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International Journal of Engineering Research and Applications (IJERA) is an open access online peer reviewed international journal that publishes research and review articles in the fields of Computer Science, Neural Networks, Electrical Engineering, Software Engineering, Information Technology, Mechanical Engineering, Chemical Engineering, Plastic Engineering, Food Technology, Textile Engineering, Nano Technology & science, Power Electronics, Electronics & Communication Engineering, Computational mathematics, Image processing, Civil Engineering, Structural Engineering, Environmental Engineering, VLSI Testing & Low Power VLSI Design etc.

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  1. 1. Sa’ude, N., Masood, S. H., Nikzad, M., Ibrahim, M., Ibrahim, M. H. I./ International Journal ofEngineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 3, May-Jun 2013, pp.1257-12631257 | P a g eDynamic Mechanical Properties of Copper-ABS Composites forFDM FeedstockSa’ude, N.,*, Masood, S. H.,**, Nikzad, M., **, Ibrahim, M.,*, Ibrahim, M.H. I.**Department of Manufacturing and Industrial Engineering, UTHM University, Johor 86400, Malaysia** Faculty of Engineering and Industrial Sciences, Swinburne University of Technology, Melbourne VIC3122,AustraliaABSTRACTThis paper presents an investigation ofdynamic mechanical properties of a copper-ABScomposite material for possible fused depositionmodeling (FDM) feedstock. The material consistsof copper powder filled in an acrylonitrilebutadiene styrene (ABS). The detailedformulations of compounding ratio by volumepercentage (vol. %) with various combinations ofthe new polymer matrix composite (PMC) areinvestigated experimentally. Based on the resultobtained, it was found that, increment by vol. %of copper filler ABS affected the storage modules(E’) and tan δ results. The storage modulus andtangent delta increased proportionally withincrement of copper filled ABS. It can beobserved that, the storage modulus and tangentdelta are dependent on the copper filled ABS inthe PMC material.Keywords - Polymer Matrix Composites, DynamicMechanical Properties, Storage Modulus, LossModulus, Tan δ, Fused Deposition Modelling.I. INTRODUCTIONRapid prototyping (RP) technology is anew technique for part fabrication in layers by alayer process. Normally, previous RP applicationsfocused on build a final product for fitting andtesting. Customer needs for the end used productand continued demand for low-cost and time savinghave generated a renewed interest in RP. A shiftfrom prototyping to manufacturing of the finalproduct will give an alternative selection withdifferent material choice, low cost part fabricationand achieving the necessary mechanical properties.One of the RP technologies available today is FusedDeposition Modelling (FDM), which involvesextrusion of plastic filament wire as feedstockmaterial. Existing FDM machine have been able todeposit only thermoplastic filament with limitedmechanical properties through the liquefied nozzle.Fig. 1 shows the schematic diagram of the FDMfilament through heated liquefied nozzle [10]. TheFDM machine can process acrylonitrile butadienestyrene (ABS) plastic material[4,9,10,11,19,21,22,23,24] and Nylon [16,17]material. Other material and polymermatrix composites (PMC) used in FDM are ABS-Iron [9,10,16,17,26], Aluminum epoxy [15] andstainless steel-ECG2[25]. Meanwhile, someresearchers focused on the optimal processparameters by Taguchi method [4,13,21,22,24],improved FDM product [22,23,25], mixing torque[9], thermal conductivity [11, 16], deposition rate[19,23] geometrical modeling and mathematicalmodel [20], [23,24] and mechanical properties[16,21,22,23,26]. Another manufacturing processfor PMC is injection moulding. In various researchwork, the composites material used in injectionmoulding are basalt-LDPE [1], iron-HDPE [2,14],iron, nickel-HDPE [3], zirconia-PE [5], copper-PE[6], stainless steel-PE [7,14], stainless steel-PEG,PMMA [8,2], iron-PP, EVA [14] and stainless steel-EVA [18]. Wu et al. [25] have investigated thedevelopment of stainless steel-ECG2 ceramiccomposite for time and cost saving using FusedDeposition Ceramic (FDC). It was mentioned that,the compounding is a very critical process toprovide homogenous powder polymer