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Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and
                   Applications (IJERA) ISSN: 2248-9622 www.ijera.com
                    Vol. 2, Issue 5, September- October 2012, pp.1922-1926
       Effect Of Moulding Temperature On The Properties Of
      Polypropylene/High Density Polyethylene/Clay/Glass Fibre
                           Composites
                        Ranjusha J P1, Anjana R1 and K E George2
                          1. Dept. of Chemical Engg., Govt. Engg. College, Thrissur
                        2. Dept. of Polymer Science and Rubber Technology, CUSAT

Abstract                                                Polymer nanocomposite(PNC) is a polymer or
         Polymer nanocomposites have emerged            copolymer having dispersed in its nanoparticles.
as a high-tech engineering material for a variety       These may be of different shape (e.g., platelets,
of applications. The present paper emphasis on          fibres, spheroids), but at least one dimension must
the comparison of polymer nanocomposites
synthesized      under      different    moulding       be in the range of 1 to 80 nm. These PNC's belong
temperature and the effects of moulding                 to the category of multi-phase systems (blends,
temperature on the preparation of polymer               composites, and foams) that consume nearly 95% of
nanocomposites by different characterization            plastics     production. These systems require
techniques. Also aims to investigate the enhanced       controlled mixing/compounding, stabilization of the
physical and mechanical properties of polymer           achieved dispersion, orientation of the dispersed
nanocomposites with different nanofillers.              phase, and the compounding strategies for all
Polymer hybrid nanocomposites based on poly             multiphase systems, including PNC, are similar [6-
propylene(PP) (80% of blend)and high density            8].
poly ethylene(HDPE)(20% of blend) blend is
selected for the present study. Nanofillers such as                Synthesis of polymer nanocomposites
nano kaolin clay (2%) and/or                  glass     include mixing /addition of nanofillers into the
fibre(GF)(20%) is incorporated in the polymer           polymer and moulding the graft obtained into
matrix.                                                 desired shapes [9]. Polymer–clay nanocomposites
         The properties of processed goods,             can be synthesized via four mixing approaches
particularly based on polymer blends, are highly        depending on the starting materials and the
depend on the processing variables and the effect       processing     techniques;     they     are    in–Situ
of moulding temperature. The study shows that           Polymerization, emulsion polymerization, solution
there is an optimum moulding temperature at             exfoliation and melt intercalation [10]. Moulding or
which maximum mechanical properties are                 moulding is the process of manufacturing by
obtained [1,2].                                         shaping pliable raw material using a rigid frame or
         Similarly,     the      actual     surface     model called a pattern. Injection moulding is a
temperature of the mould cores and cavities are         manufacturing process for producing parts from
related to, but not necessarily the same as, the        both thermoplastic and thermosetting plastic
temperature of the fluid passing through the            materials [11,12]. Material is fed into a heated
channels in the mould. It is generally understood       barrel, mixed, and forced into a mould cavity where
that melt temperature has an effect on viscosity.       it cools and hardens to the configuration of the
But melt temperature also has an influence on           cavity[13].
the final molecular weight of the polymer in the             In injection moulding, moulding conditions
moulded part[3,4].                                      have a significant influence on the final properties
Keywords: Polymer nanocomposites, nano kaolin           of the material regardless of the part design. Two of
clay, injection moulding, moulding temperature.         the process conditions that have a substantial
                                                        influence on the behaviour of the polymer are the
1. Introduction                                         melt temperature and mould temperature. Melt
         A nanocomposite is as a multiphase solid       temperature is the actual temperature of the polymer
material where one of the phases is a nanomaterial      as it exits the nozzle and enters the mould.
which has one, two or three dimensions of less than     Similarly, the actual surface temperature of the
100 nanometers (nm), or structures having nano-         mould cores and cavities are related to, but not
scale repeat distances between the different phases     necessarily the same as, the temperature of the fluid
that make up the material. In the broadest sense this   passing through the channels in the mould. It is
definition can include porous media, colloids, gels     generally understood that melt temperature has an
and copolymers, but is more usually taken to mean       effect on viscosity. But melt temperature also has an
the solid combination of a bulk matrix and nano-        influence on the final molecular weight of the
dimensional phase(s) differing in properties due to     polymer in the moulded part. Mould temperature
dissimilarities in structure and chemistry [5].         has perhaps a less obvious but often more profound

