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published online 9 March 2010Journal of Reinforced Plastics and CompositesAgus Arsad, Abdul Razak Rahmat, Azman Hassan and Shaipul Nizam Iskandar

Glass FiberMechanical and Rheological Properties of PA6/ABS Blends - With and Without Short

  

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Mechanical and Rheological Propertiesof PA6/ABS Blends � With and

Without Short Glass Fiber

AGUS ARSAD,* ABDUL RAZAK RAHMAT AND AZMAN HASSAN

Faculty of Chemical and Natural Resources EngineeringDepartment of Polymer Engineering, Universiti Teknologi Malaysia

81310 UTM Skudai, Johor Bahru, Johor, Malaysia

SHAIPUL NIZAM ISKANDAR

Polyethylene Malaysia Sdn. Bhd. Lot 3834, Kawasan Bukit Tengah, KM 105, JalanKuantan-Kuala Terengganu, 24300 Kerteh, Kemamam, Terengganu, Malaysia

ABSTRACT: Polyamide-6 (PA6), acrylonitrile-butadiene-styrene (ABS), and their blends are animportant class of engineering thermoplastics that are widely used for electronic and automotiveindustries. Many efforts have been made to improve the properties of both pure components and theblends. It was for this reason that the mechanical and rheological properties of PA6/ABS blendsystems compatibilized by acrylonitrile-butadiene-styrene�maleic anhydride was studied. Short glassfiber was also used to enhance the compatibilized blends. The systems were prepared using a twinscrew extruder. The specimens for mechanical test were molded using injection molding. The com-patibilized blends showed higher mechanical properties compared to uncompatibilized blend.However, the impact strength reduced with the introduction of short glass fiber in the blends.The processing properties of the materials have been investigated using dynamic rheometer.The rheological measurements confirmed the increased in interaction between the blend componentswith the incorporation of compatibilizer. The incorporation of short glass fiber (SGF) into thecompatibilized blends increased the storage and loss modulus as well as the viscosity of the blends.

KEY WORDS: thermoplastics composites, rheology, PA6/ABS-SGF composites.

INTRODUCTION

POLYAMIDE 6 (PA6) and acrylonitrile-butadiene-styrene (ABS) are widely used engi-neering thermoplastics. PA6 are a particularly attractive class of polymers due to the

good strength and stiffness, low friction, and excellent chemical and wear resistance. Thebeneficial properties have led to the wide range of usage especially in automotive, electricaland mechanical application. However, PA6 has some disadvantages associated with itsprocessing instability such as high mould shrinkage and dimensional stability, due toits inherent properties of rapid crystallization [1] and high moisture sensitive because of

*Author to whom correspondence should be addressed. E-mail: agus@fkkksa.utm.my

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its hygroscopic nature [2]. Therefore, the strong reasons behind blending ABS with PA6 isthat the low price of ABS compared to PA6, ease of processing, low water absorption andhigh impact strength. ABS has some strength over PA6 in low mould shrinkage, even ifother mechanical and thermal properties are not as good as PA6.

Blending of PA6 with ABS offers an interesting route to achieve new materials withpromising property combinations by optimizing their properties. Essentially, blends ofPA6 and ABS are immiscible throughout the whole range of compositions and exhibitlow impact toughness because the butadiene particles formed during the melt blendingprocess are relatively large [3]. Also, the immiscibility of PA6 and ABS in the melt stateleads to the blends with poor interfacial adhesion, unstable phase morphology and lowmechanical properties of the blends, which has limited their practical use. Therefore,reactive compatibilization is the most promising way to enhance the interfacial adhesionand improve the compatibility of the blends. During melt blending, the compatibilizer withanhydride functional group can react with amine end-group of PA6, resulting in thereduction of interfacial tension and improvement of phase dispersion and adhesionbetween PA6 and ABS phases. The ABS-grafted maleic anhydride is expected to act asreactive compatibilizer between PA6 and ABS. Aoki and Watanabe [4] reported that theaddition of certain amount of modified ABS � ABS grafted with maleic anhydride � to thePA6 has improved the dispersion phase. However, the addition of ABS leads to a reduc-tion in strength and stiffness. In contrast, reinforcing thermoplastics by short glass fiber(SGF) improved both strength and modulus; but a high content of SGF is necessary toachieve high strength and stiffness. Unfortunately, there is considerable loss in toughnessand ductility when these SGF are incorporated in the ductile polymer matrices.

