Excellent Electromagnetic Interference Shielding and High Electrical

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Excellent Electromagnetic Interference Shielding and High Electrical conductivity of Compatibilized Polycarbonate/ Polypropylene Carbon Nanotube Blend Nanocomposites Mohammed Arif Poothanari, Jiji Abraham, Nandakumar Kalarikkal, and Sabu Thomas Ind. Eng. Chem. Res., Just Accepted Manuscript • DOI: 10.1021/acs.iecr.7b05406 • Publication Date (Web): 02 Mar 2018 Downloaded from http://pubs.acs.org on March 2, 2018

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Industrial & Engineering Chemistry Research 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

Excellent Electromagnetic Interference Shielding and High Electrical Conductivity of Compatibilized Polycarbonate/Polypropylene Carbon Nanotube Blend Nanocomposites Mohammed Arif Poothanari1, Jiji Abraham1, Nandakumar Kalarikkal 1,3, Sabu Thomas*1,2 1

International and Inter University Centre for Nanoscience and Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala-686560, India 2 School of Chemicals Sciences, Mahatma Gandhi University, Kottayam, Kerala-686560, India 3 School of Pure and Applied Physics, Mahatma Gandhi University, Kottayam, Kerala686560, India Corresponding Author: [email protected]

Abstract: Herein, we have fabricated a series of immiscible blend nanocomposites based on polycarbonate/polypropylene (PC/PP) by uniformly dispersing multiwall carbon nanotubes (MWCNT) via melt mixing technique. The effect of polypropylene-grafted maleic anhydride (PP-g-MA) as a compatibilizer has played a pivotal role in reducing the interfacial tension and thereby enhancing the attenuation performance of PC/PP blends. The substantial effect of compatibilization on the dispersion of MWCNTs has resulted in higher conductivity values of 0.33 Scm-1 which is a major requirement for designing EM shields. Nevertheless, both the uncompatibilized and compatibilized blend nanocomposites have shown viscoelastic phase separation process. The percolation networks of MWCNTs in compatibilized PC/PP blends were clearly observed using a High Resolution Transmission Electron Microscope (HRTEM). There was also a remarkable 5 fold decrease in the percolation threshold and 2.5 fold increase in total shielding effectiveness (54.78 dB) of compatibilized PC/PP blends when compared to immiscible PC/PP blends (22 dB).

Key words: Carbon nanotube, Compatibilization, Polymer blend, Electrical conductivity, EMI shielding

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1. Introduction Due to the rapid increase in the number of power sources and expanding the range of frequencies spectra used, the task of screening these fields is becoming increasingly difficult and challenging. This is due to the fact that the miniaturized electronic circuits are necessary for the various complex systems. An increased miniaturization of electronic circuits reduces resistance to electromagnetic exposure. Shielding is one of the tools of electromagnetic compatibility, which should enable smooth working of systems, electrical equipment and electronics with the electromagnetic environment1,2. Therefore, selection of appropriate materials for the screens and their geometry have absolute significance in shielding. In recent years, many efforts have been carried out by microwave engineers, scientists, and technologists to develop EMI shielding materials using conducting polymer composites as they are light weight, resistant to corrosion and have process flexibility. Conductive polymer composites are attractive materials for EMI shielding applications as they can eliminate the disadvantages of conventional metal-based EMI shields owing to their light weight, versatile nature, low cost, and good processability3,4. Carbon nanotube (CNT) based polymer nanocomposites constitutes one of the popular applications of CNTs, because of their excellent electrical, mechanical, and thermal properties5,6. CNT’s could enable the development of functional and structural composites by combining nanotubes into a different polymer matrices7. Blending of low-cost polymers with expensive polymers is an attractive and inexpensive method to prepare cost effective and novel structural materials. The blending of polyolefins with engineering plastics could improve the properties of polyolefins. The blending of PP with PC can provide a new blend system which could be used in many advanced applications. However, the PC/PP blends are immiscible and incompatible, therefore suitable compatibilization is required to decrease the interfacial tension to attain good interface adhesion, and to stabilize the morphology. There are different types of compatibilizer useful in blend systems. A well-known method for modifying polyolefins is to graft maleic anhydride onto polyolefins. Polypropylene grafted maleic anhydride (PP-g-MA) has been proved as a successful compatibilizer for blending of polypropylene (PP) with polymers, where the PP portion of the polypropylene grafted maleic anhydride (PP-g-MA) is miscible with PP, and the anhydride portion interacts with the polar component of other polymer8,9. Ploypetchara et al. prepared PP/PLA blend compatibilized with PP-g-MA fabricated by melt blending method10. Zhu et al. used PP-gMAH as a compatibilizer in the PET/PP blend system11. Krištofič et al. used PP-g-MAH as a compatibilizing agent in the polypropylene/polyamide blend12. Tol et al. compatibilized 2 ACS Paragon Plus Environment


