- Original article
- Open Access
Properties of PMMA/clay nanocomposites prepared using various compatibilizers
© Kumar et al. 2015
- Received: 7 March 2015
- Accepted: 11 May 2015
- Published: 3 June 2015
In the fabrication of polymer/clay nanocomposites, the compatibilizer plays a vital role in altering the properties of nanocomposite systems. The present work primarily deals with the development of poly(methyl methacrylate) (PMMA)/clay nanocomposites containing different compatibilizers (PP-g-MA, PE-g-MA and PS-g-MA) with 5 wt.% nanoclay.
The various PMMA nanocomposites were prepared by melt intercalation method using twin screw extruder followed by injection moulding to make specimens for mechanical testing.
The mechanical, thermal and morphological properties of nanocomposites were evaluated by tensile test, impact, hardness, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The intercalated structure of the PMMA nanocomposites is validated by XRD and TEM analysis. The results are found to be good agreement with each other.
The TGA data demonstrate that PMMA nanocomposites exhibit enhanced thermal stability of 22-36 °C with respect to pure PMMA, at 50% weight loss is considered as point of reference. The PMMA nanocomposite prepared with PS-g-MA compatibilizer promotes adequate interface adhesion between the nanoclay and polymer matrix. As a result, PMMA-5-PS sample displays improved mechanical properties over PMMA-5-PP and PMMA-5-PE samples. The maximum improvement of tensile strength, Young’s modulus and hardness for the PMMA-5-PS nanocomposites over PMMA-5-PE is estimated to be 8, 2 and 26 %, respectively.
Polymer nanocomposites have received considerable interest, both in academia and in industry, because of their enhanced properties at very low loading levels compared with conventional polymer composites. They generally display superior properties such as mechanical, thermal, gas-barrier property, flame retardant and dimensional stability with respect to conventional filler composites. These improved properties are often obtained by the incorporation of nanofillers with preferably less than 100 nm in size (Ray and Okamoto 2003). Several nanoparticulates such as clay minerals, carbon nanotubes, silica and TiO2 nanoparticles are generally used in altering the physical, mechanical and thermal properties of polymers (Ahmad et al. 2006; Zheng et al. 2005; Lee et al. 2006; Etienne et al. 2007).
PMMA is an atactic, amorphous and optically transparent material with high strength, excellent dimensional stability and outdoor weather performance. However, its application is restricted at higher temperature due to its relatively poor thermal stability. To overcome this problem, nanotechnology is implemented in this field, in order to further improve the properties of PMMA. In such technology, montmorillonite (MMT) modified with organic modifier, also known as organoclay, is impregnated into polymer matrix. To obtain nanoscale dispersion of the organoclay, the modification of PMMA matrix with polar molecules is recommended prior to organoclay incorporation. Compatibilizers are generally added in the nanocomposites in order to improve the interfacial adhesion between organoclay and polymer matrix that generally results in enhanced mechanical and morphological properties (Lim et al. 2006; Chow et al. 2005).