Rheological effect on the incorporation of compatibilizer and SGF into PA6/ABSblends is a subject that has not been discussed in depth. Generally, polymer rheologicalproperties help to formulate a polymer system in respect to its processing characteristics.In addition, polymer rheological study will give an insight into physical properties of thesystem because there is interplay between the processing conditions, structure and proper-ties [5]. In this paper, the rheological properties of the blends have been investigated bymeans of dynamic rheometer.

MATERIALS AND METHODS

Samples Preparation

Both super high impact ABS resin and PA6 with the grade of Amilan CM1017 wassupplied by Toray Plastics (Malaysia) Sdn. Bhd. with a specified melt flow index of 14 and35 g/10min (at 220�C and 10 kg load). While, compatibilizer was obtained from Polyram,Ram-O Industries Limited, Israel with a brand name Bondyram� 6000. This compatibi-lizer is a maleic anhydride grafted ABS (ABS-g-MAH) with melt index and density being8 g/10min (at 220�C and 2.16 kg load) and 1.05 g/cm3, respectively. Glass fibers wereobtained from Taiwan Glass Industries Corporation, Taiwan, named as chopped strandTG183 with a filament diameter of 10 mm and an average length of 3.2mm.

PA6, ABS, ABS-g-MAH pellets, and SGF were dried at 80�C for 24 hours. The PA6/ABS ratios were 60/40. The compatibilizer concentrations were 1, 2, 3, and 5wt% of thematrix. The composites were reinforced with 10, 20, and 30wt% SGF respectively.The blends and composites were prepared by melt mixing using a Brabender twin-screw

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extruder at a speed of 90 rpm and the temperature profile adopted was 220/230/240/250�C.

The extruded strands were then air-dried and palletized. The specimens for mechanicalcharacterization experiments were molded by using injection molding.

Mechanical Properties Measurements

The tensile tests for blends and composites were conducted at room temperature at a

crosshead rate of 5mm/min with Instron Model 5567 computer-controlled testing

machine. Tensile strength, modulus, and elongation at break were simultaneously rec-orded. Izod impact strength was measured according to ASTM D256 using impact

tester. 2.54mm notch was generated on the sample surface in the thickness of 3.4mm.Measurements of mechanical properties were performed 10 times each and the average

value was obtained for its determination.

Dynamic Rheological Testing

Small-amplitude oscillatory shear measurements were performed on a RheostressRC501 in the parallel-plate geometry with diameter of 25mm and 1.5mm thickness.

The dynamic viscoelastic properties were determined with frequencies ranging from 0.05to 100 rad/s at 230�C, using strain and stress values determined the linear viscoelastic

region. All the frequency sweeps were repeated at least three times to confirm the

reproducibility.

RESULTS AND DISCUSSION

Tensile Properties of Polymer Blends

Figures 1 and 2 show the effect of ABS-g-MAH content on the tensile properties of

PA6/ABS blends. The tensile modulus of PA6/ABS blends increased with increasing ofABS-g-MAH ratio in the blends, especially at low filling rates. It shows that tensile

modulus increased drastically from 1740 to 2250MPa with the increment of 1wt% ofABS-g-MAH content. However, the tensile modulus decreased at 2% of ABS-g-MAH to

about 2040MPa. The addition of 3wt% to 5wt% of ABS-g-MAH content almost resulted

in constant modulus. This is because ABS-g-MAH became excess in amount and has notimproved much in compatibility of PA6/ABS blends. This trend could also be found

similar in tensile strength as shown in Figure 2.Figure 3 shows the elongation at break of PA6/ABS blends. The elongation can be used

to represent the behavior of toughness. It can be seen at lower amount of compatibilizer

