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MaterialCharacterisation StudyonRamieFibreUsing DSCTGAMethod

By: GurumurthyB.R and RadhalakshmiY.C

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MaterialCharacterisationStudyonRamieFibreUsingDSCTGA Method
By:GurumurthyB.RandRadhalakshmiY.C
LovelyProfessionalUniversity,DepartmentofFashionTechnology,Jalandhar,Phagwara CentralSilkBoard,CentralSilkTechnologicalInstitute,Bangalore Abstract DSCTGA studies are employed for material characterization, including thermomechanical analysis(TMA),dynamicmechanicalanalysis(DMA),differentialscanningcalorimetry(DSC), andthermogravimetricanalysis(TGA).However,thesecomplementarytechniquesareused for compositional and structure elucidation, and for investigating the viscoelastic propertiesoffibrousmaterials.Duringthemakingandprocessingoffibrousmaterialslike ramie, various parameters (including chemical composition and microstructure of various phases, as well as their distribution) are tightly controlled to impart the desired physical, mechanicalandchemicalpropertiestotheendproduct.Theprimeobjectiveofthisstudyis to characterize thermal properties of raw ramie fiber, evaluate and optimize the thermal behaviour curves. The phase transitions, crystallization and decomposition points are determined using DSCTGA tests conducted on ramie fiber. The thermal events are characterizedusingTGAandDSCanalyticaltechniquesandtheresultsobtainedfallwithin the acceptable norms of fiber behaviour. The results provide valuable information on selecting fibrous materials for fashion, apparels and textiles application, predict product performanceandhenceimproveproductquality.

Introduction
TheRamiefiberisoneofthestrongestvegetablefiberandpossesseshigheststrengthand length,gooddurabilityandabsorbencywithexcellentluster.Theseremarkablecharacters makeitrathermoresuitableforuseinthemanufactureofwidevarietyoftextiles,apparels andcordageproducts[Fig.2].ThePrincipalendusesofthisfiberincludeinmaking

Fabric Yarns IndustrialThreads Sacks Carpets Twine and Cordage and very recently in making fashion and apparel products, sewingthreads,parachutefabrics,wovenfirehoses,narrowweaving,canvas,filter clothbanknotes,cigarettepapers,blendedwithrayonandcotton(55%ramie/45% cotton)

Properties of ramie fiber qualify itself into a research material which is unique when comparedtoothernaturalfibers.Previousresearchonramiefocussedonstudyrelatedto dry and wet strength, elasticity properties and its mechanical behaviour. Characterisation

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studies on ramie fiber and analysis of its thermal behaviour posses new challenges in research related to ramie fibers. Even though there are numerous studies carried out on their thermal behaviour still thereexists nonlinearity in thermal fiber propertiesof ramie fibers which needs to be explored. In this study the objective is to analyze thermal propertiesusingexperimentaltechniqueslikeDSCTGAinstruments.

Harvestingramiefibres

Figure1:RamieTextileProducts Figure2:Ramieplant Ramie(Boehmerianivea(L.)Gaud,belongstoUrticaceaefamilyandisacommerciallyfiber yieldingplant.Theplantischaracterisedwithlargenumberoferectandslenderstemsor stalks,usuallynonbranchingandhas4to7leavesthataresilverywhiteunderneath,7.5to 15 cm. long with clusters of small greenish flowers[Fig.2], ranging from 8 to 16 mm in diameter.Thestalksturnbrownandwoodyastheymature Ramiefiberisnormallyharvested23timesayearbutundergoodgrowingconditionsthe plantcanbeharvested6timesayear.Thestemsareharvestedbycuttingatthebottomand thensubjectedtoextractionoffiber.TheExtractionoframiefiberisusuallycarriedoutin3 stages.Thecortexorbarkisremovedbyhandormachinewhichiscalledasdecortification. Scrapping the cortex to remove most of the outer bark is an important step during extraction. The stalks are then washed, dried and degummed to extract the spinnable fibers.Thedegummedramiefiberisthenspunonsimilarlinesasthatofacottonsystem.

PhysicalPropertiesoframiefibres Table1:Comparitivefibercompositionanalysisoframiefiber
Component(%) wax Hydrotrope Pectin Hemicellulose Lignin Cellulose(%) Gumcontent(%) Mulberrybast 0.78 15.72 11.91 34.90 22.26 14.03 56.28 Mulberyfiber 3.41 3.90 0.93 4.03 0.71 87.29 5.31 Ramiefiber 0.21.0 6.59.0 3.54.5 1.21.5 0.52.0 7077 1.767

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Table2:Comparativemechanicalpropertiesoframiefiberwithmulberryandcottonfiber
Fibers

Fineness /dtex

Modal Shortfiber Moisture length/mm content(%) regain(%)