Various methods have been employed for the synthesis of polymer nanocomposites with better properties such as solvent blending, in situ polymerization and melt-intercalation technique (Krajnc and Sebenik 2009; Li et al. 2008; Fu and Naguib 2006). Melt intercalation has been widely accepted and an economical method for industrial applications. The effect of various compatibilizers on polymer matrix or blends has been studied by numerous authors (Shanks and Cerezo 2012; Dayma et al. 2011; Jiang et al. 2003; Lu et al. 2004, Zhu et al. 2008). The HDPE and nitrile copolymer nanocomposites with organoclay were synthesized by solution blending method and found that greater dispersion was obtained in nitrile copolymer matrix (Jeon et al. 1998). Kim et al. (2007a, 2007b) developed PP/clay nanocomposites. They reported that the aspect ratio of clay decreased when the clay content increased and the aspect ratio increased with an increase in the PP-g-MA content. Kitayama et al. (1991) prepared triblock copolymer of PMMA and polyisobutylene by anionic polymerization and reported that block copolymer formed was rigid spherical particles, which can be used as elastomer. Kouini and Serier (2012)) found that the impact property increased with the incorporation of PP-g-MA in PP/PA66 nanocomposites. TPO/PP-g-MA/MMT nanocomposites prepared by Kim et al. (2007a, 2007b) revealed that the modulus and yield strength enhanced by increasing PP-g-MA/organoclay ratios. Zhou et al. (2007) prepared the PMMA/PVC by melt blending using PB-g-MMA as impact modifier. The result clearly indicated that the sample broke in brittle mode when the matrix was PMMA rich, while in PVC-rich system, ductile fracture occurred. Lai et al. (2009) fabricated PP/nanocomposites with two different compatibilizers (POE-g-MA and PP-g-MA) by melt mixing method. They found that PP-g-MA compatibilized system conferred higher tensile strength, modulus and optical properties as compared to POE-g-MA compatibilized system. Wang et al. (2013) reported the development of PP nanocomposites using PP-g-MA by compression method. The results suggested that MCM-41 and SBA-15 exhibited favourable effect on flammability and tensile properties of PP nanocomposites. Lin et al. (2013) studied β-PP/PA6 blends, and the results indicated that the addition of PP-g-MA resulted in PP-g-MA graft copolymer, which improved the interfacial adhesion and reduced the sizes of PA6 domains. Lee et al. (2005) synthesized the PE/clay nanocomposites containing PP-g-MA by melt-intercalation method. They found that tensile and gas barrier properties were improved at 7 % clay loading. Zhao et al. (2008) reported that the Tg and thermal decomposition temperature of PMMA nanocomposite were enhanced by 23 and 93 °C, respectively, in the presence of octavinyl-polyhedral oligomeric silseoquioxane (OV-POSS). In the study of Wang et al. (2011), the addition of PMMA/MCM-41 filler and PP-g-MA in PP nanocomposites showed better tensile and impact properties. Quintanilla et al. (2006) prepared PP/MMT nanocomposites with different grafting efficiency of PP-g-MA. The result clearly indicated that PP/Cloisite 20A nanocomposites with higher efficiency PP-g-MA (2.0) exhibited better tensile and impact properties as compared to Cloisite 30B and neat clay. The incorporation of POE-g-MA in PET/PP blends considerably improved mechanical properties such as elongation at break and impact strength (Chiu and Hsiao 2006). It is very clear from the literature review that the compatibilizer plays a major role in improving the properties of nanocomposite systems. Hence, it is essential to examine the role of various compatibilizers on the properties of PMMA nanocomposites.
To our best knowledge, no researchers have investigated the influence of compatibilizers on the properties of PMMA nanocomposites prepared using nanoclay modified with 15–35 % octadecylamine and 0.5–5 wt.% aminopropyltriethoxysilane. Thus, the aim of the present work is to investigate the role of various compatibilizers (PP-g-MA, PE-g-MA, PS-g-MA) on the properties of PMMA/clay nanocomposites developed by melt blending method. The morphological, thermal and mechanical properties of the nanocomposites are evaluated using various techniques.
PMMA (IG 840) used in this study was a commercial product from LG Polymers, South Korea. The melt flow index (MFI at 230 °C and 3.8 kg load) and specific gravity of PMMA were 5.8 g/10 min and 1.18, respectively. Nanoclay (Nanomer 1.31 PS, MMT clay surface modified with 15–35 % octadecylamine and 0.5–5 wt.% aminopropyltriethoxysilane), polypropylene-grafted maleic anhydride (PP-g-MA), polyethylene-grafted maleic anhydride (PE-g-MA) and polystyrene-block-poly(ethylene-ran-butylene)-block-polystyrene-graft-maleic anhydride (PS-g-MA) were purchased from Sigma-Aldrich, USA.