(from 0 to 3wt%), it seems that the elongation increased gradually. However, the increasein percentage of ABS-g-MAH did not show any improvement and considered as maxi-

mum elongation about 9%. These results are in agreement with the result of impactstrength (Figure 7). Generally, the low elongation is attributed to the phase separation

and resulting less compatibility between PA6 and ABS phases even with the presence ofABS-g-MAH as compatibilizer.

Mechanical and Rheological Properties of PA6/ABS Blends 3

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Tensile Properties of Polymer Composites

Figures 4 and 5 show a tensile modulus and tensile strength of polymer composites,respectively. As expected, it can be seen from the figures that the tensile strength andmodulus were effectively enhanced by the addition of SGF. Similar result was alsofound by other researchers [6]. When the amount of SGF reached 30wt%, the tensilemodulus increased drastically, but not in the case of tensile strength, which was increasedgradually. However, as shown in Figure 6, the elongation at break of composites decreased

65

60

55

50

Tens

ile s

tren

gth

(MP

a)

0 1 2

Amount of ABS-g-MAH in the blends (wt%)

3 4 5

Figure 2. Tensile strength of PA6/ABS blends vs amount of ABS-g-MAH.

2.4

2.3

2.2

2.1

2.0

Tens

ile m

odul

us (

GP

a)

1.9

1.8

1.7

1.6

1.50 1 2

Amount of ABS-g-MAH in the blends (wt%)

3 4 5

Figure 1. Tensile modulus of PA6/ABS blends vs amount of ABS-g-MAH.

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tremendously by increasing SGF into the composites, and remained at constant valuewhen the amount of SGF is beyond 10wt%. Therefore, the incorporation of SGF didnot improve the toughness of the composites.

Impact Strength of the Polymer Blends

Notched Izod Impact values are plotted as a function of ABS-g-MAH content inPA6/ABS blends as shown in Figure 7. It can be observed that the impact strengthincreased as the percentage of ABS-g-MAH was increased. Upon the incorporation of2wt% of ABS-g-MAH in the PA6/ABS blends, the impact strength increased drastically

Elo

ngat

ion

at b

reak

(%

)

15

10

5

00 1 2

Amount of ABS-g-MAH in the blends (wt%)

3 4 5

Figure 3. Elongation at break of PA6/ABS blends vs amount ABS-g-MAH.

2.5

3.0

3.5

4.0

2.0

Tens

ile m

odul

us (

GP

a)

1.50 10 20

Amount of glass fiber in the composites (wt%)

30

Figure 4. Tensile modulus of PA6/ABS composites vs amount of short glass fiber.

Mechanical and Rheological Properties of PA6/ABS Blends 5

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and reached almost a constant value when the amount of ABS-g-MAH beyond 3wt%.The improvement in impact properties, in the present of ABS-g-MAH was believed to beattributed by the compatibilization of PA6 and ABS through the chemical reactionbetween the free terminal of amine end group of PA6 and the anhydride function inABS-g-MAH. Such reaction has been reported in many literatures [7,8].

Impact Strength of Polymer Composites

The impact result of the composites is shown in Figure 8 at different amount of SGF. Itcan be observed that when the amount of SGF was increased to about 10wt%, the impact

90

80

70

60

50

40

110

100

120

Tens

ile s

tren

gth

(MP

a)

0 5 10 15 20 25

Amount of glass fiber in the composites (wt%)

30

Figure 5. Tensile strength of PA6/ABS composites vs amount of short glass fiber.

0

10

5

15

Elo

ngat

ion

at b

reak

(%

)

0 10 20

Amount of glass fiber in the composites (wt%)

30

Figure 6. Elongation at break of PA6/ABS composites vs amount of short glass fiber.