Breaking strength/CN dex1 4.13 4.95.7 2.64.7

Breaking Initial elongation modulus/ (%) CNdtex1 2.76 1.52.5 37 103 176220 6082

Static friction factor 0.49 0.22

Dynamic friction factor 0.413 0.290.57

Mulbery fiber Ramie fiber Cotton fiber

2.57 2.86.7 1.62.5

17.8

51.7

8.5 1213 78

Mass specific resistance /.g.cm2 8.66x107 1x108 1x108

60.0250.0 2331

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TableIandIIgivescomparativevaluesofmechanicalpropertiesoframiefibers.However advantagesanddisadvantagesoframiefibersaretobeconsideredbeforedesigningan apparel.Advantagesoframiefabriccanbesummarisedasunder Ramiefabricsareresistanttobacteria,mildew,alkalis,rotting,lightandinsectattack Ramiefabricshavegoodabsorbnacyandhencearecomfortabletowear,specially duringwarmweather Theyareresistanttostainaandremovalofstainsiseasyonthesefabrics Ramiefabricsarenotharmedbymildacids Dyeingiseasy Dyedgoodshavegoodwetfastnessinlaunderingthoughdarkcolorsmayloosetheir vibrancyoverrepeatedlaunderings Smoothlusturousappearanceimproveswithwashing Ramiefabricskeepsitsshapeanddoesnotshrink Ramiefabricscanbebleached However,disadvantagesoframiefabicsinclude Havinglowelasitcity Lowabarasionresistance Theywrinkleeasily Veryhighcostduetohighlabourinvlovedinfiberextraction Ramiefiberistobedegummedpriortoprocessingwhichisanadditionalcostwhen comparedtocotton

ExperimentalmethodfordeterminationofDSCTGAoframiefiber
TheramiefiberinthisstudywasobtainedfromIndianJuteIndustriesresearchassociation, Kolkata for research purpose. Differential Scanning Calorimetry (DSC) is widely used to characterise the thermophysical properties of polymers. DSC can measure important thermoplasticpropertiesincluding:

Meltingtemperature Heatofmelting Percentcrystallinity Tgorsoftening Crystallization Presenceofrecyclates/regrinds Plasticizers Polymerblends(presence,compositionandcompatibility)

Differential scanning calorimetry or DSC is a thermoanalytical technique in which the difference in the amount of heat required to increase the temperature of a sample and referencearemeasuredasafunctionoftemperature.Boththesampleandreferenceare maintainedatverynearlythesametemperaturethroughouttheexperiment.

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Figure3:DSGTGAequipments Thebasicprincipleunderlyingthistechniqueisthat,whenthesampleundergoesaphysical transformationsuchasphasetransitions,more(orless)heatwillneedtoflowtoitthanthe referencetomaintainbothatthesametemperature.Whethermoreorlessheatmustflow tothesampledependsonwhethertheprocessisexothermicorendothermic.Forexample, asasolidsamplemeltstoaliquiditwillrequiremoreheatflowingtothesampletoincrease itstemperatureatthesamerateasthereference. Thisisduetotheabsorptionofheatbythesampleasitundergoestheendothermicphase transition from solid to liquid. Likewise, as the sample undergoes exothermic processes (suchascrystallization)lessheatisrequiredtoraisethesampletemperature.Byobserving the difference in heat flow between the sample and reference, differential scanning calorimeters are able to measure the amount of heat absorbed or released during such transitions. DSCmayalsobeusedtoobservemoresubtlephasechanges,suchasglasstransitions.DSC iswidelyusedinindustrialsettingsasaqualitycontrolinstrumentduetoitsapplicabilityin evaluatingsamplepurityandforstudyingpolymercuring.TheresultofaDSCexperimentis aheatingorcoolingcurve[Figure4].

Figure4:FeaturesofDSCcurve

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ThermoGravimetricAnalysisorTGA
Thermogravimetricanalysis(TGA)isoneofthemembersofthefamilyofthermalanalysis techniques used to characterise a wide variety of materials.TGA provides complimentary and supplementary characterisation information to the most commonly used thermal technique, DSC.TGA measures the amount and rate (velocity) of change in the mass of a sampleasafunctionoftemperatureortimeinacontrolledatmosphere.Themeasurements areusedprimarilytodeterminethethermaland/oroxidativestabilitiesofmaterialsaswell astheircompositionalproperties[4]. The technique can analyze materials that exhibit either mass loss or gain due to decomposition,oxidationorlossofvolatiles(suchasmoisture).Itisespeciallyusefulforthe studyofpolymericmaterials,includingthermoplastics,thermosets,elastomers,composites, films,fibres,coatingsandpaints.TGAmeasurementsprovidevaluableinformationthatcan be used to select materials for certain enduse applications, predict product performance andimproveproductquality.

