UNIVERSITI TEKNOLOGI MARA CHARACTERIZATION OF POLYPROPYLENE (PP)/TITANIUM DIOXIDE (TIO2) BLEND POLARITY EFFECT ON DIELECTRIC PROPERTIES MOHAMAD WISHAL KURNIA BIN AZMY Dissertation submitted in partial fulfillment of the requirements for the degree of Bachelor Engineering (Hons.) (Chemical Engineering) Faculty of Chemical Engineering August 2021 AUTHOR’S DECLARATION I declare that the work in this thesis was carried out in accordance with the regulations of Universiti Teknologi MARA. It is original and is the results of my own work, unless otherwise indicated or acknowledged as referenced work. This thesis has not be submitted to any other academic institution or non-academic institution for any degree of qualification. I, hereby, acknowledge that I have been supplied with the Academic Rules and Regulations for Post Graduate, Universiti Teknologi MARA, regulating the conduct of my study and research. Name of student : Mohamad Wishal Kurnia bin Azmy Student ID no. : 2018437792 Programme : Bachelor of Engineering (Hons.) Chemical – EH220 Faculty : Chemical Engineering Thesis Title : Characterization of Polypropylene(PP)/ Titanium Dioxide (TiO2) blend polarity effect on dielectric properties. Signature of student : Date : August 2021 I SUPERVISOR’S CERTIFICATION “I hereby declare that I have read this thesis and in my opinion this thesis is sufficient in terms of scope and quality for the award of Bachelor of Engineering (Hons.) Chemical” Signature :…………………………………. Name Dr. Rahida Wati binti Sharudin :………………………………… Date 10 August 2021 :…………………………………. II Universiti Teknologi Mara Faculty of Chemical Engineering MOHAMAD WISHAL KURNIA BIN AZMY STUDENT NAME: ................................................................................. 2018437792 STUDENT NUMBER: ................................................................................. 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Signed: ................................................ 10 AUGUST 2021 Date: ........................................... ABSTRACT Nanocomposites possess different characteristics that could potentially contribute to the technological development in various sector including dental applications, dielectric enhancement, capacitors, drug delivery and many more. In this research study, a nanocomposite is formed between polypropylene (PP) and titanium dioxide (TiO2). TiO2 acts as a filler for the polymer matrix and this addition could significantly improve several properties suitable for its dielectric application. A melt intercalation method is used for the mixing process involving several process units such as rotating twin-screw extruder, pelletizer, dryer and injection molding. The dispersion of nanofiller in the host polymer matrix is identify by using a scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and LCR meter. The microscopic analysis obtained for the nanocomposite shows high dispersion at below than 4 wt.%, which clearly shown by the less agglomeration produced. Similar results is obtained for thermal properties as nanocomposite with lower than 4 wt.% shows better thermal stability and higher onset as well as maximum degradation temperature. Despite lack of studies conducted in dielectric studies of polypropylene (PP)/ titanium dioxide (TiO2) nanocomposite, performance is best considered at 10 wt.% to 20 wt.%. For total, this review paper investigate the performance of PP/TiO2 nanocomposite at three distinct properties which is surface morphology, thermal properties and dielectric performances. III ACKNOWLEDGEMENT Throughout the writing of this thesis, I have received a great deal of support and assistance. First and foremost, I would like to thank Allah the almighty for His blessings and spiritual guidance along the duration of my final year research. In addition, I would like to thank my supervisor, Dr. Rahida Wati Sharudin and co-supervisor, Prof. Madya Dr. Rahmah whose knowledge and experience were crucial in developing the research questions and methods. Your insightful feedback pushed me to improve my thinking and raise the quality of my work. Last but not least, I dedicated my heartiest thanks to my parents and colleagues for their wise advice and a compassionate ear. IV LIST OF SYMBOLS 𝜀∗ Complex Dielectric Constant 𝜀 ,, Dielectric Loss Factor 𝜀, 𝜇𝑚 𝑑001 𝐷𝑚𝑎𝑥 Dielectric Constant Micrometer D-Spacing Dielectric Displacement when Electric Field 𝐸 Strength of Electric Field 𝐽 Density of energy storage kV 𝑛𝑚 Kilovolt Nanometer rpm Rotation per minute wt.% Weight percentage V LIST OF ABBREVIATIONS AFM Atomic Fore Microscopy BHF Barium Hexaferrite CTE Coefficients of Thermal Expansion CNT Carbon Nano Tubes EM Electromagnetic EMF/RFI EPDM EV Electromagnetic and Radio Frequency Interference Ethylene Propylene Diene Monomer Electric Vehicle EVA Ethylene Vinyl Acetate FSM Fluorinated Synthetic Mica HALS Hindered Amine Light Stabilizer HDPE High-Density Polyethylene LCR Inductance (L) Capacitance (C) Resistance (R) LDPE Low-Density Polyethylene MIM Metal-Insulator-Metal MMT Montmorillonite MWNT Multi-Walled Carbon Nanotubes OTFTs Organic Thin Film Transistor PA Polyamide-12 PANI Polyaniline PCL Polycaprolactone PEEK Polyetheretherketone PET Polyethylene Terephthalate PLA Polylactic Acid. PP/TiO2 PS Polypropylene/Titanium Dioxide Nanocomposite Polystyrene PVAc Polyvinyl Acetate-Carbon Nanotube PVC Polyvinyl Chloride PVDF Polyvinylidene Fluoride VI P(VDF-HFP) RH Poly(Vinylidene Difluoride-Co-Hexafluoropropylene) Rice Husk SEM Scanning Electron Microscopy TEM Transmission Electron Microscopy TA Thermogravimetric Analyzer TGA Thermogravimetric Analysis UV Ultraviolet VII LIST OF NOMENCLATURE BaTiO3 Barium Titanate (C3H6)n Polypropylene CuO Copper Oxide Y2O3 Yttrium Oxide MD Maximum Degradation Temperature OD Onset of Degradation Temperature VIII TABLE OF CONTENTS CHAPTER ONE: INTRODUCTION ............................................................................................. 1 1.1 Research Background ....................................................................................................... 1 1.2 Problem Statement ........................................................................................................... 3 1.3 Objectives ......................................................................................................................... 3 1.4 Scope of Research ............................................................................................................ 3 1.5 Limitations of Study ......................................................................................................... 4 1.6 Thesis Outline .................................................................................................................. 4 CHAPTER TWO: LITERATURE REVIEW ................................................................................. 6 2.1 Theoretical Study of Dielectric Parameter ....................................................................... 6 2.1.1 Dielectric constant .................................................................................................... 6 2.1.2 Dielectric loss............................................................................................................ 7 2.1.3 Breakdown strength .................................................................................................. 