mixture ofstainless steel filament. The fabrication of ABS-Ironfilament wire for FDM machine has been done byMasood et al. [16,17] and Nikzad et al. [9,10] withproper formulation and mixing processes. Theymentioned that the critical properties requirementsfor high-quality composite are depending on thedesired viscosity, strength and modulus. High ironpowder loading in the Nylon will lead to dispersionissues, and the viscosity will increase withincrement of metal powder in PMC material. Nikzadet al. [10,27] have investigated the thermomechanical properties of new composite for rapidtooling in injection moulding application. It wasmentioned that, the addition of 10% iron into ABSmatrix increase the storage modulus up to 40%approximately. The tensile strength result dropsproportionally with increment of 10% by volume ofiron powder. From the DMA results obtained, itwas found that with high concentration of copper(30% by vol. %) above glass transition temperatureof ABS, the thermal conductivity increasedproportionally. The conductively begins to form atonly in 20 vol. % concentration of copperparticles[10]. Nowadays, application of FDMmaterial requires an enhanced and higher
  2. 2. Sa’ude, N., Masood, S. H., Nikzad, M., Ibrahim, M., Ibrahim, M. H. I./ International Journal ofEngineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 3, May-Jun 2013, pp.1257-12631258 | P a g emechanical property toward rapid manufacturing.Pure metal is unsuitable for deposit through theheated liquefied head by FDM machine because ofhigher melting temperature and viscosity.Nevertheless, there are limited data/researchavailable particularly dealing with the deposition ofPMC through the heated liquefied nozzle. Layeredof rapid deposition polymer composites (RDPC)with highly filled metal powder in the polymermatrix may offer the possibility of introducing newcomposite material in FDM.Figure 1 Schematic diagram of the FDM Filamentthrough heated liquefied nozzle [10]The aim of this study is to developcomposite feedstock with copper, ABS andsurfactant powder for FDM process. The researchfocuses on developing a proper formulation andmixture procedure of constituent materials forobtaining the homogeneous condition to produce thefeedstock form. The main outcome from this studyis to produce a strong, flexible, smooth andconductive feed stock to be produced by extrusionmachine. The optimum composition of mixing ratioof constituent material was made by an injectionmoulding process for dynamic mechanical analysis.In this study, two main types of constituentmaterials were used to develop the new compositematerial. The first material, used for the matrix, isthe ABS thermoplastic powder with lower meltingtemperature approximately 266°C, flexible andstiffness and suitable material for extrusion process.The copper particle was mixed with the ABSmaterial as binder content to form the composite inBrabender mixer. The additive material is needed inorder to control the melt flow behavior during anextrusion process. Results will be presented fordynamic mechanical properties, including storagemodulus (E’), loss modulus (E”) and Tan δ.II. EXPERIMENTAL2.1 Fabrication of FDM FeedstockThe fabrication of a new composite ofFDM feedstock, required three types of theconstituent material, which is a copper powder, ABSplastic and surfactant material. The ABS material issupplied by Dutatek Sdn. Bhd. (Selangor,Malaysia). The density of ABS was 1.03 g/cm3andmelting temperature 266 ºC. ABS materials are anenvironmental friendly material because they arecompletely recyclable. Fig. 2 shows the ABSmaterial for injection process. The copper powder issupplied by Saintifik Bersatu Sdn. Bhd. (Johor,Malaysia). The chemical composition is 99.9 %copper powder, and the particles size distribution is17µm ~ 130 µm respectively with meltingtemperature 1080 °C and specific gravity 9.84g/cm3. Fig. 3 shows the copper material used incompounding process and Fig. 4 shows the SEMimages of pure copper powder (300x) with differentgrain size distribution in a millimetre.Figure 2 ABS Material Figure 3 CopperPowderThe amount of each compoundingcomposites is depending upon the volumepercentage weight. In this experiment, the actualamount of compounding was determined andcalculate by equation (1) following relationship[10]:Wc = Wcop +WABS (1)(1-Ws%)Where;Wc Weight of composite material in gramsWcop Weight of copper powder in gramsWABS Weight of ABS powder in gramsWs% Weight percentage (wt. %) of surfactantmaterialFigure 4 SEM Image of pure copper powder (300x)The distributions of the copper powder, ABS andsurfactant composition are 57% to 63% ABS, 22%