Preparation of PMMA/clay nanocomposites
Prior to melt intercalation, PMMA pellets and organoclay were dried in a vacuum oven at 80 and 65 °C, respectively, for 12 h. PMMA nanocomposites containing 5 wt.% of organoclay and 5 wt.% of compatibilizer were prepared by melt intercalation technique in a twin screw extruder (Make: Specifiq Engineering and Automats, Vadodara, India; Model-ZV-20 HI TORQUE). In a typical experiment, PMMA, organoclay and different compatibilizers were fed into the extruder and the obtained extrudate was quenched in water at room temperature. Subsequently, the extrudate was cut into pellets and then dried before being injection moulded (JSW, Japan; Model-180 High Pressure) at 180–250 °C to make specimens for mechanical testing. Hereafter, the nanocomposites prepared using PP-g-MA, PE-g-MA and PS-g-MA along with 5 wt.% nanoclay is referred as PMMA-5-PP, PMMA-5-PE and PMMA-5-PS. Pure PMMA sample was also prepared by a similar method in the absence of compatibilizer and clay.
Fourier transform infrared spectroscopy (FTIR)
The FTIR analysis of different nanocomposites was performed on Shimadzu Fourier transform infrared spectroscopy to confirm the different functional peaks in nanocomposites.
X-ray diffraction analysis
X-ray diffraction (XRD) profile of organoclay and various PMMA nanocomposite samples were measured under air at room temperature by AXS D8 ADVANCE Fully Automatic Powder X-ray Diffractometer (Bruker) with Cu-Kα radiation (λ = 0.15406 nm) and Ni filter. The patterns were recorded for 2θ range from 1°–50° with 0.05 s−1 scan speed.
Transmission electron microscopy
The transmission electron microscopy (TEM) image of PMMA nanocomposites were obtained on JOEL, Model-JEM-2100 transmission electron micro analyser with an accelerating voltage of 200 KV.
The tensile properties were measured based on ASTM D 638 at a crosshead speed of 5 mm/min using INSTRON (M 3382, UK) universal testing machine. The flexural strength and modulus of PMMA nanocomposites were measured according to ASTM D790. The test was carried out on INSTRON (M 3382, UK) universal testing machine. A rectangular bar was placed on the 3-point bending configuration at 1.45 mm/min deformation rate. Both the tests were performed at 23 ± 2 °C and 50 ± 5 % relative humidity. Five samples were tested for each composition, and the average value was reported. Impact strength measurements were performed using an impactometer (M/s Tinius Olsen, USA). The hardness (Shore D) of the nanocomposites was measured according to ASTM D2240. Ten readings were taken at different regions for each sample, and average value was reported.
Differential scanning calorimetry (DSC) was performed on a Metler Toledo-1 series to evaluate the glass transition temperature (Tg) of the PMMA nanocomposites. Samples were heated from 25 to 250 °C at a rate of 10 °C min−1 under nitrogen atmosphere.
Thermo gravimetric analysis
The thermogravimetric analysis (TGA) was recorded on Mettler Toledo thermoanalyser under a nitrogen atmosphere at a heating rate of 10 °C/min from room temperature to 700 °C.
The FTIR of PMMA and its nanocomposites show a characteristic peak at 1731 cm−1, which denotes the >C = O group present in the polymer. The band at 986 cm−1 denotes the -C-H bending of polymer chain. The peak observed at 1436 cm−1 corresponds to -O-CH3 deformation of PMMA. The band exhibited at 2994 cm−1 is due to the ester methyl stretching vibrations. The peak appeared at 2950 cm−1 corresponding to the asymmetric stretching vibration of -CH3 group. A very clear and sharp peak is noticed in the range of 3438–3442 cm−1 that shows the intra-molecular hydrogen bonding between nanoclay and PMMA Mohanty and Nayak (2010). As the pure polymer and different composite samples mainly consist of PMMA, it is observed that there is no much difference among composites prepared with various compatibilizers (Fig. 2c–e). Mohanty and Nayak (2010) also reported similar type of result with PMMA-g-MA and Closite 30B clay.