8 2.1.4 Electric resistivity ..................................................................................................... 8 2.2 Dielectric Nanocomposites .............................................................................................. 9 2.2.1 Ceramic nanocomposites .......................................................................................... 9 2.2.2 Polymeric nanocomposites ..................................................................................... 12 2.2.3 Nanoscale filler ....................................................................................................... 14 2.3 Structure and Morphologies ........................................................................................... 17 2.4 Polarity effect of nanocomposites .................................................................................. 19 2.5 Polypropylene (PP)/Titanium Dioxide (TiO2) Nanocomposite. .................................... 22 2.6 Additives for polymer composites ................................................................................. 24 2.6.1 Fillers ...................................................................................................................... 24 2.6.2 Combustion modifiers............................................................................................. 25 IX 2.6.3 Release agents ......................................................................................................... 25 2.6.4 Lubricants ............................................................................................................... 25 2.6.5 Anti-block additives ................................................................................................ 26 2.6.6 Catalysts .................................................................................................................. 26 2.6.7 UV stabilizers.......................................................................................................... 27 2.6.8 Optical brighteners .................................................................................................. 27 2.6.9 Plasticizers .............................................................................................................. 28 2.6.10 Coupling agents ...................................................................................................... 29 2.7 Nanocomposites and its potential ............................................................................... 29 CHAPTER THREE: METHODOLOGY ..................................................................................... 30 3.1 Materials Preparation ..................................................................................................... 30 3.1.1 In-situ intercalative polymerization ........................................................................ 30 3.1.2 Template synthesis (sol-gel technology) ................................................................ 31 3.1.3 Melt intercalation .................................................................................................... 31 3.2 Analysis .......................................................................................................................... 33 3.2.1 Microscopic analysis ............................................................................................... 33 3.2.2 Thermal measurement ............................................................................................. 35 3.2.3 Dielectric properties ................................................................................................ 37 CHAPTER FOUR: RESULTS AND DISCUSSION ................................................................... 38 4.1 Surface Morphology ....................................................................................................... 38 4.2 Thermal Analysis ........................................................................................................... 46 4.3 Dielectric Properties ....................................................................................................... 53 4.3.1 Dielectric loss.......................................................................................................... 53 4.3.2 Dielectric constant .................................................................................................. 55 4.3.3 Dielectric permittivity ............................................................................................. 56 X 4.3.4 Dielectric resistivity ................................................................................................ 57 4.3.5 Dielectric conductivity ................................................................................................. 57 4.3.6 Electrolyte uptake capability ........................................................................................ 58 CONCLUSION ............................................................................................................................. 59 REFERENCES ............................................................................................................................. 60 XI LIST OF TABLE Table 3.1: Comparison of nanocomposite synthesis..................................................................... 32 Table 4.1: Morphological structure of PP/TiO2 nanocomposite. .................................................. 38 Table 4.2: Summary of morphological structure of PP/TiO2. ...................................................... 40 Table 4.3: Morphological structure of reinforced PP/TiO2 nanocomposite ................................. 44 Table 4.4: Summary of morphological structure of PP/TiO2 nanocomposite. ............................. 45 Table 4.5: Thermogravimetric analysis (TGA) of PP/TiO2 nanocomposite................................. 46 Table 4.6: Summary of thermogravimetric analysis (TGA) of PP/TiO2 nanocomposite. ............ 48 XII LIST OF FIGURE Figure 1.1: Plastic world demand by resin types 2018. .................................................................. 2 Figure 1.2: Thesis outline on characterization of polypropylene (PP)/titanium dioxide (TiO2) blend polarity effect of dielectric properties. ............................................................................................ 5 Figure 2.1: PVDF-ceramic films enhanced route ......................................................................... 11 Figure 2.2: Published articles from 1920 to 2016 ......................................................................... 12 Figure 2.3: Nano fillers classification. .......................................................................................... 14 Figure 2.4: Examples of nanofillers .............................................................................................. 16 Figure 2.5: Nanocomposite morphologies (a) conventional nanocomposite, (b) intercalated nanocomposite; (c) exfoliated nanocomposite.............................................................................. 17 Figure 2.6: Ion change structure (a) when no electrical field (b) electrical field is applied. ........ 19 Figure 2.7: AFM images of EVA with 3% MWNTs . .................................................................. 21 Figure 2.8: Sol-gel processing for TiO2. ....................................................................................... 