                                                                                             1922 | P a g e
Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and
                   Applications (IJERA) ISSN: 2248-9622 www.ijera.com
                    Vol. 2, Issue 5, September- October 2012, pp.1922-1926
effect on final properties. In semi-crystalline        moulding temperature whereas for fibre reinforced
materials the mould temperature is an important        composites it is 1900C. The flexural strength or
factor in determining the degree of crystallinity in   three point bending of composites with different
the polymer [14, 15].                                  moulding temperatures are shown in Figure 3.
                                                       Similar trend as tensile strength is obtained for
2. Experimental                                        flexural strength also. The addition of glass fibre
2.1 Materials                                          and nanoclay increases the flexural strength and
         Polypropylene homo polymer (PP):              modulus.
(REPOLH110MA) and high density polyethylene                                        42                                              Pure




                                                        Tensile strength N/mm2
(HDPE) (REPOL H110MA) were supplied by M/s                                         40                                              P+GF
Reliance Industries Ltd., Hazira, Gujarat                                          38                                              P+A-CLAY
Nanoclay: Nanocaliber-100 both modified and                                        36                                              P+A-CLAY+GF
unmodified clay with ion exchange ,supplied by                                     34                                              P+U-Clay+GF
English     Indian      Clays      Limited  ,Veli,                                 32                                              P +U-clay
Thiruvananthapuram, Kerala,India. The clay is one                                  30
dimensionally nano sized, ion exchanged with                                                   180°C      190°C     200°C
cationic amino salts and spray dried. Glass Fibre                                               Moulding Temperature 0C
supplied by SHARON ENTERPRISES INDIA                   Fig.1 Tensile Strength of composites moulded at
LIMITED, Kochi, Kerala, was used in the study.         different temperatures

2.2 Methods
                                                                                       3200                                      Pure
         Preparation of hybrid composites: All           Tensile modulus
                                                                                       2700                                      P+GF
composites were prepared in an internal mixer
                                                             N/mm2

Torque Rheometer (Thermo Haake Rheocord 600).                                          2200                                      P +U-clay

The rotor speed was set at 50 rpm. The components                                      1700                                      P+A-CLAY

of 40 g were loaded to the mixing chamber through                                      1200
                                                                                                                                 P+A-CLAY+GF
the hopper and compounded at 1600C temperature                                                                                   P+U-Clay+GF
                                                                                        700
for 8 minutes , with rotor speed of 50 rpm. Nano                                                 180°C     190°C     200°C
clay used was preheated to about 750C for 45                                                     Moulding Temperature 0C
minutes to remove moisture content and polymers        Fig.2 Tensile Modulus of composites moulded at
taken in the 80% PP and 20%HDPE by weight are          different temperatures
melt compounded in the Haake melt mixer. The                     For polymer/clay composites the optimum
composites so prepared were hot pressed in a           moulding temperature for high flexural strength is
hydraulic press, cut into pieces and moulded using a   1800C whereas for fibre reinforced composites it is
semi-automatic plunger type injection moulding         1900C. This is because the fibre loading increases
machine.                                               viscosity and hence reduce proper flow and
                                                       orientation of molecules during moulding.
          Testing of hybrid composites: The
specimens obtained after moulding were tested for                                 49
                                                        Flexural Strength N/mm2




tensile and flexural properties in a Shimadzu                                     47
                                                                                                                                     Pure
Autograph Universal Testing Machine (UTM)),                                       45                                                 P+GF
impact strength in Resil Impact Testing Machine                                   43                                                 P+U-clay
according     to   ASTM     standards.   Thermal                                  41
characterization is done by differential scanning                                 39
                                                                                                                                     P+A-clay

calorimetry(DSC) and TAӨ600 model is used for                                     37                                                 P+A-caly+GF
thermogravimetric analysis (TGA). SEM images                                      35                                                 P +U-Clay +GF
were taken with JSM 6390 with an accelerator                                                  180°C       190°C       200°C
voltage20 kV on a vacuum atmosphere. X-ray                                                       Moulding Temperature 0C
diffraction (XRD) is also used for morphological       Fig.3 Flexural Strength of composites moulded at
study and is done using broken advanced X-ray          different temperatures
diffractometer.                                                                        3950                                         P+GF
                                                                                       3450
                                                        Flexural Modulus




                                                                                                                                    P +U-clay
3. Results and discussion                                                              2950
                                                                                                                                    P+A-CLAY
                                                             N/mm2




3.1 Mechanical Properties                                                              2450
                                                                                                                                    P+A-CLAY+GF
          The tensile strength and modulus of                                          1950
                                                                                                                                    P+U-Clay+GF
nanocomposites moulded at three different                                              1450
                                                                                                                                    Pure
temperatures are shown in Figure.1 and 2. The                                           950
addition of clay to the fibre reinforced composites                                     450
affects its strength very much. For polymer clay                                                  180°C     190°C     200°C

composites higher strength is obtained for 1800C                                                  Moulding Temperature 0C