co-continues PS/PA6 blend using the reactive styrene-maleic anhydride copolymer with 2 wt% maleic anhydride. They have investigated the effect of compatibilization on the phase inversion and the stability of the resulting co-continuous blend structures13. The high aspect ratio of the multiwalled carbon nanotube (MWCNT) favourable for high electrical conductivity in polymer nanocomposites at very low MWCNT loading. Many researchers have studied the MWCNT based polymer blend nanocomposites for EMI shielding applications14,15. Meinke et al. reported that MWCNTs selectively localized in the continuous PA6 phase in PA6/ABS blends and percolation threshold was lower than the PA6/MWCNT composites16. Goldel et al. found that MWCNTs selectively localized in the PC phase in PC/SAN co-continuous blend17. Bose et al. reported that the electromagnetic shielding effectiveness of PS/PMMA with surface-functionalized multiwall carbon nanotubes. They found that the shielding efficiency (SE) for blends with pristine and NH2MWNTs was >24 dB at room temperature18. Al-Saleh et al. had studied PP/PE with graphene nano-platelets and carbon nanotube blend nanocomposites. They found that CNT and GNP were selectively localized in the PE component. The conductivity and EMI shielding effectiveness (SE) were found to increase with MWCNT volume percentage due to the 1D geometry of the MWCNT which was more effective than the 2D geometry of the GNP in creating conductive networks19. Huang et al. studied the EMI shielding properties of PC/ABS/nickel-coated carbon fiber nanocomposite and they have achieved EMI shielding effectiveness of about 47 dB20. Su et al. reported that percolation threshold of MWCNTs filled PC/PVDF blends was much lower than those of MWCNTs-filled individual polymers. The CNTs were selectively localized in the PC phase, and a double percolation phenomenon is observed in this blend21. In another work, CNT-based nanocomposites of polypropylene (PP) and cyclic butylene terephthalate (CBT) were prepared by diluting the masterbatch, thereby achieved an improvement in electrical conductivity of PP/CBT blends through a double percolation22. The immiscible blend of polycarbonate/ polystyrene in 1:1 ratio was used to disperse the carbon nanotube (CNT) by solution processing technique. The CNT percentage determined the location of the CNT in the immiscible blend. When the CNT loading was only 0.05 wt%, the CNT was located in the PS Phase, whereas, at a higher loading of the CNT, at 5 wt%, a good level of dispersion of the nanotubes could be found in both the phases, ie in PC phase and PS Phase23. Biswas et al. fabricated a ternary polymer blend structure using PC, PVDF and PMMA with good electrical, and electromagnetic interference shielding properties24. The MWCNTs preferentially localised in the PVDF phase and PMMA acted as an interfacial modifier in PC/PVDF blends. They have achieved the 3 ACS Paragon Plus Environment

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shielding effectiveness of 37 dB at 18 GHz frequency. In another approach the multiwall carbon nanotubes are localised at the interface of PVDF/ABS blends by wrapping the nanotubes with PMMA25. The addition of 3 wt% PMMA wrapped MWCNT into the blend nanocomposites shows shielding effectiveness of 32 dB, which clearly indicates an efficient three dimensional network of MWCNTs at the interface. Li et al. developed co-continuous natural rubber/epoxidized natural rubber blends nanocomposites with carbon black by towroll mixing26. Increasing the epoxidation level of epoxidized natural rubber promotes the preferential location of CB and creates stronger dielectric loss, thus enhancing the microwave absorption properties. The good dispersion of the CNT leads to the formation of a percolate network in the PC/PS blend even at a lower loading of CNT of 0.05wt%. Wang et al. studied that the effect of MWCNTs on the morphology of PP-g-M compatibilized PA6/PP blends27. Mehrad et al. reported the impact properties of PP-g-MA compatibilized PP/EPDM/CNT and found the fine distribution of CNTs in the presence of PP-g-MA28. The dispersion of CNTs could be improved by incorporating polar group-containing polymers. The PP-g-MA is a polar copolymer which acts as a compatibilizer in the PC/PP blends. The main objective of this work is to develop high EMI shielding materials with excellent conductivity for communication devices and automotive applications. A systematic study has been performed on the effect of maleic anhydride-grafted polypropylene (PP-g-MA) as a compatibilizer on the electromagnetic shielding effectiveness and dispersion of the state of MWCNTs. To the best of our knowledge till now no studies have been reported in compatibilized PC/PP blend nanocomposite containing MWCNT to attenuate EM radiation. In addition, the study also aims to explore the effect of MWCNT loading on the viscoelastic phase separation, morphological changes and dielectric properties of compatibilized PC/PP blend nanocomposite. 2. Experimental 2.1 Materials Polycarbonate (PC) (Makrolon® 6557- melt flow index = 1.2 g/10 min) was purchased from Bayer Materials Science, Germany. The isotactic polypropylene (iPP) (H359 FG- melt flow index = 38 g/10 min)) was collected from Reliance, India Ltd, India. Polypropylene grafted with maleic anhydride (PP-g-MA) was supplied by Sigma-Aldrich. The multiwall carbon nanotube (MWCNT) (NC7000) was provided by Nanocyl, Belgium. The diameter of CNTs varies from 10 to 20 nm and the length is order of 1.5 µm and 90 % purity. Dichloromethane used in this study was of AR grade obtained from Merck Chemicals, India.