The main diffraction peak for nanoclay, pure PMMA, PMMA-5-PE, PMMA-5-PP and PMMA-5-PS sample, is obtained at 2θ value of 4.15°, 13.34°, 2.74°, 2.54° and 2.70°, respectively. The d001 spacing is calculated from peak positions using Bragg’s law: λ = 2d sin θ, where λ is the X-ray wave length (1.5406 Å). The basal spacing of the d001 peak of organically modified nanoclay is estimated as 2.13 nm. In the nanocomposites, a large broad hump is originated from the PMMA matrix. The d-spacing (d001) value of PMMA-5-PE, PMMA-5-PP and PMMA-5-PS is found to be 3.22, 3.47 and 3.26 nm, respectively. This clearly reveals that nanoclay layers have been introduced in the nanocomposites as a single polymer chain enters between the silicate layers, and a tactoid morphology results with alternating polymeric and inorganic layers. The diverse d-spacing value obtained for the PMMA nanocomposite with different compatibilizer materials is probably due to the amount of polymer penetrated between the clay platelets and the interaction between a particular compatibilizer with PMMA matrix.
Transmission electron microscopy (TEM)
It is clear from Fig. 5 that PMMA nanocomposites demonstrate slightly lower tensile strength as compared to pure PMMA. It is known that PMMA is brittle in nature to some extent, and the addition of nanoclay particles provides further brittleness characteristics in the amorphous polymer, thus leading to a slight decrease in tensile strength. It is also observed that tactoid structure present in the polymer matrix (see Fig. 4) leads to lower tensile strength. The PMMA-5-PS nanocomposite shows the tensile strength of 55.5 MPa by the incorporation of PS-g-MA compatibilizer, which is higher than that of PMMA-5-PP and PMMA-5-PE samples. One of the main reasons is that both polystyrene and PMMA are amorphous in nature. Hence, there may be a possibility that PS makes good compatibility with PMMA resulting to enhanced tensile strength over other composites.
Figure 7 represents the Shore D hardness (ASTM D2240) of pure PMMA and its nanocomposites. The hardness of PMMA nanocomposites increases with incorporation of nanoclay and compatibilizer. The average value of the Shore D hardness is observed to be 58, 62, 70 and 78 for pure PMMA, PMMA-5-PE, PMMA-5-PP and PMMA-5-PS nanocomposites, respectively. All the nanocomposites exhibit better hardness over pure PMMA. The increase in the hardness is due to the presence of clay platelets in the polymer matrix. The clay platelets adequately restrict the indentation and thus enhance the hardness of the nanocomposites. It is noteworthy to mention that improvement of hardness for PMMA-5-PS sample is significant in comparison with PMMA-5-PP and PMMA-5-PE. PMMA-5-PS nanocomposite demonstrates a maximum improvement of Shore D hardness of 34 % over pure PMMA.
Differential scanning calorimetry (DSC)
Thermo gravimetric analysis (TGA)
PMMA nanocomposites with different compatibilizer have been successfully prepared by melt compounding technique.
It is found from the XRD analysis that PMMA-5-PS sample shows a d-spacing of 3.26 nm. The TEM image also demonstrates that PMMA-5-PS nanocomposite possesses partially exfoliated structure.
The tensile modulus of nanocomposites increases by the incorporation of compatibilizers, and it is found to be 16, 17 and 20 % higher over pure PMMA for PMMA-5-PP, PMMA-5-PE and PMMA-5-PS, respectively.
The hardness (Shore D) is also improved by 34 % for PMMA-5-PS as compared to pure PMMA.
TGA study reveals that the entire nanocomposites exhibit enhanced thermal stability when compared with pure PMMA.
Among all the materials, PMMA-5-PS nanocomposite display shows optimum mechanical properties.
We would like to thank the Central Instruments Facility, IIT Guwahati, for helping us to perform TEM analysis. XRD used in this work was financially supported by a FIST grant (SR/FST/ETII-028/2010) from the Department of Science and Technology (DST), Government of India.
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