23 Figure 2.9: Properties of bis-benzoxazolyl-stilbene and bis-benzoxazolyl-thio-phene ................ 28 Figure 2.10: Tensile strength and elongation study on plasticizer effect ..................................... 28 Figure 3.1: General process flow .................................................................................................. 30 Figure 3.2: Sol-gel complete equation. ......................................................................................... 31 Figure 3.3: Injection molding machine ......................................................................................... 33 Figure 3.4: SEM microscope (Inkson, 2016). ............................................................................... 35 Figure 3.5: Thermogravimetric analyzer. ..................................................................................... 36 Figure 3.6: TGA thermogram (Awad & Khalaf, 2019). ............................................................... 37 Figure 4.1: SEM micrographs of neat PP (0 wt.% TiO2).............................................................. 41 Figure 4.2: SEM micrographs of PP/TiO2 (a) 0.5 wt.% (b) 1.5 wt.% .......................................... 42 Figure 4.3: SEM micrographs of PP/TiO2 at 4 wt.% .................................................................... 42 Figure 4.4 SEM micrographs of PP/TiO2 (a) 10 wt.% (b) 40 wt.% ............................................. 43 Figure 4.5: Graph on different OD values (oC) versus the TiO2 content (wt.%). ......................... 48 Figure 4.6: Graph on different MD values (oC) versus the TiO2 content (wt.%). ........................ 49 Figure 4.7: Thermogram of PP/TiO2 nanocomposite ................................................................... 50 Figure 4.8: Thermogram of PP/TiO2 nanocomposite ................................................................... 51 XIII Figure 4.9: Thermogram of PP/TiO2 nanocomposite (1) 0 wt.% TiO2 (2) 1 wt.% TiO2 (3) 5 wt.% TiO2. .............................................................................................................................................. 51 Figure 4.10: Frequency dependent dielectric loss tangent (a) 10 wt.% TiO2 (b) 20 wt.% TiO2 (c) 40 wt.% TiO2 (d) 50 wt.% TiO2. ................................................................................................... 53 Figure 4.11: Frequency dependent dielectric loss tangent (1) neat PP (2) 0.5 wt.% TiO2 (3) 1% TiO2 (4) 4 wt.% TiO2. ................................................................................................................... 54 Figure 4.12: Volume content dependent dielectric loss tangent ................................................... 54 Figure 4.13: Frequency dependent dielectric constant (a) 10 wt.% TiO2 (b) 20 wt.% TiO2 (c) 40 wt.% TiO2 (d) 50 wt.% TiO2......................................................................................................... 55 Figure 4.14: Volume content dependent dielectric permittivity at different TiO2 concentrations 56 Figure 4.15: Dielectric permittivity at different TiO2 concentrations........................................... 56 Figure 4.16: Volume content dependent electrical resistivity (a) 25oC, (b)50oC (c)75oC (d)100oC ....................................................................................................................................................... 57 Figure 4.17: Frequency dependent dielectric conductivity of nanocomposites (a) 10 wt.% TiO2 (b) 20 wt.% TiO2. ............................................................................................................................... 57 Figure 4.18: Volume content dependent electrolyte uptake capability......................................... 58 XIV 1. CHAPTER ONE: INTRODUCTION 1.1 Research Background Present modern contemporary world are seeking for better alternatives on petroleum- derived and other non-renewable resources. In an attempt to reduce the carbon footprint, automotive industry are taking alternatives to seek for better green technology approach whilst achieving the desired vehicle quality. Green technology can be defined as an improvement and utilization of products and systems to preserve the natural environment as well as present resources which simultaneously reduce the significant effect of current human activities (Iravani et al., 2017). Hence, an application of green concept is also conceptualize by implementing and promoting usage of electric vehicle (EV). Common market share of the industry is currently dominated by the world’s largest EV manufacturer, TESLA Inc. and their initial footsteps are now followed by another automotive supplier, namely Ford, Volkswagen, Honda and many more. Generally, electrical vehicle is a vehicle that runs on an electric motor, rather than combustion fuel which produce harmful carbon monoxide to the surrounding. This is to combat the rising issues of pollution and current global warming. Therefore, such initiatives receive huge interests on investors and consumers, ensuring the industry profitability in the long term. However, high demand of products also lead to high numbers of research and development efforts. Dielectric materials is an important insulation materials, located at the heart of EV. Issues relating to EV are often related with the degradation and ageing of the motorized unit. This occurrences are also affected by the bearings and insulation materials. Such poor performance are often affected by the thermal, electrical and mechanical factors. In an effort to produce a reliable, lighter and cheaper, research studies are conducted on the degradation mechanisms. A study by K. N. Gyftakis on the insulation materials under thermal also concluded that insulation samples possess varies values which has the tendency to give low capacitance and resistance. In total, it is clearly signify that dielectric measures is an important consideration for promising insulation prognosis in an electric vehicle (Gyftakis et al., 2016). 1 Incorporation of nanocomposite to the dielectric materials is because of its high capability to store energy and can be applied on electrical vehicle industry. Polymeric nanocomposite particularly can be applied to different energy storage devices such as lithium-ion batteries, supercapacitors and membrane fuel cell . These components plays a major role for producing a flexible and wearable electric energy storage devices as experimental analysis shows an improvement on electrical conductivity and stability . A driving factor for such performance are also influence by the dielectric constant and electric breakdown strength which identify the storage density mainly for capacitors applications (T. Zhang et al., 2021). Figure 1.1: Plastic world demand by resin types 2018 (Plastics Europe, 2019). Figure 1.1 shows heavy world consumption of plastics according to type of resin. Among all, polypropylene (PP) shows the highest application and often sought after by manufacturers in meeting the market needs, surpassing other type of commodities plastics such as polyvinyl chloride (PVC), polystyrene (PS) and polyethylene terephthalate (PET). Its good insulating properties with high arc resistance and dielectric strength ensures its vast applications for electrical sectors (C. Mike Chung, 2012). Therefore, this thesis will be focusing on the enhancement of PP with TiO2 as the nanoscale filler for the dielectric applications. 