GPOM #641638, VOL 62, ISS 4

Flow Characteristics and Dynamic Behavior of Polyamide6/Acrylonitile Butadiene Styrene (PA6/ABS) Blends

AGUS ARSAD, ABDUL RAZAK RAHMAT, AZMAN HASSAN, MUNIRAH MOKHTAR SHAIFUL, and NIZAM MADDALI

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Flow Characteristics and Dynamic Behavior of Polyamide 6/Acrylonitile Butadiene Styrene (PA6/ABS) BlendsAgus Arsad, Abdul Razak Rahmat, Azman Hassan, Munirah Mokhtar Shaiful, and Nizam Mad Dali

Flow Characteristics and Dynamic Behavior of Polyamide6/Acrylonitile Butadiene Styrene (PA6/ABS) Blends

AGUS ARSAD1, ABDUL RAZAK RAHMAT1, AZMAN HASSAN1, MUNIRAH MOKHTAR SHAIFUL1, andNIZAM MAD DALI2

51

Q2 Enhanced Polymer Research Group (EnPRO), Department of Polymer Engineering, Faculty of Chemical Engineering, UniversitiTeknologi Malaysia, Skudai, Johor Bahru, Johor, Malaysia2Polyethylene Malaysia Sdn. Bhd., Kawasan Bukit Tengah, Kerteh, Kemamam, Terengganu, Malaysia

Received &Q5

10

The objective of this research was to investigate the effect of incorporation of maleic anhydride grafted acrylonitrile-butadiene-styr-ene (ABS-g-MAH) on rheological properties of PA6/ABS blends. Flow properties of the blends were examined by dynamic andcapillary rheometers. The dynamic rheological analyses showed an increase in complex viscosity with the incorporation of a com-patibilizer. The reduction of tan d peaks showed enhanced interfacial interaction between PA6 and ABS phase, which resulted in

15 the enhancement of melt strength. The power law index analysis showed that 1.5wt.% resulted in minimum n and maximum Kvalue for the blends while still retaining the pseudoplastics behavior necessary for plastics processing and prediction for the enduse performance of the PA6/ABS blends.

Keywords: PA6=ABS blends, power law index, rheological, viscosity

20 1. Introduction

Research on polyamide 6=acrylonitrile butadiene styrene(PA6=ABS) started about two decades ago [1].However,moststudies have focused on mechanical [2–3], morphological [4],and thermal [5] properties and a very limited study was found

25 in extensive rheological investigations, in particular on flowcharacteristics using capillary rheometer and dynamic beha-vior using rotational rheometry. The rheological approachwas proved to be an effective technique to study the interfaceproperties in polymer blends [6–7]. Many authors have dis-

30 cussed the approaches of improving the properties of PA6by reacting the polymers which contain appropriate chemicalfunctionalities with amine end groups of the PA6 during meltprocessing such as acrylonitrile butadiene styrene (ABS)[8–13], ethylene-propylene-diene (EPDM) [14], ethylene-

35 propylene rubber (EPR) [15], poly(phenylene oxide) [16–17],poly(phenylene ether) [18], polyolefin elastomer [19], ethylenecopolymer [20], and natural rubber (NR) [21].

PA6 is blended with ABS because of good processabilityand high impact strength of ABS compared to PA6 [11]. Sev-

40 eral types of compatibilizers have been used in the previousstudies for PA6=ABS blends [7–12]; however, very littleinformation has been reported on using ABS-grafted-maleic

anhydride as a compatibilizer. In this study, a desirable com-bination of ABS and PA6 will be realized by adding ABS-g-

45MAH as a compatibilizer to enhance the phase adhesion ofthe blends. Previously, many authors have investigated therheological properties of PA6 [13, 22–26] and ABS [27–29]blends, respectively, and a limited number of studies forPA6=ABS blends.. Therefore, this paper will investigate

50the rheological properties of PA6=ABS blends and the influ-ence of the compatibilizer concentration of ABS-g-MAH inorder to provide interface properties information and toestablish adequate processing parameters of PA6=ABSblends prepared by extrusion and injection molding.