                                                                                                                              1923 | P a g e
Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and
                                         Applications (IJERA) ISSN: 2248-9622 www.ijera.com
                                          Vol. 2, Issue 5, September- October 2012, pp.1922-1926
Fig.4 Flexural modulus of composites moulded at                                                                        2                                 P+A-Clay+GF
different temperatures                                                                                                                                   180C
                                                                                                                                                         P+GF 180C




                                                                                            Weight Derivative %/0C
                                                                                                                     1.5
                          0.4                                                                                                                            P+A-clay+GF
                                                                             Pure
 Impact Strength N/mm2



                                                                                                                                                         190C
                         0.35                                                P+GF                                      1
                                                                             P+U-clay
                          0.3                                                                                        0.5
                                                                             P+A-CLAY
                         0.25
                                                                             P+U-clay+GF                               0
                          0.2                                                P+A-clay+GF
                                                                                                                     -0.5
                                                                                                                            0   200   400     600           800
                         0.15
                                    180°C       190°C         200°C                                          Temperature 0C
                                            Moulding temperature 0C
                                                                                           Fig.7 Temperature Dependence                             of      Weight
Fig.5. Impact strength of composites moulded at                                            Derivative for Composites.
different temperatures
                                                                                           Table. 2 Results of TGA of different composites
         From figure.5 it is found that the impact                                                            Temperature
strength is high for composites moulded at 1900C.                                                                             Temperature
                                                                                                              of onset of
Further temperature of moulding will cause                                                                                    of complete
                                                                                             Composites       thermal
degradation of polymers which reduces the strength.                                                                           degradation,
                                                                                                              degradation,
                                                                                                                              °C
                                                                                                              °C
3.2 Thermal Properties                                                                       P+GF
         In order to investigate the effect of                                                                345.89          470.25
                                                                                             (180°C)
different nanofillers on the degree of crystallinity,                                        P+A-Clay+
DSC curves of compounds were analysed.                                                                        350.99          470
                                                                                             GF (180°C)
Table.1 Crystallization Temperature of composites                                            P+A-Clay+
    Composite                  Crystallization                                                                331.06          474.64
                                                                                             GF (190°C)
                               Temperature 0C
    PP/HDPE/GF                 113.81                                                                 These results indicate that as moulding
    PP/HDPE/A-clay             119.08                                                      temperature increases, thermal stability of
    PP/HDPE/A-clay/GF          119.98                                                      composites decreases. Thermal stability of hybrid
         The results show that the crystallinity                                           composites is higher than that of the composite
increases in the presence of nanoclay and it’s not                                         without nanoclay (PP/HDPE/20%GF). At the same
affected by the processing conditions used. The                                            time, the hybrid composite moulded at 1800C gives
presence of nanoclay platelets dispersed in the                                            better performance than that moulded at 1900C.
hybrid matrix promotes heterogeneous nucleation,
thus increases the crystallization rate and increases                                      3.3 Morphological Study
the degree of crystallinity.                                                                         The pictures do however give a much
           Thermal stability of the hybrid composite                                       better feel of the particles in 3D space. Several SEM
was studied using TGA. The thermogravimetric                                               images were taken at various magnifications to
curves are plotted in figures 6 and 7. The addition                                        characterize the hybrid composite. SEM results for
of clay increases the decomposition temperature of                                         fractured surface of moulded samples are given
hybrid composites.                                                                         below. SEM micrograph of fracture surface of
                                                                                           80PP/20HDPE pure blend is given in the figure.8
                         120

                         100                                   P+GF 180C

                          80
 Weight %




                                                               P+A-clay+GF 180C
                          60
                                                               P+A-Clay+GF 190C
                          40

                          20

                           0
                                0     200     400       600   800
                                        Temperature 0C                                     Fig.8 SEM image of                           fracture    surface        of
                                                                                           80PP/20HDPE pure blend.
Fig.6 Temperature Dependence of Weight Loss for
Composites



                                                                                                                                               1924 | P a g e
Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and
                   Applications (IJERA) ISSN: 2248-9622 www.ijera.com
                    Vol. 2, Issue 5, September- October 2012, pp.1922-1926
Figure.9 shows the tensile fracture surface           nanoclay is there along with the short fibres in the
micrograph of PP/HDPE/20%GF. In this case the         polymer matrix and better interaction between the
glass fibres are evenly distributed in the polymer    nanoclay and fibres can be seen. Matrix is more
matrix.                                               homogeneous and more adhesion between fibre and
                                                      matrix is seen in the presence of nanoclay As the
                                                      result, PP/HDPE/2%Amino-clay/20%GF hybrid
                                                      composite gives better strength as compared to that
                                                      of the composite with fibre alone.




Fig.9 SEM image of          fracture   surface   of
PP/HDPE/GF composite.