2 1.2 Problem Statement Polypropylene (PP) is one of the polymer that industrial sector often interested as it provide beneficiaries such as inexpensive and good chemical resistance to a broad variety of bases and acids. Although PP is very desirable, major drawbacks such as low melting temperature, low UV and thermal stability gives a negative impact to the material performance. Other than, polymer applications as dielectric also has reduce operating efficiency at low temperature operation. This contributes to its undesirable preferences on harsh conditions such as advanced microelectronics and aerospace power systems (Q. Li et al., 2016). Last but not least, there are very few research studies has been done on the dielectric perspective, particularly polarity aspects. This contributes to insufficient data as full enclosure on the matter could not be concluded. 1.3 Objectives This research study is conducted to achieve the outlined objectives below: 1. To conduct the dielectric study on polypropylene (PP)/titanium dioxide (TiO2) nanocomposite. 2. To analyze the dispersion and morphological structure contributing to the polarity performance. 3. To conduct a study on thermal properties of PP/TiO2 nanocomposite. 1.4 Scope of Research This thesis focused on reviewing the development of polypropylene (PP)/titanium dioxide (TiO2) nanocomposite with each synthesis method discussed for better dispersion objectives. The produced nanocomposite is analyzed on three different aspects which is surface morphology, thermal properties and dielectric analysis. In addition, other alternatives on polymer enhancement via different method are also discussed. This is for better understanding on current technological approach for achieving the best polymer traits. 3 1.5 Limitations of Study In order to achieve the desired polypropylene (PP)/ titanium dioxide (TiO2) nanocomposite dispersion, interaction between the host polymer and the nanoscale filler need to interact with each other, forming the highest dispersion. High dispersion which was later experimented by Scanning Electron Microscopy (SEM) proves that the morphological structure of the formed nanocomposite plays a vital role in producing better thermal and dielectric properties. To achieve the objective, in-situ intercalative polymerization is the best option. However, the method are not recommended because of the availability of monomer, leaving researchers choices on melt intercalation method. Other than that, microscopic analysis is used in this study to identify the surface morphology of the formed nanocomposite. However, using SEM as the preferred choice is expensive and commonly situated at large organization. Following that, dielectric studies of PP/TiO2 nanocomposite are still not extensively discussed by researchers as initial studies are often focused on the thermal and mechanical properties only. 1.6 Thesis Outline Chapter one focuses on the introductory of nanocomposite and its application in dielectric and energy storage industries. Three objectives are highlighted for this thesis with significant limitation affecting the study. Chapter two reveals the variety of dielectric nanocomposites which are commonly found in recent investigations, which is ceramic and polymeric nanocomposites. After that, the morphological structure and polarity effect of nanocomposite is further discussed. Detail insight of polypropylene (PP)/titanium dioxide (TiO2) is highlighted further in the chapter with other recommendations aside from fillers used to improve the polymer properties. Chapter 3 further analyzes different alternative to produce nanocomposite at certain dispersion quality. Equipment used for thermal, dielectric and surface morphology is outlined. Chapter 4 analyzes the results obtained from several researchers on the three aspect with complete justification on different behavior of polymer before conclusion is being made. 4 Figure 1.2: Thesis outline on characterization of polypropylene (PP)/titanium dioxide (TiO2) blend polarity effect of dielectric properties. 5 2. CHAPTER TWO: LITERATURE REVIEW 2.1 Theoretical Study of Dielectric Parameter Understanding on the dielectric properties are primarily important and significant in creating a general overview of dielectric loss, dielectric polarization as well as charge behavior occurring simultaneously within the composite. Presented hereby are few of the parameters required for our studies which are dielectric constant, dielectric loss, breakdown strength and electrical resistivity. 2.1.1 Dielectric constant Dielectric constant or relative permittivity can be defined as the study of electric potential energy, that is well stored in a material. It is measured in the form of induced polarization, influenced by the circulating external field. The polarization occurs due to several factors which is electronic, atomic, dipolar, space charge and ionic (Dorey, 2012). This factors will influence the high relative permittivity properties of a material as the highest portrays active factors occurring subjected to an electrical field. Commonly, it is prescribed as ratio between the dielectric permittivity towards vacuum or dry air properties (Wood et al., 2001). In insulation application, the dielectric constant should be kept low as prevention of electrical transfer could be minimized. High dielectric constant is desired in capacitor application. In other application, high dielectric value is also used for film as a dielectric in a capacitor. This is to minimize the capacitor dimension, storing the energy value at high volume (McKeen, 2012b). Based on a study conducted by BingYue Tsui et. al., the insulators is stacked with a dielectric of Yttrium oxide (Y2O3) to improve the thermal performance of the dielectric of metal-insulator-metal (MIM) capacitor. It is concluded that the dielectric constant of material does affect the capacitance density, since the parameters combined with low leakage current requirement makes up a promising MIM capacitors (With et al., 2010). Other than that, it can also be observed that dielectric constant pose significant effect towards the dielectric strength in the solid insulation application (Liu et al., 2019). The influence are done by two methods, which is cavity discharge and molecular polarization in an indirect way. 6 The said factor could influence the breakdown strength, increasing its application in integrated circuit applications. By using dielectric constant as the prime manipulated factor, dielectric studies are highly interested in its influence on ionic transport as prescribed on a research study by Bill K. Wheatle. Although some researches believed that ionic conductivity remains unexplored and unknown (Barteau et al., 2013), others believed that the contributing factors towards ionic conductivities properties is because of the host polymer polarity (Wheatle et al., 2017). A polymer host with a low dielectric constant will not cause the ionic aggregates, leaving them with low ion diffusion. The article stresses that polymer dielectric constant does influences the overall ionic conductivity although the mobility of ion is dependent towards the host polarity. 