552. Experiment

2.1 Materials

PA6 (Amilan CM1017) and super high impact ABS(100� 01) resin were supplied by Toray Plastics (Malaysia)Sdn. Bhd with melt flow index of 35 g=10min (at 230�C

60and 2.16 kg load) and 14 g=10min (at 220�C and 10 kg load),respectively. The compatibilizer was obtained from Polyram(Israel), with the brand name Bondyram1 6000, and isrecommended as a coupling agent for styrene compound.The melt index and density of ABS-g-MAH are 8 g=10min

65(at 220�C and 2.16 kg load) and 1.05 g=cm3, respectively.

2.2 Preparation of PA6/ABS Blends

Prior to blending, PA6, ABS, and ABS-g-MAH pellets weredried at 80�C for 24 hours. The PA6=ABS ratio was 50=50.

Address correspondence to: Agus Arsad,Q1 Enhanced PolymerResearch Group (EnPRO), Department of Polymer Engineer-ing, Faculty of Chemical Engineering, Universiti TeknologiMalaysia, 81310 UTM Skudai, Johor Bahru, Johor, Malaysia.E-mail: agus@cheme.utm.my

International Journal of Polymeric Materials, 62: 1–6

Copyright # 2013 Taylor & Francis Group, LLC

ISSN: 0091-4037 print/1563-535X online

DOI: 10.1080/00914037.2011.641638

3b2 Version Number : 7.51c/W (Jun 11 2001)File path : p:/Santype/Journals/TandF_Production/Gpom/v62n4/GPOM641638/GPOM641638.3dDate and Time : 25/10/12 and 14:08

The compatibilizer concentrations were 1, 3, and 5% wt of70 the matrix. The blends were prepared by melt mixing using

a Brabender counter-rotating twin-screw extruder.

2.3 Rotational Rheological Analysis

Small-amplitude oscillatory shear measurements were per-formed on a Rheostress TC501 in parallel-plate geometry

75 at Technical Service Laboratory, Polyethylene (M) Sdn.Bhd. The round samples with 25mm diameter and 1.5mmthickness were prepared using compression molding at245�C. The dynamic rheological testing was performedunder frequency sweeps ranging from 0.05 to 100 rad=s.

80 The frequency sweep measurements were carried out undernitrogen atmosphere at 230�C. The values of flow activationenergy were determined using the Willliam-Landel-Ferry(WLF) equation [30] and Arrhenius equation [31].

2.4 Capillary Rheological Analysis

85 Rheological analysis of the various blends was performedusing a Rosand Dual Capillary Rheometer at TechnicalService Laboratory, Polyethylene (M) Sdn. Bhd, Kertih,Terengganu. Rheological data were recorded for all theblends over a shear rate range of 10 to 3000 sec�1. The cal-

90 culated rheological data results are Bagley corrected. Theappearance shear rate and appearance shear viscosity wereconverted to actual shear rate and actual shear viscosityusing the method of Weissenberg-Rabinowitsch correction[32]. Then, the values of power law index, n and consistency

95 index, K were determined.

3. Results and Discussion

3.1 Rotational Rheological Properties Analyses

The complex viscosity dependence on frequency at differentcompatibilizer amount in PA6=ABS blends are shown in

100 Figure 1.Q4 From the figure, the highest of ABS-g-MAHcomposition in the mixture was found to be much more vis-cous than the lower and without ABS-g-MAH. Therefore,the data indicates that the viscosities of PA6=ABS blends

were affected by adding small amounts of ABS-g-MAH.105The incorporation ofABS-g-MAHtoPA6=ABSblends results

in significant changing of rheological properties of the blends.During blending of PA6 with ABS and ABS-g-MAH, the meltviscosity of PA6=ABS blends strongly increased as a result ofgraft formation between the PA6amine-end groups and the

110ABS-g-MAH anhydride groups.The PA6=ABS blends exhibited relatively strong

frequency-rheology. In general, the polymer blends showeda typical behavior, exhibiting a shear-thinning regime at allfrequencies studied. Figure 1 showed that at a fixed fre-

115quency, the complex viscosity increased with the amountof compatibilizer. This indicates that the compatibilizerreduced the interfacial tension and enhanced the interfacialadhesion between the domains phase and matrix phase. At1 and 3wt.% concentration of compatibilizer in PA6=ABS

120blends, the complex viscosities of blends containing the com-patibilizer were almost equal. Specifically, the incorporationof 5wt.% of ABS-g-MAH into 50=50 PA6=ABS blendsrevealed a sharp drop in viscosity beyond 30 s�1 of the shearrate. This could be that the rubber particles of ABS lose their

125entanglement and agglomeration to form uniform orien-tation and increased the flowability [33].