                                                      Fig.12 SEM images of Hybrid composite moulded
                                                      at 1800C




Fig.10 SEM Image of Fracture Surface of
PP/HDPE/A-clay Composite
Figure.10 shows the tensile fracture surface of
PP/HDPE/2% Amino-clay, in this case nanoclay is
dispersed in the polymer matrix. In these figures,    Fig.13 SEM image of PP/HDPE/2% Amino-
we can see the maximum exfoliation.                   clay/20%GF
                                                                  Figure.12 and figure.13 represents the
                                                      SEM images of PP/HDPE/A-clay/GF hybrid
                                                      composites moulded at 1800C and 1900C
                                                      respectively. There is not much variation found in
                                                      the dispersion of clay particles in the polymer
                                                      matrix. These results show that         the moulding
                                                      conditions do not affect the morphological features
                                                      of the composites.
                                                                X-ray diffraction is used to determine
                                                      crystal morphology of the nanoparticles in the
                                                      composite. Nanoclay is in the form of layers or
                                                      stacks of platelets. This leads to isomorphic
                                                      substitution within layers and generates a negative
                                                      charge exchange capacity. During melt mixing,
                                                      polymer precursor or preformed polymer penetrated
                                                      in to the gallery space between the layers. In the
                                                      composite, the gap between the single sheets (d-
                                                      spacing value) should be widened to get enhanced
                                                      properties.
                                                                In this study the XRD analysis is
                                                      performed for pure Amino-clay, PP/HDPE/A-clay
                                                      composite and PP/HDPE/A-clay/Glass Fibre
                                                      composites. The results obtained are plotted in the
Fig.11 SEM images of PP/HDPE/2% Amino-                figure 12. It is shown that the d-spacing value of the
clay/20%GF.                                           PP/HDPE/A-clay composite is higher than that of
Figure.11 shows the tensile fracture surface of       amino-clay.
PP/HDPE/2% Amino-clay/20%GF, in this case


                                                                                           1925 | P a g e
Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and
                                Applications (IJERA) ISSN: 2248-9622 www.ijera.com
                                 Vol. 2, Issue 5, September- October 2012, pp.1922-1926
 d-spacing value 0A   8                                   A-clay             [5].    Hasmukh A Patel, Rajesh S Somani, Hari
                                                                                     C Bajaj And Raksh V Jasra, “Nanoclays
                                                          P+A-Clay
                      6                                                              for polymer nanocomposites”, Bull. Mater.
                                                          P+A-clay+ GF               Sci., Vol. 29, No. 2, April 2006, pp. 133–
                                                                                     145. © Indian Academy of Sciences.
                      4                                                      [6].    Clays, Nanoclays, and Montmorillonite
                                                                                     Minerals      By      FAHEEM        UDDIN,
                      2                                                              Metallurgical And Materials Transactions,
                                                                                     Volume 39a, December 2008.
                17        12
                           22
                  Angle 2θ°                                                  [7].    P.M. Ajayan, L.S. Schadler, P.V. Braun
Fig.14 Results of XRD- Comparison of d-spacing                                       (2003). Nanocomposite science and
value of composites.                                                                 technology. Wiley. ISBN 3527303596.
                                                                             [8].    D.Y.Godovsky(2000) Applications of
         In hybrid composite the d-spacing value is                                  Polymer-Nanocomposites. Advances in
further increased, which indicate the complete                                       Polymer science vol. 153:165-205.
dispersion of nanoclay and glass fibres in the                               [9].    J.K. William, H.H. James, A.M. Jefferey,
polymer matrix. This increased d-spacing value                                       “Handbook       of      Polypropylene    and
explains the enhanced properties of hybrid                                           Polypropylene Composites”, Edited by
composites compared to others.                                                       Haruhun G. Karian, Mercel Dekker Inc,
                                                                                     New York, 1999.
Table.3 Results of XRD showing d-spacing values                              [10].   E. Manias, A. Touny, L. Wu, K.
of Amino clay and composites                                                         Strawhecker, B. Lu, and T. C. Chung,
   Angle d-spacing value, °A                                                         Chem.                                 Mater.,
   2θ°                                                                               Polypropylene/Montmorillonite
                                                                                     Nanocomposites. Review of the Synthetic
                                                        PP/HDPE/A-                   Routes and Materials Properties, Vol. 13,
                                  Amino    PP/HDPE/                                  3516–3523, 2001.
                                                        clay/Glass
                                  Clay     A-clay                            [11].    H. Ishida, S. Campbell, and J. Blackwell,
                                                        Fibre
                                                                                     Chem. Mater,         General Approach to
                12.28             7.204    7.29         7.351                        Nanocomposite Preparation, Vol. 12,
                19.89             4.459    4.582        4.654                        1260–1267, 2000.
                21.13             4.201    4.317        4.397                [12].   Robert H. Todd, Dell K. Allen, Leo Alting.
                24.74             3.595    3.634        3.697                        Manufacturing Processes Reference Guide
                                                                                     Industrial Press Inc., 1994. pg. 243.
4. Conclusions                                                               [13].   Mora,       JC;        Polymers       Product
     The effect of moulding temperature on the                                       Manufacturing; Part Design, Mold Design,
properties of composite based on PP/HDPE (80/20)                                     Process, Production Controls, & Facilities.
was studied in this work. The study shows that the                           [14].   Douglas M. Bryce. Plastic Injection
moulding temperature has significant effect on the                                   Molding:        Manufacturing         Process
mechanical and thermal properties of the composite.                                  Fundamentals. SME, 1996.
The optimum moulding temperature depends on the                              [15].   “The Importance of Melt & Mold
desired mechanical/thermal properties of the                                         Temperature” By Michael Sepe from
composite for its application. The incorporation of                                  Michael P. Sepe LLC From: Plastics
nano clay and glass fibres improves the properties of                                Technology Issue: December 2011.
PP/HDPE blends. The enhancement in physical
properties is well explained by morphological
characterization.