2.1.2 Dielectric loss Dielectric loss is the study of electrical energy lost via conduction after the energy field is used (Dorey, 2012). Its significance can be used and enhance to calculate the complex dielectric constant for dielectric spectroscopy studies. The values were calculated by using the following equations: 𝜀 ∗ = 𝜀 ′ − 𝑖𝜀 ′′ Where 𝜀 ′ is the dielectric constant and 𝜀 ′′ is the dielectric loss factor (C. Zhang & Stevens, 2008). With increasing temperature, the dielectric loss significantly increases as well. However, if exposed at low frequencies, the value drops due to migration of ion within the material (Bouaamlat et al., 2020). E.M. Gojayev et. al. research focusing on dielectric properties for LDPE modified, by adding biological fillers (fish bone). By using an immittance meter, he able to conclude that the dielectric performance of the material is increase, from both dielectric permeability and dielectric loss results. This is because the dielectric and electric conductivity are highly dependent towards filler volume and frequency value. Adjusting both parameters influences the particles proportion, thus reaching desired properties of enhanced LDPE (Gojayev et al., 2019). Other than that, materials with excellent dielectric loss properties are heavily applied in fabrication as well as antenna designs (Freitas et al., 2020). This includes bismuth niobate, niobium pentoxide, zirconia nitrate, magnesium silicate as well as titanium dioxide. 7 2.1.3 Breakdown strength Electrical breakdown strength is the measure of electrical field limit before an electron conduction occur in the insulator (Dorey, 2012). Significantly, it identifies the maximum limit for the operation as approaching them could result in higher tendency for efficiency reduction. In a study conducted by R.Keefe and W.Zenger, breakdown strength is a prime measurement to conclude the role of interface between two distinct polymers, nanoparticle-filled polymers and micron-filled polymers. According to several researchers, nanocomposites will have greater interfacial area as compared to microcomposites. This is proven from the particle surface affecting the properties, influencing the volume fraction of polymer (Ash et al., 2004). Eventually, it will affect the properties of the dielectrics, mainly breakdown strength properties. In addition to the studies, the breakdown of polymeric dielectrics are influenced by several factors. This include accumulation of bulk charge, type of bonding, free volume, temperature, degree of crystallinity as well as interfacial area (M. Roy et al., 2005). Other studies also highlighted the potential of a quasiconductive region. Quasi-conductive region is partial overlapping between an interaction zone with the nanocomposites (Ash et al., 2004). Studies concluded that this regions allows charge dissipation to occur, hence, improving the overall dielectric breakdown strength of the material. In addition, it could also be influenced by two possible factors; scattering mechanism and space charge distribution (Holmes, 1986). In total, breakdown strength is an important practical dielectric properties in identifying the maximum capability of material before allowing current to flow. 2.1.4 Electric resistivity Electric resistivity can be studied using two distinct research area which is surface resistivity and volume resistivity. Surface resistivity, by definition is the resistance measure on leakage current on insulating material’s surface (Anshuman Shrivastava, 2018a). Insulation is the common application towards surface resistivity. An example of its application is the usage of plastic films which is used for isolation for an electric system. Therefore, its surface resistivity have to be kept high for the integration of materials. Other applications include conductors, sensor as well as packaging purpose. Based on a study by Robert Spragg et. al., the surface resistivity conducted can be influenced by two factors. Those are temperature parameter and sample storage and conditioning. 8 Temperature parameter are closely related towards ionic mobility, which then follows the Arrhenius relationship. Keeping the specimens at different solutions portrays distinct inconsistent outcome. During physical analysis, measures should be taken as it relates to dilution on pore solution, affecting the frequency spectra (Spragg et al., 2013). Volume resistivity, on the other hand, is the resistance measure on leakage current in the insulating material’s body (Anshuman Shrivastava, 2018a). It is commonly applied in a conductive plastic composite which dispersion in a conductive filler is the major desire. Other applications includes EMI/RFI shielding effectiveness which are applicable towards conductive fillers. There are various factors influencing the volume resistivity. While others are influenced by electric field strength (Sirviö et al., 2008), nanocomposites are primarily influenced by particles charge distribution. A study was conducted by S. Ju on the low-density polyethylene composites, analyzing the surface chemistry as well as deep traps produced by the nanoparticles. According to their analysis, the volume resistivity of nanocomposites able to be improved with an addition of the silica filler (Ju et al., 2014). This is mainly a good indication of the carrier mobility occurring in the composites, allowing charges to accumulate on the surface of the sample. 2.2 Dielectric Nanocomposites 2.2.1 Ceramic nanocomposites By definition, ceramic-based nanocomposites is a ceramic composites which consists of multiple solid phases, which at least one of them are in the nanoscale volume (less than 100nm) (Kerkeni et al., 2016). Ceramic materials are initially used as a conventional electrostatic capacitors. Barium titanate (BaTiO3) are one of the widely used ceramics in capacitance and ferroelectric applications. A research study conducted by Long Wu stresses that the dielectric properties of BaTiO3 are highly dependent on its microstructure. The higher the size reduction, the better the relative permittivity performance (Wu et al., 2009). It is later then concluded that the size of the material also influences the ferroelectric phase transition temperature. Although BaTiO3 is well known for its high dielectric breakdown resistance, using the material alone poses several disadvantage towards the system. It is observed that usage of BaTiO3 alone causes high leakage and brittleness when applied with thermal stress (Kurzweil, 2009). 