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strength decreased drastically. The drastically reduction could be due to matrix embrittle-ment [9]. Beyond this point, the small increment in impact strength with further additionabout 20wt% SGF to be due to the fact that the fibers are shorter length and shorter fibersare effective energy absorbers by pull-out and debonding. The impact strength decreasedwith further increase of SGF to about 30wt% could be due to poor interfacial adhesion.

Rheological Properties of Polymer Blends

Figures 9 and 10 show the relationship between dynamic storage modulus G0, dynamicloss modulus G00 and frequencies ! for PA6/ABS blends at different amount ofABS-g-MAH at 230�C. It can be observed that G00 is greater than the G0 for all componentsat low frequencies. It also can be seen that within the ! range tested, curves ofG0 andG00 vs !

5.5

5.0

4.5

4.0

3.5

3.0

2.5

2.0

Impa

ct s

tren

gth

(kJ/

m2 )

0 1 2 3 4 5

Amount of ABS-g-MAH in PA6/ABS blends (wt%)

Figure 7. Impact strength of PA6/ABS blends vs amount of ABS-g-MAH.

4.5

4.0

3.5

3.0

2.5

2.0

Not

ched

impa

ct s

tren

gth

(kJ/

m2 )

0 10 20 30

Glass fiber content in composites (wt%)

Figure 8. Impact strength of PA6/ABS composites vs amount of short glass fiber.

Mechanical and Rheological Properties of PA6/ABS Blends 7

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for blends were located between the virgin PA6 and ABS, and almost followed a linear

mixing rule. It can be found that, the virgin PA6 obeyed the linear viscoelasticity model

[10,11], but not for the blends. In addition, compatibilized PA6/ABS blends, G0 and G00

increased significantly with increasing of ABS-g-MAH content. On the other hand, the

slopes of the blends at low frequencies appeared to slightly increase compared to the

virgin PA6. This is believed to be due to the fact that the dynamic rheological behavior of

blends mainly influenced by PA6 matrix as a continuous phase. It also indicates the new

structure formation in these blends. This result is in agreement with previous studies [12,13].

Sto

rage

mod

ulus

G′ (

Pa)

1.0E+05

1.0E+04

1.0E+03

1.0E+02

1.0E+01

1.0E+000.01 0.1 1

Frequency, w (rad/s)

10

PA6

′00

′01

′02

′03

′05ABS

100

Figure 9. Relationship between the dynamic storage modulus G0 and frequencies, ! for PA6/ABS blends atdifferent amount of ABS-g-MAH at 230�C.

Loss

mod

ulus

G′′

(Pa)

1.0E+05

1.0E+04

1.0E+03

1.0E+02

1.0E+010.01 0.1 1

Frequency, w (rad/s)

10

PA6

′00

′01

′02

′03

′05

ABS

100

Figure 10. Relationship between the dynamic loss modulus G00 and frequencies, ! for PA6/ABS blends atdifferent amount of ABS-g-MAH at 230�C.

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It is well known that the end group of PA6 is amine and capable of reacting with maleicanhydride groups in ABS-g-MAH and forms grafted co-polymer at interface of the blends.These interactions can stabilize the interface by reducing the interfacial tension, resultingin enhancement of the interfacial viscosity and adhesion. This is the reason why thosecompatibilized PA6/ABS blends exhibited higher G0 and G00 than uncompatibilized PA6/ABS blends. The rheological behavior of the blends at low ! region seems to graduallydeviated from that of virgin PA6 which is responsible for the existence of heterogeneousstructure. This is attributed to the result of increase in complex viscosity due to enhance-ment of macromolecular. The enhancement of macromolecular was caused by the inter-action between amine end-groups of PA6 and maleic anhydride groups in ABS-g-MAHand formed co-polymer at the interface of the blends.