References
        [1].                   Tony     Whelan,      Injection   Molding
                               Handbook 2nd Ed pg 13
        [2].                   Mora,       JC;     Polymers       Product
                               Manufacturing; Part Design, Mold Design,
                               Process, Production Controls, & Facilities.
        [3].                   “The Importance of Melt & Mold
                               Temperature” By Michael Sepe from
                               Michael P. Sepe LLC From: Plastics
                               Technology Issue: December 2011.
        [4].                   HI *Whelan, Tony. Polymer Technology
                               Dictionary Springer, 1994.

                                                                                                                 1926 | P a g e

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La2519221926

  • 1. Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.com Vol. 2, Issue 5, September- October 2012, pp.1922-1926 Effect Of Moulding Temperature On The Properties Of Polypropylene/High Density Polyethylene/Clay/Glass Fibre Composites Ranjusha J P1, Anjana R1 and K E George2 1. Dept. of Chemical Engg., Govt. Engg. College, Thrissur 2. Dept. of Polymer Science and Rubber Technology, CUSAT Abstract Polymer nanocomposite(PNC) is a polymer or Polymer nanocomposites have emerged copolymer having dispersed in its nanoparticles. as a high-tech engineering material for a variety These may be of different shape (e.g., platelets, of applications. The present paper emphasis on fibres, spheroids), but at least one dimension must the comparison of polymer nanocomposites synthesized under different moulding be in the range of 1 to 80 nm. These PNC's belong temperature and the effects of moulding to the category of multi-phase systems (blends, temperature on the preparation of polymer composites, and foams) that consume nearly 95% of nanocomposites by different characterization plastics production. These systems require techniques. Also aims to investigate the enhanced controlled mixing/compounding, stabilization of the physical and mechanical properties of polymer achieved dispersion, orientation of the dispersed nanocomposites with different nanofillers. phase, and the compounding strategies for all Polymer hybrid nanocomposites based on poly multiphase systems, including PNC, are similar [6- propylene(PP) (80% of blend)and high density 8]. poly ethylene(HDPE)(20% of blend) blend is selected for the present study. Nanofillers such as Synthesis of polymer nanocomposites nano kaolin clay (2%) and/or glass include mixing /addition of nanofillers into the fibre(GF)(20%) is incorporated in the polymer polymer and moulding the graft obtained into matrix. desired shapes [9]. Polymer–clay nanocomposites The properties of processed goods, can be synthesized via four mixing approaches particularly based on polymer blends, are highly depending on the starting materials and the depend on the processing variables and the effect processing techniques; they are in–Situ of moulding temperature. The study shows that Polymerization, emulsion polymerization, solution there is an optimum moulding temperature at exfoliation and melt intercalation [10]. Moulding or which maximum mechanical properties are moulding is the process of manufacturing by obtained [1,2]. shaping pliable raw material using a rigid frame or Similarly, the actual surface model called a pattern. Injection moulding is a temperature of the mould cores and cavities are manufacturing process for producing parts from related to, but not necessarily the same as, the both thermoplastic and thermosetting plastic temperature of the fluid passing through the materials [11,12]. Material is fed into a heated channels in the mould. It is generally understood barrel, mixed, and forced into a mould cavity where that melt temperature has an effect on viscosity. it cools and hardens to the configuration of the But melt temperature also has an influence on cavity[13]. the final molecular weight of the polymer in the In injection moulding, moulding conditions moulded part[3,4]. have a significant influence on the final properties Keywords: Polymer nanocomposites, nano kaolin of the material regardless of the part design. Two of clay, injection moulding, moulding temperature. the process conditions that have a substantial influence on the behaviour of the polymer are the 1. Introduction