  3. 3. Sa’ude, N., Masood, S. H., Nikzad, M., Ibrahim, M., Ibrahim, M. H. I./ International Journal ofEngineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 3, May-Jun 2013, pp.1257-12631259 | P a g eto 24 % copper powder and 15 % to 19% surfactantby volume percentage. A binder material based ABSplastic and surfactant (S) powder was added as thesurfactant agent for smoothest flow of mixture ofmaterials.Firstly, ABS material was cut into the smallest sizeand approximately 2 mm - 5 mm in length. Afterthat the ABS materials were then loaded inBrabender mixer, type W50 at 180 oC forcompounding process in constant speed. In order toachieve a homogeneous mixture, the compoundingprocedure was followed. The maximum volume ofthe mixer is 55 cm3per mix approximately and oneto three hour mixing time. Fig. 5 shows the (a)Brabender mixer, (b) Compounding process of ABSand copper materials. The PMC compounding wereanalyzed by scanning electron microscope(SEM)images to ensure a homogeneous compounding isacceptable for feedstock preparation. At the end, thesurfactant was added into compounding to reducethe inter particle forces and to lubricate the powder.(a) (b)Figure 5 (a) Brabender Mixer (b) Compoundingprocess of Copper, ABS and surfactant MaterialThe compound was crushed by machine toform the pellets with 2 mm – 6 mm in sizeapproximately. Fig. 6 shows the (a) PMC materialafter the Brabender mixer and (b) PMC materialafter crushing process. The feedstock pellet wasinjection moulded on a horizontal NP7-1F mouldingmachine for dynamic mechanical analysis (DMA)properties test specimens. Table I shows thecomposition of constituents of copper filled ABScomposite material for five samples of PMCcompounded with the different density value. Thevolume percentage ratio of copper, ABS andsurfactant material are shown in Fig. 7(a) (b)Figure 6 (a) The PMC material after the brabendermixer (b) The PMC material after crushing process.Due to the copper powder loading in the ABSmatrix, the density of the composite increasesproportionally with an increment of copper powder.An important issue in the extrusion process is theviscosity of the composite material to flow throughthe injection mould. In this study, two methods wereused to determine the value of composite density.Firstly, the density of composite was measured byexperiment and secondly by equation. In theexperiment, the measurement of density was carriedout by the Mettler Toledo apparatus. The theoreticaldensity of the composite was calculated by equation(2) by Kate, 1987 [29].dc = Vfdf + Vpdp(2)where,dc Theoretical density of the compositeVf Volume percentage of filler copperVp Volume percentage of ABS polymerdf Density of filler copperdp Density of ABS polymerFigure 7 Distribution of volume percentage ofcopper, abs and surfactant materialsTable I. Constituents of copper filled abs compositesmaterialMaterialBy VolumePercentage(vol. %)Densitybyequation(g/cm3)Density byexperimental(g/cm3)ABS CopperA 100 0 - 1.03B 78 22 2.77 2.23C 77 23 2.82 2.34D 76 24 2.87 2.40E 75 25 2.93 2.43F 74 26 2.98 2.52
  4. 4. Sa’ude, N., Masood, S. H., Nikzad, M., Ibrahim, M., Ibrahim, M. H. I./ International Journal ofEngineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 3, May-Jun 2013, pp.1257-12631260 | P a g eHopperScrewMotionBarrelFeedRear 2FrontMiddleRear 1NozzleFigure 8 Injection molding machine [26]2.2 The Specimen Fabrication by InjectionMouldingThe injection moulding process was usedto fabricate the specimens. The machinespecifications are the screw diameter 19 mm,injection capacity 14 cm³, injection rate 50cm³/second and injection pressure 161 MPa.Standard test specimens of DMA were preparedbased on ISO 178 or ASTM D790. Due to thenumerous type of dynamic mechanical instrument,specimen size is not fixed by this practice. Thespecimen size used was 80 mm x 10 mm x 3.2 mmin the analysis. Zone temperatures consist of fiveareas, where the nozzle temperature was 170 oC,front and middle were set to 175 oC and 165 