SimultaneousDSCTGAmeasurements

Figure5:SimultaneousDSCTGAmeasurements A simultaneous DSCTGA device [Fig 5] is used to characterize ramie material exhibiting a weight change ora phase change between ambient and 1500 oC. (i.e.); the mass of a substance and the difference in energy inputs into a substance and a reference material are both measured simultaneously as a function of temperature while the substance and reference material are subjected to a controlled temperature program. The procedure followedinmeasurementofDSCTGAforramiefiberissummarisedasunder.
1. Selectthedesiredinstrumentforyourexperiment[DSCTGA]fromthethermal

analysisuserinterface 2. SelectingthedesiredmodeofoperationasDSCTGAorTGADTA 3. Selectingandpreparingasampleinvolvepreparingasampleoftheappropriatesize, selecting the sample cup, and placing the sample in the cup. For DSCTGA experiments, the ceramic (aluminum) 90L cups must be used. For TGADTA

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4.

5. 6. 7. 8.

experiment, the ceramic (40L or 90 L) or platinum (40 L or 110 L) cups are acceptable alternatives. Platinum is generally prepared for TGADTA work. All cup typesarereusable. Loadingandtaringthesamplecup(andareferencecup)onthebalance.Taringthe cups ensures that the weights measured by the balance reflect the weight of the sampleonly.Thisshouldbedonebeforeeachexperimentwiththefurnaceclosed EnteringexperimentalinformationthroughtheTAcontroller Creatingandselectingthethermalmethodonthecontroller,andscheduletherun Starting the experiment by selecting Control/Start or click the Start button on the toolbar Asresultsfromthemeasurements,onecanmonitortherealtimesignals,plot,and methodprogress

Resultsanddiscussions
TheDSCTGAcurveillustratesthechangeinheatflow,andtheDSCbaselineindicatesthe alteration of the specific heat capacity of ramie fiber. A strong endothermic peak is observedat1000C[1].Withincreasingintemperatureafastdeformationoftheramiefibers occursintheTGAgraphwhichrepresentstheprocessofthermalsofteningandfusion.At 1000CwaterisbeinglostandhencewefindapeakinDSCandalsolossinweightinTGAand then the degradation of fiber begins around 3804000C so another endothermic peak is observed.

Figure6:DSCTGAplotforramiefiber

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Conclusions The experimental DSCTGA characterization results of ramie fiber show remarkable behaviourandconfirmstotheoreticalassumptionsrelatingtothermalpropertiesoframie fiber.TheexperimentalgraphsofDSCTGAdemonstratetheglasstransitiontemperatures, Degradationtemperatures,phasetransitionsoframiefiberwhichfallwithintheacceptable normsincontexttothermalbehaviouroframiefibers.However,thischaracterisationstudy on material properties of ramie fibers helps to provide valuable information on selecting fibrousmaterialsformakingcertainfashionandapparelenduseproducts.Thestudyalso helpstopredictproductperformanceandimproveproductquality. Acknowledgements The author wishes to acknowledge Director, Indian Jute Industries research association, Kolkataforprovidingramiefibermaterialforresearch.TheauthoralsowishestothankProf. Srinivasan Raghavan (Vasu), Swati Naik, of Material Research Centre, Indian Institute of Science,BangaloreforpermittingtoconducttestsonDSCTGAInstruments.Inadditionthe author wishes to convey regards to Dr. Malavika Bihar, Product Development scientist at TiconaCelaneseCorporationforprovidingliteratureassistanceanddiscussions. References [1]ZhaoTieLiu,ZhifengSun,Zhongwenliu,JianLu,HepingXiong,Benzylatedmodification and dyeing of ramie fiber in superficial carbon dioxide, Journal of Applied polymer science,Vol.107,18721878(2008) [2]Gatewood.B.M;Wu,J.C;Roberts,A.S.Textilechem.Colour,1998,30,39 [3]Ansari.I.A;East.G.C;Johnson.D,JournalofTextileInstitute,1999,90,469 [4]Thakur.R;Sarkar.R;Sarmah.R,IndianJournaloffibreTextiles,1999,12,276 [5]Liu,X.X;He,W.Y.TextSciResearch,2004,1,1 [6]Jin.Y.A;Geng.Q.Y;Hu.X.M,WoolTextileJournal,2004,7,53 [7]Heritage.K.J;Mann.J;Gonzaleze.R,JournalofPolymersci,PartA;GenPap1963,1,671 [8]Schmidt.A;Bach.E;Schollmeyer.E,DyesandPigments,2003,56,27 [9]Chen.X.Y;Guo.Q.P;Mi.X.L,BamboofiberreinforcedpolypropylenecompositesAstudy ofmechanicalproperties.Journalofappliedpolymerscience,1998,69,189195 [10]PrasadB.M;Sain.M.M,Mechanicalpropertiesofthermallytreatedhempfibresininert atmosphereforpotentialcompositereinforcement,Mater.Res.Innov,2003,7,231238 [11]Mwaikambo.L.Y;Ansell.M.P,Chemicalmodificationofhempsisaljuteandkopakfibers byalkalization.Jofappliedpolymerscience,2002,84,22222234 [12]Wei.W.S;Zhou.X.Dyeingfinishing,1996,22,5 Imagecourtesy:http://www.ramielinenhemp.com

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