melt temperature and mould temperature. Melt A nanocomposite is as a multiphase solid temperature is the actual temperature of the polymer material where one of the phases is a nanomaterial as it exits the nozzle and enters the mould. which has one, two or three dimensions of less than Similarly, the actual surface temperature of the 100 nanometers (nm), or structures having nano- mould cores and cavities are related to, but not scale repeat distances between the different phases necessarily the same as, the temperature of the fluid that make up the material. In the broadest sense this passing through the channels in the mould. It is definition can include porous media, colloids, gels generally understood that melt temperature has an and copolymers, but is more usually taken to mean effect on viscosity. But melt temperature also has an the solid combination of a bulk matrix and nano- influence on the final molecular weight of the dimensional phase(s) differing in properties due to polymer in the moulded part. Mould temperature dissimilarities in structure and chemistry [5]. has perhaps a less obvious but often more profound 1922 | P a g e
  • 2. Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.com Vol. 2, Issue 5, September- October 2012, pp.1922-1926 effect on final properties. In semi-crystalline moulding temperature whereas for fibre reinforced materials the mould temperature is an important composites it is 1900C. The flexural strength or factor in determining the degree of crystallinity in three point bending of composites with different the polymer [14, 15]. moulding temperatures are shown in Figure 3. Similar trend as tensile strength is obtained for 2. Experimental flexural strength also. The addition of glass fibre 2.1 Materials and nanoclay increases the flexural strength and Polypropylene homo polymer (PP): modulus. (REPOLH110MA) and high density polyethylene 42 Pure Tensile strength N/mm2 (HDPE) (REPOL H110MA) were supplied by M/s 40 P+GF Reliance Industries Ltd., Hazira, Gujarat 38 P+A-CLAY Nanoclay: Nanocaliber-100 both modified and 36 P+A-CLAY+GF unmodified clay with ion exchange ,supplied by 34 P+U-Clay+GF English Indian Clays Limited ,Veli, 32 P +U-clay Thiruvananthapuram, Kerala,India. The clay is one 30 dimensionally nano sized, ion exchanged with 180°C 190°C 200°C cationic amino salts and spray dried. Glass Fibre Moulding Temperature 0C supplied by SHARON ENTERPRISES INDIA Fig.1 Tensile Strength of composites moulded at LIMITED, Kochi, Kerala, was used in the study. different temperatures 2.2 Methods 3200 Pure Preparation of hybrid composites: All Tensile modulus 2700 P+GF composites were prepared in an internal mixer N/mm2 Torque Rheometer (Thermo Haake Rheocord 600). 2200 P +U-clay The rotor speed was set at 50 rpm. The components 1700 P+A-CLAY of 40 g were loaded to the mixing chamber through 1200 P+A-CLAY+GF the hopper and compounded at 1600C temperature P+U-Clay+GF 700 for 8 minutes , with rotor speed of 50 rpm. Nano 180°C 190°C 200°C clay used was preheated to about 750C for 45 Moulding Temperature 0C minutes to remove moisture content and polymers Fig.2 Tensile Modulus of composites moulded at taken in the 80% PP and 20%HDPE by weight are different temperatures melt compounded in the Haake melt mixer. The For polymer/clay composites the optimum composites so prepared were hot pressed in a moulding temperature for high flexural strength is hydraulic press, cut into pieces and moulded using a 1800C whereas for fibre reinforced composites it is semi-automatic plunger type injection moulding 1900C. This is because the fibre loading increases machine. viscosity and hence reduce proper flow and orientation of molecules during moulding. Testing of hybrid composites: The specimens obtained after moulding were tested for 49 Flexural Strength N/mm2 tensile and flexural properties in a Shimadzu 47 Pure Autograph Universal Testing Machine (UTM)), 45 P+GF impact strength in Resil Impact Testing Machine 43 P+U-clay according to ASTM standards. Thermal 41 characterization is done by differential scanning 39 P+A-clay calorimetry(DSC) and TAӨ600 model is used for 37 P+A-caly+GF thermogravimetric analysis (TGA). SEM images 35 P +U-Clay +GF were taken with JSM 6390 with an accelerator 180°C 190°C 200°C voltage20 kV on a vacuum atmosphere. X-ray Moulding Temperature 0C diffraction (XRD) is also used for morphological Fig.3 Flexural Strength of composites moulded at study and is done using broken advanced X-ray different temperatures diffractometer. 3950 P+GF 3450 Flexural Modulus P +U-clay 3. Results and discussion 2950 P+A-CLAY N/mm2 3.1 Mechanical Properties 2450 P+A-CLAY+GF The tensile strength and modulus of 1950 P+U-Clay+GF nanocomposites moulded at three different 1450 Pure temperatures are shown in Figure.1 and 2. The 950 addition of clay to the fibre reinforced composites 450 affects its strength very much. For polymer clay 180°C 190°C 200°C composites higher strength is obtained for 1800C Moulding Temperature 0C 1923 | P a g e