oC,while for rear 2 and rear 1 was 130 oC and 160 oC.The feeding temperatures were set to 70 oC with thecooling time is10 second. In order to prevent themelt from sticking at the screw, the barreltemperature was used from low to high temperature.Fig. 8 and Fig. 9 shows, the injection mouldingmachine and the zone temperature in injectionmoulding machine.Figure 9 Zone temperature in injection moldingmachine[26].Figure 10 Comparison of dynamic mechanicalproperties of virgin ABS and 10% iron-powderfilled ABS [10]2.3 Dynamic Mechanical Analysis (DMA)DMA is a technique used to measure themechanical properties of an elastic, inelastic andviscous material. Normally, DMA works in thelinear viscoelastic range, and it is more sensitive tostructure. In dynamic mechanical test, the materialstiffness and the loss modulus were measured. Thecomplex modulus(E*) will be calculated based on amodulus equals stress/strain. From the resultobtained on the graph for E* and measurement ofTan Delta (tan δ), the storage modulus (E’) and lossmodulus (E”) will be calculated[28]. The storagemodulus (E’) was used as the elastic component,and it is related in the stiffness sample of polymercomposite material. Furthermore, the loss modulus(E”) was used as viscous component and is relatedin the ability of the sample to dissipate mechanicalenergy through molecular motion. Finally, tangentof phase difference (tan δ) will provide theinformation about the relationship between theelastic and inelastic for polymer matrix compositematerial. According to Nikzad et al. [10], it wasfound that the glass transition temperature increasedproportionally with an increment of 10% iron inABS. The peak glass transition temperature(Tg) ofunfilled ABS is 126 oC and glass transitiontemperature(Tg) of 10% filled ABS is 118.9 oC.Furthermore, the Tan δ will be calculated based onthe loss modules divide by storage modulus value.Fig. 10 shows the comparison of dynamicmechanical properties of virgin ABS and 10% iron-powder filled ABS[10].III. RESULTS AND DISCUSSIONIn this study, the experiment was done onDMA 2980, manufactured by TA instrument, whichis a common equipment used for analysis. In thisstudy, two main dynamic mechanical propertiesobserved are the storage modulus (E’) and the lossfactor (tanδ) for the copper-ABS feedstock. Storagemodulus value is a measure of the maximum energy
  5. 5. Sa’ude, N., Masood, S. H., Nikzad, M., Ibrahim, M., Ibrahim, M. H. I./ International Journal ofEngineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 3, May-Jun 2013, pp.1257-12631261 | P a g estored in the composites material during one cycleof oscillation [30]. Three (3) sample with differentcompounding of PMC has been done by extrusionprocess for sample preparation used in DMAanalysis. Each PMC compounding consists of fivepieces for each sample for analysis. The DMAsetting was dual cantilever with amplitude 15 µmand temperature ramp of 10 oC/min up to 160 oC.The specimen size from injection moulding were cutinto 57 mm x 10 mm x 3.2 mm and clamped in thedual cantilever mode in DMA machine.Table II Storage modulus, loss modulus and tandelta of composites with 22 % copper filled in ABSpolymer.Temperature(oC)Max StorageModulus(MPa)LossModulus(MPa)Tan δ40 52731 10018 0.19050 35176 9118 0.25960 16941 4341 0.25670 11827 2780 0.23580 9787 2404 0.24690 7333 2022 0.276100 2360 809 0.343110 551 459 0.833120 145 88 0.608130 90 27 0.306140 68 16 0.235Fig. 11 shows the results of temperaturescan for the three dynamic properties for the 22%copper filled in ABS material. The testing was donefor a temperature range of 30 oC to 160 oC at fixedfrequency of 1 Hz. In Fig. 11, the complex viscosityis in Y-1 axis, the storage modulus in Y-2, the lossmodulus in Y-3 and tan delta in Y-4 axis withtemperature variation in X axis. The results showsthat for the 22 % copper filled in ABS polymer, thecomplex viscosity, the storage and loss modulusdecrease with increase in temperature. Themaximum glass transition temperature of 22 %copper filled in ABS was 113 oC and the tan delta is0.8813 approximately. Increment of 22 % copperfilled in ABS increased the storage modulus up to551MPa and the loss modulus up to 459 MPa.Table II shows the detailed values for the storagemodulus, loss modulus and tan delta of compositeswith 22 % copper filled in