9 Introduction of another nano-scale solid phase attracts researchers on its vast potential especially in terms of dielectric capabilities. It is commonly mixed with another polymer to create positive energy storage properties. Sunil Kumar et. al. had conducted a practical research on polymer-ceramic nanocomposite by using polyvinylidene fluoride (PVDF) and barium hexaferrite (BHF). Based on the results obtained, the dielectric constant had improved for 18 times than the normal PVDF value at 1KHz (S. Kumar et al., 2018). The incorporation of BHF influences the 𝛽 crystalline phase, allowing PVDF to convert electrical energy into mechanical energy when electrical field is applied. Other than that, electrostatics and interfacial interaction also causes the dielectric constant to increase. However, addition of BHF has its own limitation when the 𝛽 phase signifies decreasing trend on the next trial after addition of (0.7) PVDF-(0.3) BHF nanocomposite. Other than that, a study also has been conducted to identify the nanoparticle distribution for polymer-ceramic nanocomposites. The analysis conducted by Ziming Cai et. al. focused on the application towards pulsed power system. The system heavily relies on the charging-discharging capability as well as power density. The relationship between breakdown voltage and dielectric permittivity is as shown below: 𝐽=∫ 𝐷𝑚𝑎𝑥 0 𝐸𝑑𝐷 Where 𝐽 is the density of energy storage, 𝐷𝑚𝑎𝑥 is the dielectric displacement when electric field strength is applied, 𝐸 is the strength of electric field and 𝐷 is the dielectric displacement. Due to insufficient practical lab analysis conducted on quantified description, simulation by using a Clark-Evans test is performed (Cai et al., 2017). Based on the quantified method developed, the higher quantified criterion, 𝑧𝑚 , the nanocomposite produced becomes harder to breakdown. As a result, the nominal breakdown strength doubled as the ceramic particles become larger. In general, ceramic-based nanocomposite has wide applications mainly in electrical or dielectric application. Study conducted by Shiva Adireddy et. al. focused on applying polymer-ceramic nanocomposites in high energy density applications. Even though dielectric permittivity requirement had been achieved by conventional methods, introducing fillers to the host could improve the low performance of breakdown strength (Adireddy et al., 2015). 10 Figure 2.1 shows the enhanced route proposed by the author to obtain the films at desired 30µm thickness. As a result, both dielectric loss and breakdown strength significantly improved as well as keeping the relative permittivity at a high level. In total, analysis and results obtained proved that the said composite produced by solvothermal method able to utilize in capacitive energy storage applications. Sonification for 10 minutes. Stir by using a magnetic stirrer at 120oC for 1 hour. The solution is drop casted onto a glass plate before annealed. Film is quenched in ice-water bath, peeled and deposited onto the surface. Figure 2.1: PVDF-ceramic films enhanced route (Adireddy et al., 2015) Another interesting field of study is conducted by Mohamad Sobirin et. al., which uses strontium and ferrite to produce a dielectric capacitor. Ferrite ability to store charge is the prime factor of its selection to be used with a ceramic composites. However, the application of ferrite has its own limitation that it requires doping elements, namely strontium. Based on analysis on the surface structure with a Scanning Electron Microscopy (SEM), the particle size volume reduces as mass of strontium ferrite increases. Such phenomenon will cause ceramic solid to be stronger in the weight-bearing. However, the best capacitance performance is observed when 5 grams of strontium ferrite is used, and as the addition of materials continued, the compressive strength also increased (Faizal et al., 2016). With different applications of ceramic nanocomposite, it is definitely favors for its high mechanical (Hapuhinna et al., 2020) and electrical properties (Yoon et al., 2009), high electrical resistivity and better thermal stability (Khattak et al., 2018) . 11 2.2.2 Polymeric nanocomposites Attention on polymeric nanocomposites has been highlighted in recent years due to its wide ability in improving dielectric properties of materials. Ability to manipulate the chemical and physical properties attracts researchers to enhance new and better innovations on the area (Broitman, 2018). Polymer nanocomposite, by definition is polymers that has been reinforced with nanomaterials (Tofighy & Mohammadi, 2020). Although nanocomposite possess promising properties, the complex interfacial areas are one of the most challenging aspect due to its small scale specific area which influence the interaction between both polymer and nanoparticles (Kerkeni et al., 2016). This in turns inhibit uniform dispersion between them, making it hard to be synthesized and analyzed. Figure 2.2: Published articles from 1920 to 2016 (Broitman, 2018). Polymer/ceramic nanocomposite is one of the research area that are studied mainly on its potential towards energy storage performance. The performance of film capacitors directly related towards the energy density, allowing them to sustain the electrical volume whilst converting the direct current into alternating current (Fan et al., 2019). In a study conducted by Xin Yang on P(VDF-HFP) polymer matrix and BaTiO3 ceramic fillers, the homogenous dispersion of the nanocomposite is promoted by the hot-press during non-equilibrium processing. This is highly important to the analysis as morphology and structure are the factor to manipulate the nanoparticles distribution (X. Yang et al., 2020). Due to the interfacial area from the multilayer arrangement of nanocomposite, the breakdown strength, permittivity and energy density also increases. 12 Besides that, several studies also has been done by various researchers on potential of organic/inorganic polymer nanocomposite, which secondary components are embedded in an organic substrate. Polymer/aluminum is an extensive of the area which focusing on decoupling capacitor applications. In comparison between singularity of passive components and embedded capacitor, electrical performance are superior in embedded capacitor, apart from reduction in size and costs (Goosey, 2004). This is proven from an analysis by Jianwen Xu et. al. on using core metallic aluminum and nano aluminum oxide. The great particle distribution of coupling agent later improves the dielectric constant of the composite (Xu & Wong, 2007). Apart from application in wastewater industries (Dhillon & Kumar, 2018), its uses widen Organic Thin Film Transistor (OTFTs) application as hybrid of organic and inorganic material have the desired physical trait (Yu et al., 2016). In present world’s alternatives towards green technology, polymeric nanocomposite also has been enhanced to provide alternative pathways in enriching usage of renewable raw materials, bio-sourced polymers (Mistretta et al., 2021). This could reduce industrial dependent on petroleum-based materials such as propylene and polyethylene since they are non-biodegradable and unsustainable. Based on a research study by V Kumar et. al., biopolymers such as polylactic acid (PLA) and polyhydroxyalkanoate portrays promising feedbacks. Addition on nanofillers on the biopolymers resulting to an increase in mechanical interlocking in the rough surface, improving the bionanocomposite’s impact strength (V. Kumar et al., 2013). Present modification also has been brought upon introducing lignin to produce a biodegradable insulator (Oliviero et al., 2017), conserving environmental profile. Consideration on green technology spikes during these past few years, driving the sustainable development and investment on a foundation filled with ecological advantages (M. Guo et al., 2020). It can be used towards energy storage application which able to replace present oil-consuming vehicles. In line with the aim of greener technology and practices, implementing nanocomposite on energy storage applications could introduce energy and cost-efficient films for hybrid electric cars and solar cells. The invention on films between electrolyte and electrodes proves the high capacity with promising cycle efficiency (Sadiq et al., 2017) as well as relative permittivity (Ramesh et al., 2003). Distinct behavior pattern on all levels of frequency are usually associated with electrode polarizations. 