Figure 11 shows the relationship between the complex viscosity g* and frequency, ! forPA6/ABS blends at different amount of ABS-g-MAH at 230�C. It is evident that thecomplex viscosity increased with increasing the frequencies, indicating that the melt ofthese polymers belong to pseodoplatics fluids and have the flow properties of shear thin-ning. However, the virgin of PA6 had a slightly constant complex viscosity and showed aNewtonian flow behaviour [11] at low frequencies. Followed by a shear-thinning regime atmoderate frequencies. The shear thinning of virgin PA6 was less than virgin ABS andother blends. It can be explained that the molecular chains of PA6 are rigid and hence hardto tangle each other, whereas virgin ABS with flexible chains possesses much more entan-glements than PA6 [14,15].

With the incorporation of ABS-g-MAH, it can be found that the complex viscosityincreased with increasing of ABS-g-MAH content at low frequencies range due to improve-ments of phase structure and interfacial adhesion between PA6 and ABS. It is believed to bedue to the graf-formation by reacting amine end-group of PA6 with maleic anhydride inABS-g-MAH. These results are in agreement with a previous study [16]. These results arealso confirmed by the result of tan � as shown in Figure 12, which is, the more amount ofABS-g-MAH introduced into the blends, the lower of tan � peak to be and thus less energy

1.0E+05

1.0E+04

1.0E+03

1.0E+020.01 0.1 1

Frequency, w (rad/s)

10

PA6′00′01′02′03′05ABS

100

Com

plex

vis

cosi

ty h

∗ (P

as)

Figure 11. Relationship between the complex viscosity g� and frequencies, ! for PA6/ABS blends at differentamount of ABS-g-MAH at 230�C.

Mechanical and Rheological Properties of PA6/ABS Blends 9

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dissipated by the polymer systems. Therefore, by the addition of SGF, the reduction of tan �peak can also be associated with the decreased mobility of the polymer chains.

Rheological Properties of Polymer Composites

The G0 and G00 results for the polymer composites and polymer blends are shown inFigures 13 and 14, respectively. Again, rise in storage modulus with increasing SGF con-centration was observed at all frequencies. These polymer composites can be categorizedas liquid-like material, because the G00 is greater than G0 at all range of frequencies studyregardless of the amount of SGF in the systems. This phenomenon is because SGF actedas a lubricant and caused the polymer phase of PA6 and ABS to easily slip at interphaseand interface level.

Tan

d

6.0

5.0

4.0

3.0

2.0

1.0

0.00.01 0.1 1

Frequency, w (rad/s)

10

′00

′01

′02

′03

′05

100

Figure 12. Relationship between the tan � and frequencies, ! for PA6/ABS blends at different amount ofABS-g-MAH at 230�C.

Sto

rage

mod

ulus

G′ (

Pa)

1.0E+06

1.0E+02

1.0E+03

1.0E+04

1.0E+05

0.01 0.1 1

Frequency, w (rad/s)

10

0

10

20

30

100

Figure 13. Relationship between the dynamic storage modulus G00 and frequencies, ! for PA6/ABS compo-sites at different amount of short glass fiber at 230�C.

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Figure 15 represents the relationship between complex viscosity and frequencies, ! for

PA6/ABS composites containing different amounts ranging from 0 to 30wt% of SGF at

230�C. It can be seen that the trend in complex viscosity growth associated with SGF

loading. At all frequencies, the complex viscosity of the polymer composites was larger

than unfilled PA6/ABS blends. It can also be found, that the complex viscosity decreased

with the increasing of frequencies. This observation is due to the deformation of the SGF

at high frequencies and its associated contribution to an increase in fluidity of the matrix

phase. When more SGF added into the blends, the SGF droplets began to grow and

coalesce, causing an increase in the complex viscosity [17]. Generally, all the blend systems

showed a non-Newtonian behavior at all frequencies.The information on how efficient the polymer composites lose energy to molecular rear-

rangements and internal friction, can be obtained by understanding the relation between tan

� of PA6/ABS composites vs frequency and is shown in Figure 16. The tan � is very sensitive

Loss

mod

ulus

G′′

(Pa)

1.0E+06

1.0E+02

1.0E+03

1.0E+04

1.0E+05

0.01 0.1 1

Frequency, w (rad/s)

10

0

10

20

30

100

Figure 14. Relationship between the dynamic loss modulus G0 and frequency, ! for PA6/ABS composites atdifferent amount of short glass fiber at 230�C.