Figure 2 shows the relationship between rheological stor-age modulus G0 and frequencies x for the PA6=ABS blendscontaining different amounts of ABS-g-MAH. It can be seen

130that, within the frequency range tested, the storage modulusincreased with increasing frequency. The curves of G0 versusx almost followed a linear mixing rule, which is at fixed fre-quency; the storage modulus increased with increasing theamount of compatibilizer. It was found that the values of

135G0 of the compatibilized blend were slightly higher as com-pared to the uncompatibilized blends within the whole fre-quencies region, indicating the formation of a newstructure in these blends. Similar results of PA6 blended withmaleated triblock copolymer styrene-b-(ethylene-co-buty-

140lenes)-b-styrene (SEBS-g-MA) have been reported by Wangand Zheng [34]. It is believed that the interaction hasoccurred between amine end-groups of PA6 with the maliecanhydride groups in ABS-g-MAH and formed co-polymersat the interface of the blends. The interaction can stabilize

145the interface by reducing the coalescence and interfacial ten-sion, resulting in enhancement of the interfacial adhesionand viscosity. On the other hand, it should be emphasizedthat with the increasing amount of ABS-g-MAH, the storagemodulus of the blends at the low-frequency region seems to

150gradually deviate from the uncompatibilized PA6=ABSblends, which is responsible for the existence of co-polymerat the interface of the blends. This phenomenon could beattributed to increasing the relaxation time due to theenhancement of macromolecular chains in PA6=ABS=

155ABS-g-MAH blends.Figure 3 presents the response of loss modulus G00 against

frequencies at different amounts of compatibilizer for PA6=ABS. As far as G00 is concerned, it can be seen that highercontent of compatibilizer (5wt.%) in the blends produced a

160higher loss modulus, indicating higher energy dissipationcompared to the blends with lower compatibilizer content.

Fig. 1. Plot of complex viscosity versus frequency at differentamounts of compatibilizer for PA6=ABS blends. (Figure isprovided in color online.)

2 A. Arsad et al.

These loss modulus responses of PA6=ABS blends appearedto deviate systematically from the behavior without the com-patibilizer to higher compatibilizer content. In other words,

165 the loss modulus behavior followed the ‘‘rule of mixing,’’which shows a predictable increasing trend with increasingcompatibilizer content. Khan and co-workers [35] reportedthat the addition of the compatibilizer into PC=ABS blendschanged slightly the ratio of the plastic phase components

170 (polystyrene, acrylonitrile-styrene) to the rubbery phasecomponent (polybutadiene, butadiene-styrene, butadiene-acrylonitrile) altering the interaction between these phases.This indicates that the viscous component of the blendscould be changed, since the compatibilizer has a similar

175 ABS basic component. It has been reported that the viscoe-lastic behavior and loss modulus of ABS depend strongly onthe rubber phase or, more precisely, on the degree of graftingof the rubber particles in ABS phase [7,29,33,36]. As a result,the change of rubber phase ratio due to incorporation of

180 compatibilizer increased the loss modulus responses ofPA6=ABS blends.

Figure 4 shows the magnitude of tan d as a function offrequencies at different composition of ABS-g-MAH in

PA6=ABS blends. The incorporation of ABS-g-MAH attrib-185uted to the enhancement of interfacial interaction, resulting

in the enhancement of melt strength. Therefore, the incor-poration of the compatibilizer can lead to higher meltstrength, higher elasticity, lower viscosity, and lower tan d.From Figure 4, it can be seen that the blend without the

190compatibilizer showed the highest tan d. The introductionof ABS-g-MAH into PA6=ABS reduced the tan d value,increasing the melt strength and elasticity. It can be con-cluded that ABS-g-MAH has successfully compatibilizedand improved the rheological properties of the blend of

195PA6 and ABS.It is very difficult to find any crossover of G0 and G00 curves

at which G0 is equal to G00 and tan d is defined as equal to 1.Because of the intensive increment in tan d values of mostobtained PA6=ABS blends, the value of tan d should always

200be more than 1. The material exhibits solid-like behavior, ifG0 is more than G00, or liquid-like behavior, if G00 is more thanG0. The compatibilized PA6=ABS blends showed a liquid-likebehavior and can be categorized as viscoelastic material,which was easy to process at this processing temperature.

