specimenswere obtained from two kinds of woven fabrics, andapplied several tests to these specimens such astensile and tearing strength and pilling.

Materials usedIn the study, two kinds of woven fabrics in which tech-nological properties were shown in table 1 were used.

PretreatmentThe pretreatment processes were implemented tothe woven fabrics by order of the singeing, washing,scouring (with peroxide-caustic) and mercerizing(with 28 Be caustic).

Enzymatic process and dyeingThe bio-polishing processes were applied to thesamples along with different finishing steps usingacid cellulase enzyme: process I (PI) without enzymatic process (no

enzyme); process II (PII) enzymatic treatment after pre-

treatment (before dyeing); process III (PIII) enzymatic treatment after dyeing.In the recipe of the enzyme treatment, the wetting(1 g/l) and anti-creasing (1 g/l) agents were used withacid cellulase enzyme (Rucolaze TZE 1 g/l). Theenzymatic processes were applied by exhaust


Fig. 1. Schematic presentation of the activity of cellulaseon the cellulosic material [1]

Table 1

THE TECHNOLOGICAL PROPERTIES OF THE FABRICS

SpecimensRaw Material Lineer density,

texYarn density,

thread/cm

Mass perunit area

(grey fabrics),g/m2

Width, cm

Weave

Warp Weft Warp Weft Warp Weft

Fabric 1, F1

100% cotton(combed)

cotton ++ elastane 78 dtex

10 20 100 32 169.6 1804/1 satin

Fabric 2, F2

100% cotton(combed)

cotton ++ elastane 78 dtex

10 20 107 35 150.6 180

method in the industrial jet dyeing machine at pH55.5 and 1/10 liquor ratio, according to the graphicshown in figure 2. The enzyme used in the study wassupplied bu Rudolf & Duraner (Bursa/Turkey).The cellulase enzyme was applied at 50C during60 minutes. The entire solution was raised to a tem-perature of 80C for 10 minutes to deactivate theenzyme. According to the PI, we did not apply any enzymatic

process. However, we implemented the enzymatictreatment, according to the figure 2, before and afterdyeing in both PII and PIII, respectively. In the Part I

and Part II, with the help of these three processes,we tried to find out both the necessity of the cellulaseenzyme treatment for the fully pretreated cottonbased woven fabrics and the sequence of theenzyme process in the finishing line in Part II.The fabrics were dyed in the same jet machine at60C (izotherm method) during 60 minutes in a dye-bath containing 20 g/l salt and 10 g/l sodium bicar-bonate at pH 1112. We preferred Remazol RedRGB, Remazol Blue RR and Remazol Ultra YellowRGB (DyStar) at three different owf % as 0.5% (light)2% (medium) 3.5% (dark) in order to find out theeffect of the cellulase on the CIELab values of thedyed fabrics. The Remazol Red RGB (Reactive RedMix), Remazol Blue RR (Reactive Blue Mix) andRemazol Ultra Yellow RGB (Reactive Orange 107)reactive dyes have VS/MCT, VS/VS and VS/MCTanchor group, respectively. According to this experimental plan, 54 specimenswere obtained as shown in table 2. We did not applyany chemical or mechanical finishing process to thesamples after dyeing and enzyme processes.

Investigation methods

PillingThe pilling resistance of the fabrics was determinedusing a Martindale pilling and abrasion tester,according to EN ISO 12945-2 [15]. We finished thetest at 2 000 revolutions for two samples.

AbrasionThe abrasion character of the samples were mea-sured using Martindale pilling and abrasion tester,according to EN ISO 12947-2 (the breakdown of thespecimen) and EN ISO 12947-3 (determination of themass loss) [16]. With the help of this analysis, wetried to determine the abrasion resistance perfor-mance of the surface of the woven samples towardsexternal mechanical effects.

Weight (mass per unit area) lossThe mass per unit area of the all samples were mea-sured according to TS 251 [17]. According to theresults of this test, the weight loss formed dependingon the cellulase enzyme applications was determined.

Strength lossWe analyzed both tensile and tearing strengthsaccording to EN ISO 13934-2 and EN ISO 13937-1,respectively [18].

Microscopically observations The effects of the cellulase enzyme treatments on thesurface of the cotton based woven fabrics wereexamined by scanning electron microscopy (SEM) at50 x magnification. These searchs were made on aJeal-NeoScope scanning electron microscope(Japan) established in SKM- Kahramanmara.

RESULTS OBTAINED

Strength propertiesWe measured the tensile and tearing strength perfor-mances of all samples.

Tensile strengthThe results of the tensile strength of the F1 and F2samples can be seen in figure 3 and figure 4, respec-tively. The bio-polishing process partly hydrolyses thecotton which has a negative effect on the fabricstrength. According to the figure 3 and figure 4, ingeneral, it was determined that the tensile strengthdecreased for both F1 (no. 127) and F2 samples(no. 2854) depending on the enzyme applications


Fig. 2. The graphic of the enzymatic application

Fig. 3. Tensile strength results of F1 samples

Fig. 4. Tensile strength results of F2 samples

Acetic acid(pH 5 5.5)

Cellulase enzyme

Enzyme application

Enzyme applicationDischarge

50C 60'

80C 10'

approximately for all stages. However, it was clearthat the change on the strength showed differencesaccording to the sequence of the enzyme application(before PII or after dyeing PIII). In addition, we

found out that the strength loss was measured biggeron the samples obtained from PII than samples pro-

duced on the PIII line. In PII, we dyed samples pro-

cessed with cellulase enzyme different from PIII, and

enzyme is possible to cause damage cellulose struc-ture. Because of this possible

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