  • 3. Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.com Vol. 2, Issue 5, September- October 2012, pp.1922-1926 Fig.4 Flexural modulus of composites moulded at 2 P+A-Clay+GF different temperatures 180C P+GF 180C Weight Derivative %/0C 1.5 0.4 P+A-clay+GF Pure Impact Strength N/mm2 190C 0.35 P+GF 1 P+U-clay 0.3 0.5 P+A-CLAY 0.25 P+U-clay+GF 0 0.2 P+A-clay+GF -0.5 0 200 400 600 800 0.15 180°C 190°C 200°C Temperature 0C Moulding temperature 0C Fig.7 Temperature Dependence of Weight Fig.5. Impact strength of composites moulded at Derivative for Composites. different temperatures Table. 2 Results of TGA of different composites From figure.5 it is found that the impact Temperature strength is high for composites moulded at 1900C. Temperature of onset of Further temperature of moulding will cause of complete Composites thermal degradation of polymers which reduces the strength. degradation, degradation, °C °C 3.2 Thermal Properties P+GF In order to investigate the effect of 345.89 470.25 (180°C) different nanofillers on the degree of crystallinity, P+A-Clay+ DSC curves of compounds were analysed. 350.99 470 GF (180°C) Table.1 Crystallization Temperature of composites P+A-Clay+ Composite Crystallization 331.06 474.64 GF (190°C) Temperature 0C PP/HDPE/GF 113.81 These results indicate that as moulding PP/HDPE/A-clay 119.08 temperature increases, thermal stability of PP/HDPE/A-clay/GF 119.98 composites decreases. Thermal stability of hybrid The results show that the crystallinity composites is higher than that of the composite increases in the presence of nanoclay and it’s not without nanoclay (PP/HDPE/20%GF). At the same affected by the processing conditions used. The time, the hybrid composite moulded at 1800C gives presence of nanoclay platelets dispersed in the better performance than that moulded at 1900C. hybrid matrix promotes heterogeneous nucleation, thus increases the crystallization rate and increases 3.3 Morphological Study the degree of crystallinity. The pictures do however give a much Thermal stability of the hybrid composite better feel of the particles in 3D space. Several SEM was studied using TGA. The thermogravimetric images were taken at various magnifications to curves are plotted in figures 6 and 7. The addition characterize the hybrid composite. SEM results for of clay increases the decomposition temperature of fractured surface of moulded samples are given hybrid composites. below. SEM micrograph of fracture surface of 80PP/20HDPE pure blend is given in the figure.8 120 100 P+GF 180C 80 Weight % P+A-clay+GF 180C 60 P+A-Clay+GF 190C 40 20 0 0 200 400 600 800 Temperature 0C Fig.8 SEM image of fracture surface of 80PP/20HDPE pure blend. Fig.6 Temperature Dependence of Weight Loss for Composites 1924 | P a g e
  • 4. Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.com Vol. 2, Issue 5, September- October 2012, pp.1922-1926 Figure.9 shows the tensile fracture surface nanoclay is there along with the short fibres in the micrograph of PP/HDPE/20%GF. In this case the polymer matrix and better interaction between the glass fibres are evenly distributed in the polymer nanoclay and fibres can be seen. Matrix is more matrix. homogeneous and more adhesion between fibre and matrix is seen in the presence of nanoclay As the result, PP/HDPE/2%Amino-clay/20%GF hybrid composite gives better strength as compared to that of the composite with fibre alone. Fig.9 SEM image of fracture surface of PP/HDPE/GF composite. Fig.12 SEM images of Hybrid composite moulded at 1800C Fig.10 SEM Image of Fracture Surface of PP/HDPE/A-clay Composite Figure.10 shows the tensile fracture surface of PP/HDPE/2% Amino-clay, in this case nanoclay is dispersed in the polymer matrix. In these figures, Fig.13 SEM image of PP/HDPE/2% Amino- we can see the maximum exfoliation. clay/20%GF Figure.12 and figure.13 represents the SEM images of PP/HDPE/A-clay/GF hybrid composites moulded at 1800C and 1900C respectively. There is not much