205This is because the blends had more PA6, thus had goodprocessability at this setting temperature as compared toABS.

Figure 5 shows a comparison of the curves of G0 versus G00

at different compositions of ABS-g-MAH in the PA6=ABSblends. Sarkhel and co-workers [37] have manipulated the

210Cole-Cole plot qualitatively to study the effect of blend misci-bility or compatibility LDPE=HDPE blends. From Figure 5,it can be observed that the incorporation of compatibilizerreduced the slope of the curve G0 versus G00. In other words,the addition of compatibilizer increased the elasticity due to

215grafting reaction of amine-end group and maleic anhydridefunction inABS-g-MAH. The deviation of theG0 curves moreprominent at low frequency. Krache [38] et al. reported thatthe elasticity of the compatibilized blends was increased dueto yield stress effects and the development co-continuous

220structure. This indicates that the ABS-g-MAH improved thecompatibility of PA6=ABS blends.

Figure 6 shows the effect of compatibilizer content onactivation energy of viscous flow at different PA6

Fig. 2. Plot of storage modulus, G0, versus frequency at differentamounts of compatibilizer for PA6=ABS blends. (Figure isprovided in color online.)

Fig. 3. Plot of loss modulus, G00, versus frequency at differentamounts of compatibilizer for PA6=ABS blends. (Figure isprovided in color online.)

Fig. 4. Plot of tan d versus frequency at different amounts ofcompatibilizer for PA6=ABS blends. (Figure is provided incolor online.)

PA6/ABS BlendsQ3 3

concentration. The incorporation of 1wt.% of compatibili-225 zer decreased the activation energy of flow. This was

expected because at this compatibilizer level the amountwas fairly enough to reduce interfacial tension and enhancedthe interfacial adhesion between PA6 and ABS phases. Gen-erally, the interfacial adhesion of immiscible and incompat-

230 ible blends is not strong enough because the interfacialtension of the blend components is high. Therefore, theintroduction of the compatibilizer reduces the interfacial ten-sion as well as the particle size of dispersed phase resulting inan improvement of interfacial adhesion. The addition of

235 ABS-g-MAH at 1wt% generally decreased the Ea of polymerblends, and resulting in polymer blends that are moretemperature-sensitive [39]. The activation energy increasedwith the addition of more than 3wt.% ABS-g-MAH. Beyond3wt% of compatibilizer, ABS-g-MAH is in excess within the

240 blends, which means that the more functional group ofmaleic anhydride is accessible and may result in overwhelm-ing interfacial interaction due to the repulsion of the polargroup in ABS phase to the PA6 phase. The lower flow acti-vation energy means that the material behaves in a more

245elastic or, in other words, increasingly solid-like behavior[40]. In general, the compatibilized interaction and acti-vation energy of flow could be interrelated because moreenergy is needed to break the interactions and allow thematerial to flow. Thus, the figure showed that 1wt% is

250enough of the compatibilizer, providing stronger interactionthan higher or no compatibilizer.

3.2 Capillary Rheological Properties Analyses

The capillary rheological properties of blends reveal shearstress, shear rate, and shear viscosity as well as power law

255index values on the compatibilization effect. Figure 7 showsthe plot of actual shear stress versus actual shear rate forPA6=ABS blends for different amount of ABS-g-MAH. Itcan be seen that the curves apparently deviate from the lin-ear relationship of shear stress with the shear rates inclining

260towards the axis of shear rate, suggesting that the blends arepseudoplastics fluids. It seems that the addition of the com-patibilizer did not change the shear stress of all the PA6=ABS blends at low shear rate. However, the shear stressesare changed slightly at higher shear rate.

265Figure 8 shows the effect of ABS-g-MAH as a compatibi-lizer of PA6=ABS blends at various shear rates. The flowcurves for the compatibilized blends were basically similarto that of the uncompatibilized blends. The results show thatthe shear viscosity of all the blends decreased with increasing

270shear rate, which is typical of pseudoplastics non-Newtonianor shear-thinning plastics. The decrease in shear viscositycould be attributed to the alignment of chain segments ofPA6=ABS blends in the direction of applied stress.