ABS polymer.Figure 11 Dynamic Mechanical Properties of 22%copper powder filled ABS.Table III Effect of copper filled in ABS on the TgMaterialHeatingrate(°C/min)HeatflowOnset(W/g)TgOnset(°C)TgMidpoint(°C)Abs Pure 10 -0.1235 104.5 106.2Co71%,29%Abs10 -0.0661 98.9 102.0Co72%,28%Abs10 -0.0881 100.5 102.7Co73%,27%Abs10 -0.0881 100.8 102.7Co74%,26%Abs10 -0.0523 101.7 103.6Co75%,25%Abs10 -0.0688 100.5 102.73.2 Differential Scanning Calorimetry(DSC)The measurements of glass transitiontemperature (Tg) and heat flow were carried out byTA Instrument Q50 for differential scanningcalorimeter (DSC). In this analysis, the sampleswere encapsulated on aluminum pans with 10.5 mgsample weight, prepared by extrusion method. Theselected heating rate was 10 °C/min for each ABSand compounding material to achieve goodresolution. The DSC test was carried out mainly toinvestigate the effect of copper filled in ABSmaterial from injection molding with differentcompositions on the Tg temperature value. Theresults for ABS pure and injected compoundingsample with different compositions are shown inTable III. Fig. 12 shows the DSC results for pureABS material, where the glass transitiontemperature is found to be 104.5 oC on onset. Fromthe results obtained, the increment of copper filledin ABS matrix does not much affect on the glasstransition temperature(Tg). The maximum Tg onsetof compounding 74% copper filled in 26 % ABS is101.7 oC approximately. The minimum value of Tg
  6. 6. Sa’ude, N., Masood, S. H., Nikzad, M., Ibrahim, M., Ibrahim, M. H. I./ International Journal ofEngineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 3, May-Jun 2013, pp.1257-12631262 | P a g eonset is 98.9 oC with heat flow -0.0661 W/g for 71%copper filled in 29 % ABS. It is observed that, theTg value decreases in the copper filled in ABSmatrix. The detail of the heat flow of pure ABS and74% copper powder filled in 26% ABS for FDMfeedstock are shown in Fig. 13 and Fig. 14.Figure 12 Glass transition temperature(Tg) of pureABSFigure 13 Glass transition temperature(Tg) of 74%copper filled in 26% ABSFigure 14 Heat Flow of copper powder filled inABS with different composition.IV. CONCLUSIONSA new PMC feedstock with copper powderfilled in ABS was successfully produced fordynamic mechanical analysis. The DMA testing hasbeen successfully used to produce results for thestorage modulus (E’), loss modulus (E”) and TanDelta (δ). The results show that, the dynamicmechanical properties of copper filled in ABS aregreatly affected by the volume percentage of thecopper content. The suitable material and binderselection, mixing method and parameter setting onmelting temperature, pressure and cooling time mayoffer a great potential area for the metal feedstockfabrication in the wire filament extrusion throughthe extruder machine.AcknowledgementsThis research was conducted by the visitingfirst author at Industrial Research InstituteSwinburne (IRIS), Faculty of Engineering andIndustrial Sciences, Swinburne University ofTechnology, Victoria, Melbourne, Australia.References1. Akinci, Mechanical and MorphologicalProperties of basalt filled Polymer MatrixComposites, Science Journal, 35, 2009, 29-32.2. Gungor, Mechanical Properties of Ironpowder filled high density PolyethyleneComposites, Journal of Materials andDesign, 28, 2007, 1027-1030.3. Huang, S. Liang, and X. Qu, The Rheologyof metal Injection Molding, Journal. ofMaterial Processing Technology, 137,2003, 132-137.4. H. Lee, J. Abdullah, and Z. A. Khan,Optimization of Rapid PrototypingParameters for Production of Flexible ABSObject, Journal of Materials ProcessingTechnology, 169, 2005, 54-61.5. L. Merz, S. Rath, V. Piotter et. al.,Feedstock Development for micro powderInjection Molding, MicrosystemTechnolology, 8, 2002, 129-132.6. L. Moballegh, J. Morshedian and M.Esfandeh, Copper Injection Molding usinga Thermoplastic binder based on paraffinwax, Journal of Materials Latters, 59,2005, 2832-2837.7. M. A. Omar, I. Subuki, N. Abdullah andM. F. Ismail, The influence of palm stearincontent on the Rheological Behavior of316L stainless steel MIM compact, volume(2), No. 2, Journal of Science andTechnology, 2010, 1-14.8. S. Y. M. Amin, K. R. Jamaludin and N.Muhamad, Rheological Properties ofSS316L MIM Feedstock prepared with
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