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2.2 Sample preparation All the blend nanocomposites were prepared by using Brabender 33-internal melt mixer with a cavity size of 55 cm3 and chamber temperature of 230 °C at 60 rpm for 10 minutes. Prior to mixing, PC was dried at 120 °C in oven for 12 hours to eliminate all moisture. The mixed sample is compression moulded at a temperature of 230 ºC for 2 minutes and is cooled to room temperature at the same pressure (100 kg /cm3). 2.3 Characterizations The cryogenically fractured surface of the blend nanocomposites was analysed using Scanning Electron Microscopy (SEM) (JEOL- ESEM) to assess the morphological properties. The cryocut specimens were prepared using an ultra-microtome (Leica, Ultracut UCT) to study the MWCNT dispersion and morphological details of nanocomposites by using Transmission Electron Micrsocsopy (TEM) (JEOL-2100 HRTEM). Solvent extraction study was used to evaluate the degree of the continuity of the polymer phase. Circular sample disk of samples (2mm thickness and 10mm diameter) were dipped in 200 ml of dichloromethane for 24 hours to dissolution of the PC phase. It was then kept in an oven at 80 °C and the weight of the disks after extraction was noted.

The degree of

continuity PC phase was evaluated based on its original weight and the change in weight during etching, by Equation 129–33. (1) Where øi is the degree of continuity of phase i, mi0 is the initial mass of phase i, and mif is the mass of phase i after extraction. Dielectric properties of the compression moulded samples of 10 mm diameter were measured in the frequency range (100 Hz to 2 MHz) using an Impedance Analyzer (Agilent E4980A). The electrical conductivity of prepared samples was measured with two different measurement setup. For the samples with electrical conductivity 5 wt%), a remarkable enhancement in the reflected power (R) and decrease in the absorbed and transmitted powers occur with increase of the sample conductivity. On the basis of equation 7 and 8, the R, A and T values can be calculated to be 0.7948, 0.2051 and 1.62 × 10−5 for PC/PP/MWCNT/PP-g-MA nanocomposites with 10 wt% of MWCNT, which illustrates that 79.48% of the input power was reflected back from the sample at Port1. Also, only 20.51% of the power was transferred into the sample and 1.62 × 10−3 % was ejected from the sample at Port 2. The 99.999% of transferred power into the sample was absorbed in the sample and only 0.001 % was transmitted to port 2. From this observation, it is evident that the nanocomposites also exhibit good absorption abilities. The permittivity parameters and electrical conductivity of nanocomposites increase with MWCNT loading favouring the impedance miss match phenomena which eventually enhance the reflection rather than absorption by the material. Therefore, at higher loading of MWCNTs most of the incident wave is reflected by conductive sample surface54,55.

4.

Conclusions

High-performance electromagnetic shielding PC/PP blend nanocomposite was developed via melt blending method. The addition of PP-g-MA into the PC/PP blend causes the refinement of the co-continuous morphology, decreased interfacial tension and suppression of coalescence. The co-continuous morphology of PC/PP/PP-g-MA has been unchanged by the inclusion of MWCNT. Both the uncompatibilized blends and compatibilized nanocomposites showed viscoelastic phase separation due to the dynamic asymmetry of the PC phase and PP phase. The compatibilization of PC/PP blend, increases interfacial area between PC and PP phases and reduces the interfacial tension, which lead to the formation of a percolation network of MWCNTs in both phases through the diffused interface.

Compatibilized

PC/PP/MWCNT nanocomposites displayed outstanding electrical, dielectric and EMI shielding properties due to the fine dispersion of MWCNTs in the blend system. The electrical percolation threshold of PC/PP/MWCNT/PP-g-MA is shown at 1 wt% loading of 22 ACS Paragon Plus Environment


MWCNT. Dielectric properties of compatibilized blends significantly improved due to the high number of polymer-nanotube interface and which contributes reasonably to the interfacial polarization. The shielding effectiveness 54.78 dB was attained for a 2 mm thick shield (at 3 GHz frequency) sample with 10 wt% of MWCNT for compatibilized PC/PP/MWCNT nanocomposite. All the experimental results in this work have proved an effective method to fabricate a lightweight and highly conductive composites for highperformance EMI shielding for mobile phone communication, electronic devices and automotive applications.

Supporting Information Degree of continuity of PC with respect to MWCNT loading in the PC/PP/PP-g-MA blend nanocomposites.

Acknowledgments This project is funded by Ministry of Electronics and Information Technology (MeitY), Govt .of India, New Delhi. The authors also would like to acknowledge the financial support from DST– Govt. of India through Nano Mission, PURSE and FIST schemes and UGC – Govt. of India through SAP DRS schemes

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