Figure 8 again shows that, at lower shear rate, the vis-275cosity seems at constant value, and it can be predicted all

the blends showed a Newtonian molten flow. Thus, theincorporation of compatibilizer significantly did not changemuch in the non-Newtonian behavior at lower shear rate.However, the dependence of shear viscosity on the shear rate

280at low shear rate regime is more pronounced as the amountof compatibilizer varied. In general, the compatibilizer had

Fig. 5. Plot of log G0 versus log G00 for PA6=ABS blends atdifferent amounts of compatibilizer. (Figure is provided in coloronline.)

Fig. 7. Plots of shear stress as a function of shear rate for PA6=ABS blend at different compositions of ABS-g-MAH. (Figure isprovided in color online.)

Fig. 6. Plot of activation energy of flow, Ea, versus amounts ofcompatibilizer for PA6=ABS blends. (Figure is provided incolor online.)

4 A. Arsad et al.

little effect on the shear viscosity for the whole range ofshear rate studied. The viscosity increased with increasingthe amount of compatibilizer at a fixed shear rate. The increase

285 in viscosity was probably due to increased interaction betweenthe PA6 and ABS as a result of decreased interfacial tensionand increased entanglement. Similar findings were reportedon the effect of the blend of polystyrene and polybutadieneusing two different types of compatibilizers [41].

290 The drastic effect on flowability of PA6=ABS blends wasnoticed upon increasing the concentration of compatibilizer,as shown in Figure 9. There was a reduction in power lawindex upon the addition of 1wt.% of compatibilizer andan increase when the compatibilizer was increased up to

295 3wt.%. This reduction of power law index at 1wt% of com-patibilizer could be due to the good interaction between ABSand PA6 phases. The increase of power law index when thecompatibilizer was about 3wt.% was believed to be due to anexcess amount of compatibilizer that formed agglomeration

300 within their phases and reduced the interfacial adhesion.

This also can be related to the value of consistency index,where it attributes to the viscosity. Furthermore, the powerlaw index has slightly decreased with increasing the compa-tibilizer concentration up to 5wt.%, though the consistency

305index increased with added compatibilizer. The increase incompatibilizer could recover more entanglement and thusmade the molecular orientation more difficult. This resultis similar to the study of PA6=LDPE blends compatibilizedby poly(ethylene-co-methacrylic acid) [42]. From the figure,

310it also can be predicted that 1.5wt.% compatibilizer pro-duced a minimum power law index and maximum consist-ency index, thus the amount has been suggested as theoptimum concentration of compatibilizer for PA6=ABSblends while retaining the pseudoplastics behavior of the

315blends.

4. Conclusions

In this research, detailed rheological analysis of PA6=ABSblends was carried out using the rotational and capillary rhe-ometer techniques. From the rotational rheometer, the

320effects of compatibilizer concentration, frequency, and tem-perature on rheological properties were studied. The PA6=ABS blends exhibited relatively strong frequency-rheologyor big frequency-dependence. The polymer blends showeda typical behavior, exhibiting a shear-thinning regime at all

325frequencies studied. At a fixed frequency, the complex vis-cosity increased with the amount of compatibilizer, indicat-ing that the compatibilizer reduced the interfacial tensionand enhanced the interfacial adhesion between the ABSphase and PA6 phase. Capillary rheometer data shows

3301.5wt.% of compatibilizer resulting in minimum power lawindex, n, and maximum consistency index, K, and thus issuggested as the optimum concentration of ABS-g-MAHfor PA6=ABS blends and indicates that improved interfacialadhesion was developed. Generally, understanding the rheo-

335logical properties will help the polymer technologist to pre-dict the processing and the end-use performance of thePA6=ABS blends.

Acknowledgment

Financial support from the Ministry of Higher Education340(MOHE) through Grant No. 78043 is highly appreciated.

The authors are particularly grateful for the support of themembers of Technical Service Laboratory at Polyethylene(M) Sdn. Bhd. Kerteh, Terengganu. Without their collabor-ation, this work would not have been realized.

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