Com

plex

vis

cosi

ty h

∗ (P

as)

1.0E+05

1.0E+03

1.0E+01

0.01 0.1 1

Frequency, w (rad/s)

10

0

10

20

30

100

Figure 15. Relationship between the complex viscosity and frequencies, ! for PA6/ABS composites atdifferent amount of short glass fiber at 230�C.

Mechanical and Rheological Properties of PA6/ABS Blends 11

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with structural change [18] and decreased with the incorporation of SGF, which is mainlydue to the existence of effective interfacial bonding between SGF and PA6/ABS matrix sothat the energy dissipation in the composite was limited. Otherwise, if the interfacial adhe-sion is poor, applied energy will be dissipated in the form of heat due to the interactionbetween the fiber and matrix. Consequently, the peak of tan � will increase with decreasingthe interfacial adhesion. In the composite systems, the decreasing of tan � is due to incor-poration of SGF, resulting in an improvement in damping and showing that the polymercomposites are more elastic [19]. It can be observed from the figure that the tan � decreaseddrastically when 10wt% of SGF was introduced into the composite. It can also be observedthat 20 and 30wt% of SGF have a considerably similar effect on tan � at all frequenciesstudied, this resulted in the incorporation of SGF and improved the damping and elasticityof PA6/ABS composites.

Tan � is also very sensitive with structural change of the composites and viscoelasticbehavior. This can be determined using the analysis of tan � peak. The figure shows that aviscoelastic peak occurred at the frequency around 2�5 rad/s and depends on concentra-tion of SGF in the PA6/ABS composites. It can be observed, that the unreinforced com-posite has a highest tan �, indicates less elastics than the reinforced composites. The elasticbehavior became more prominent with the highest amount of SGF. In other words, theviscoelatics disappeared when increasing the SGF content. Tan � peak also indicates asolid�liquid transition, in which the composite undergoes a transition with increasingfrequency. At the transition point, tan � is expected to be independent of frequency.When the frequency increased beyond this transition point, a dominating elastics response(solid behavior) of the composite became more obvious. At frequency about 100 rad/s, allthe composites showed considerably identical tan � value indicating the SGF has notaffected the viscoelastic behavior of the composites.

CONCLUSIONS

The mechanical properties of PA6/ABS blends and SGF reinforced PA6/ABS compo-sites have been studied considering the effect of ABS-g-MAH and SGF content, respec-tively. The amount of ABS-g-MAH in the PA6/ABS blends was found to have significant

Tan

d

5.0

4.0

3.0

2.0

1.0

0.00.01 0.1 1

Frequency, w (rad/s)

10

0

10

20

30

100

Figure 16. Relationship between the tan � and frequencies, ! for PA6/ABS composites at different amount ofshort glass fiber at 230�C.

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effects on the mechanical and rheological properties as well as the ratio of SGF in thepolymer composites. It was exhibited that the tensile and flexural properties improvedupon the addition of ABS-g-MAH at its various compositions into the PA6/ABS blends,while the toughness properties decreased with introduction of SGF in the composites. Theprocessing properties of the materials have been investigated by using dynamic rhe-ometers. The rheological measurements confirmed the increase in interaction betweenthe blends components, especially with ABS-g-MAH as a compatibilizer. The incorpora-tion of SGF into the compatibilized blends increased the storage and loss modulus as wellas the viscosity of the blends.

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