variation found in the dispersion of clay particles in the polymer matrix. These results show that the moulding conditions do not affect the morphological features of the composites. X-ray diffraction is used to determine crystal morphology of the nanoparticles in the composite. Nanoclay is in the form of layers or stacks of platelets. This leads to isomorphic substitution within layers and generates a negative charge exchange capacity. During melt mixing, polymer precursor or preformed polymer penetrated in to the gallery space between the layers. In the composite, the gap between the single sheets (d- spacing value) should be widened to get enhanced properties. In this study the XRD analysis is performed for pure Amino-clay, PP/HDPE/A-clay composite and PP/HDPE/A-clay/Glass Fibre composites. The results obtained are plotted in the Fig.11 SEM images of PP/HDPE/2% Amino- figure 12. It is shown that the d-spacing value of the clay/20%GF. PP/HDPE/A-clay composite is higher than that of Figure.11 shows the tensile fracture surface of amino-clay. PP/HDPE/2% Amino-clay/20%GF, in this case 1925 | P a g e
  • 5. Ranjusha J P, Anjana R, K E George / International Journal of Engineering Research and Applications (IJERA) ISSN: 2248-9622 www.ijera.com Vol. 2, Issue 5, September- October 2012, pp.1922-1926 d-spacing value 0A 8 A-clay [5]. Hasmukh A Patel, Rajesh S Somani, Hari C Bajaj And Raksh V Jasra, “Nanoclays P+A-Clay 6 for polymer nanocomposites”, Bull. Mater. P+A-clay+ GF Sci., Vol. 29, No. 2, April 2006, pp. 133– 145. © Indian Academy of Sciences. 4 [6]. Clays, Nanoclays, and Montmorillonite Minerals By FAHEEM UDDIN, 2 Metallurgical And Materials Transactions, Volume 39a, December 2008. 17 12 22 Angle 2θ° [7]. P.M. Ajayan, L.S. Schadler, P.V. Braun Fig.14 Results of XRD- Comparison of d-spacing (2003). Nanocomposite science and value of composites. technology. Wiley. ISBN 3527303596. [8]. D.Y.Godovsky(2000) Applications of In hybrid composite the d-spacing value is Polymer-Nanocomposites. Advances in further increased, which indicate the complete Polymer science vol. 153:165-205. dispersion of nanoclay and glass fibres in the [9]. J.K. William, H.H. James, A.M. Jefferey, polymer matrix. This increased d-spacing value “Handbook of Polypropylene and explains the enhanced properties of hybrid Polypropylene Composites”, Edited by composites compared to others. Haruhun G. Karian, Mercel Dekker Inc, New York, 1999. Table.3 Results of XRD showing d-spacing values [10]. E. Manias, A. Touny, L. Wu, K. of Amino clay and composites Strawhecker, B. Lu, and T. C. Chung, Angle d-spacing value, °A Chem. Mater., 2θ° Polypropylene/Montmorillonite Nanocomposites. Review of the Synthetic PP/HDPE/A- Routes and Materials Properties, Vol. 13, Amino PP/HDPE/ 3516–3523, 2001. clay/Glass Clay A-clay [11]. H. Ishida, S. Campbell, and J. Blackwell, Fibre Chem. Mater, General Approach to 12.28 7.204 7.29 7.351 Nanocomposite Preparation, Vol. 12, 19.89 4.459 4.582 4.654 1260–1267, 2000. 21.13 4.201 4.317 4.397 [12]. Robert H. Todd, Dell K. Allen, Leo Alting. 24.74 3.595 3.634 3.697 Manufacturing Processes Reference Guide Industrial Press Inc., 1994. pg. 243. 4. Conclusions [13]. Mora, JC; Polymers Product The effect of moulding temperature on the Manufacturing; Part Design, Mold Design, properties of composite based on PP/HDPE (80/20) Process, Production Controls, & Facilities. was studied in this work. The study shows that the [14]. Douglas M. Bryce. Plastic Injection moulding temperature has significant effect on the Molding: Manufacturing Process mechanical and thermal properties of the composite. Fundamentals. SME, 1996. The optimum moulding temperature depends on the [15]. “The Importance of Melt & Mold desired mechanical/thermal properties of the Temperature” By Michael Sepe from composite for its application. The incorporation of Michael P. Sepe LLC From: Plastics nano clay and glass fibres improves the properties of Technology Issue: December 2011. PP/HDPE blends. The enhancement in physical properties is well explained by morphological characterization. References [1]. Tony Whelan, Injection Molding Handbook 2nd Ed pg 13 [2]. Mora, JC; Polymers Product Manufacturing; Part Design, Mold Design, Process, Production Controls, & Facilities. [3]. “The Importance of Melt & Mold Temperature” By Michael Sepe from Michael P. Sepe LLC From: Plastics Technology Issue: December 2011. [4]. HI *Whelan, Tony. Polymer Technology Dictionary Springer, 1994. 1926 | P a g e