13 2.2.3 Nanoscale filler Dispersing nanoscale filler into the host material can alter the properties and structure, giving nanodielectric research a new novel approach for electrical insulation application. The dimensions of nanoscale fillers are one-dimensional (1D) nanofillers, two-dimensional (2D) nanofillers and three-dimensional (3D) nanofillers. By definition, one-dimensional nanofillers are fillers with a 1-100nm particle sizes (Bishop, 2011). Most of 1D nanofillers are dependent on its unique shape structure, making them desirable in nanodevices component formation. Applications of 1D nanomaterials ranges from microelectronics until biomedical products. Their electrical and optic properties influences the desire to utilize them as an aid towards composite that require significant boost on their performance. Arrangement of the nanofillers dimensions are shown below: Figure 2.3: Nano fillers classification (Akpan et al., 2018). G.-M. Kim et. al. utilizes layered silicate, a primary example of 1D nanofillers with a polyamide-12 (PA-12) composite. Usage of organic and inorganic hybrid materials are favorable due to its substantial reinforcement efficiency compared to other composites. Although thickness of the composite are not affected by the introduction of the fillers, the morphology of layered silicates occurring in PA-12 had a drastic change (G. M. Kim et al., 2001). Apart from that, the nanocomposite able to achieve an ultimate macroscopic trait by using an electron microscope, signifying the improvement of toughness and stiffness characteristics. Polymer/layered silicate nanocomposite also have the ability of other unique properties, namely thermal stability , flammability reduction (Gilman, 1999) and improvement on gas barrier properties (Nanocomposites, 2001). 14 For two-dimensional (2D) filler, on the other hand, is a nanofiller which consists of two dimensions less than 100nm. As shown in Figure 2.3, tubes, filaments or fiber are one of the common shape or representation of the nanofiller. Its common application includes cellulose fiber (Paul et al., 2010), molybdenum sulfide (D. Cheng et al., 2019), cerium oxide (Mohanapriya et al., 2016) and copper oxide (Ambalagi et al., 2018). In comparison with 1D and 3D nanofillers, 2D nanofillers possess better flame-retardant traits. A study conducted by Saisy K. Esthappan et. al. further proves by using zinc oxide nanofillers (2D) on PP composites. Addition of zinc oxide to the composite significantly improves in terms of thermal stability and mechanical properties as compared to neat PP composite (Saisy K. Esthappan et al., 2015). It is believed that the strong interaction and morphologies between them increases the degradation temperature limit. In total, thermal motion of the nanocomposite gives the desired properties. Silver are one of the other choices to produce a nanocomposite with improved properties. Silver nanomaterials are synthesized by various approaches: physical, chemical, photochemical and biological (Karak, 2018b). A study conducted by Lisa Riviere et. al. uses silver fillers with polyetheretherketone (PEEK) to produce a homogenous nanocomposite mixture. At a microscopic level, the nanocomposite’s performance on thermal diffusivity and conductivity increased significantly. However, application on a macroscopic level produces a decrease trend for every increment of silver content (Rivière et al., 2016). For dielectric properties, silver nanofillers gives the same improvement on electrical conductivity because of increase in both wire intersections and percolation probability (Fang & Lafdi, 2021). Apart from that, silica are also used as nanofiller for nanocomposite in different fields such as coatings, chemo sensors and pervaporation membrane. Layered silica nanocomposites behaves differently when applied with a host polymer matrix . Type of silica (hydrophobic and nonhydrophobic) will determines the water vapor permeabilities and are further detected by a water vapor adsorption measurement. Although mechanical properties such as stiffness and elastic modulus is increased, addition of silica poses no significant changes on the thermal stability (Gómez et al., 2016). It is also observed that its effect on degradation temperature for some materials (LDPE) only can be foreseen when high quantity of silica is used in the blending method (Olmos et al., 2015). Regardless, dielectric properties of modified particles still increases in comparison to pure composite materials (Shin et al., 2008). 15 Figure 2.4: Examples of nanofillers (Akpan et al., 2018). Nanofillers in three dimensional (3D) are relatively different as compared to other two configurations. It is signified as having three equiaxed particles in nanometer scale. Common shapes of 3D are spherical and cubical shapes as shown in the Figure 2.3. Other names for 3D nanofillers includes nanoparticles, nanosphere, zero dimensional nanoparticles, nanogranules or isodimensional. 3D nanofillers are a vital factor in polymer nanocomposites as improvement on the properties can be further enhanced. This includes good mechanical properties (W. D. Kim et al., 2012), low cost and resistance to ultraviolet (UV) (Baishya et al., 2019). 16 2.3 Structure and Morphologies Composite materials consists of two or more materials combined together by a variety of means. Due to their physically different feature, microscopy usage allows them to be easily identifies. Apart from that, distribution in a controlled manner allows them to attain better quality and properties as compared to singular components. By accurate definition, composite materials are made up of two or more components complimenting each other, producing a material that outperforms its individual properties. Polymers are extensively used mainly as composite materials due to its processing ability at low temperature and usage of classical methods to achieve the definite goals. Similarly, nanocomposite is a composite materials with at least one dimension of nanometers and its made to improve the properties, performance and quality. Polymer-clay nanocomposites are one of the most prominent research as it is largely commercialized to automotive industry, contributing to its vast research conducted. Figure 2.5: Nanocomposite morphologies (a) conventional nanocomposite, (b) intercalated nanocomposite; (c) exfoliated nanocomposite (Chen et al., 2008). As shown in Figure 2.5, there are three types of composite morphologies which is conventional composites, intercalated nanocomposites and exfoliated nanocomposites. For every composite produced, the basal plane spacing or d-spacing, d001 can be used to significantly describe the current morphological structure. By definition, basal plane spacing is the distance measure from the plane to the corresponding plane in the other layer. For conventional composites (or often called immiscible) the polymers are unable to enter the galleries of layers and the basal plane spacing remains unchanged. This also describes that the structure are identical with traditional microcomposites. 17 For an intercalated nanocomposites, the d001 is increased, signifying larger inter layer spacing (Leporatti, 2019). However, the self-assembled, multilayered structures remain stacked, providing only a limited extent (Thomas, 2016). Another study conducted by Bruna Louise Silva et. al. focusing on exfoliated nanocomposites between clay and high-density polyethylene (HDPE) nanocomposites using two different method; solution and melting mixing. Although solution intercalation possess lower degree of crystallinity, the components are homogeneously dispersed and have an excellent thermal stability (B. L. Silva et al., 2014). Another study conducted by InNan Jan et. al states that since its discovery by the Toyota research group, the uniformity of silicate when dispersed in host polymer is still unraveled. Difference in morphologies of silicate shows the effectiveness on distribution, leading towards better performance of exfoliated on hardness perspective (Jan et al., 2005). Exfoliated or miscible nanocomposites portrays potential because of its structural arrangement and improvements for the nanocomposite properties. Exfoliated morphologies gives a large d001 (typically 10nm apart), signifying a disordered array and totally pushed away from the unit layer and the plane, resulted from delamination (Leporatti, 2019). A study has been conducted by Alexander B. Morgan et. al. on preparing an exfoliated polystyrene/clay nanocomposites by using a sonication. Based on readings collected from the X-ray diffractometer, montmorillonite (MMT) gives better results as compared to fluorinated synthetic mica (FSM). This shows that both clay type and mixing energy have the ability to determines the clay exfoliation properties upon utilizing solvent blending as the fixed method (Morgan & Harris, 2004). An extensive part of exfoliated nanocomposite which d001>10nm includes another three different types of nanoscale morphologies which is ordered, disordered and partial exfoliation. These arrangements cannot be identified by a typical X-ray diffractometer, hence regards as an exfoliated nanocomposites. Ordered exfoliation describes the homogenous morphology which nano-layers are maintained and layers are individually scattered through the entire polymer matrix. Care should be taken as exfoliated materials able to lose the order when melt processing method is applied (Morgan & Gilman, 2002). As opposed to disorder exfoliation concept, disorder exfoliation shows an entirely scattered arrangement with nano-layers dispersing through the system. An intermediate morphology can also be obtained from the partial exfoliation which portrays dispersed exfoliated layers with small-intercalated layers. 18 2.4 Polarity effect of nanocomposites Influence of nanodielectrics excellent thermal and mechanical properties correlates with polarity interaction between the host polymer matrix and the nanoscale dispersed fillers (C. Zhang & Stevens, 2008). By definition, matrix polarity can be signify as the polymer/filler interfacial interactions and exfoliation degree (Parameswaranpillai, 2017). Polarity is vital for nanocomposites both structural properties which is strength and elongation. Many researches article proves that the polarity eventually affects the interaction zones between the polymer matrix and the nanoparticle (S. Li et al., 2011). Hence, there are four distinct major classification of polarization in dielectric application which is electronic polarization, ionic polarization, dipolar polarization and interfacial polarization. These categories of polarization are separated according to the resonance and relaxation regimes. Figure 2.6: Ion change structure (a) when no electrical field (b) electrical field is applied (Fan et al., 2019). Application of atom as an external electric field, an induced dipole moment is produced (Lopes et al., 2009). This causes electrons to become lighter than the positive nucleus, making them easily displaced by the field. Electronic polarization focuses on the dipole moment generated when the negative charge separation from the positive nucleus is taking place (Fan et al., 2019). The source of electronic polarization charge configuration comes from the valence electrons (Castet et al., 2008). Both electronic and ionic polarization highly dependent on the polymers band gaps (Lu & Meng, 2015). As a result, both have no dielectric loss measures because of its occurrences in radio and power frequency ranges. Generally, ionic polarization as shown in Figure 2.6 can be studied only on ionic crystals (D. Kumar et al., 2020). When an electrical field is applied, the negative ions went into the -x direction whereas positive ions moves into the +x direction. 19 Dipolar polarization, on the other hand, occasionally occurs in both polar liquids and polar gases (Kao, 2004). With electrical field becomes absent, thermal agitations caused the molecules to be randomly oriented. As electrical field is introduced, material will caused a net polarization as a result from alignment and arrangement of dipoles standing parallel towards the electrical field direction (Fan et al., 2019). Dipolar polarization occurs in the polymer relies on the polar groups and polymer chain geometry. Non-polar polymers have low dielectric permittivity resulting from dipole moments cancelling each other (H. M. Ahmed & Aziz, 2008) . In addition, the dielectric constant also significantly reduced because of thermal agitation affecting the dipole. Study conducted by Tamara P. Stepanova et. al. on the polar polymers stated that they have higher dielectric permittivity due to its permanent dipoles moment and low molecular interaction (Stepanova et al., 2015). On the other hand, Maxwell-Wagner-Sillars polarization or commonly called as interfacial polarization happens from the accumulation of positive and negative space charges at the interface (Kao, 2004). As a result, dipole moments produce dipole moments, appearing in the polarization vector. Based on a study by Zhanhui Peng et. al., Maxwell-Wagner polarization is the prime factor on the promotion of internal barrier layer capacitor effect. Once interface polarization is improved, a giant boosts on the dielectric permittivity is expected (Peng et al., 2020). Interfacial polarization in real polymer-based materials are affected by several factors, such as film-electrode partial contact, impurities presence (Iannarelli et al., 2020), crystal-amorphous interfaces (A. B. Silva et al., 2011) and homogeneous dispersion (Putson et al., 2013). This causes unknown amount of time for them to discharge, making them only utilized at low frequency range. Since nanocomposites consists of blended between two different components, the polarity effect causes significant changes on the end properties. One of the changes is the morphology and mechanical properties of nanocomposites. A study has been conducted by Sophie Peeterbroeck et. al. on the effect of ethylene vinyl acetate copolymers (EVA) matrix polarity after forming a nanocomposite with a purified multi-walled carbon nanotubes (MWNTs). In order to achieve a homogeneous dispersion of fillers in the polymer matrix, melt blending or melt mixing method is the preferable way to prevent the agglomeration (Song & Youn, 2005). From atomic force microscopy (AFM) observation in Figure 2.7, vinyl acetate content only gives small adjustment to 20 the overall polarity of EVA-carbon nanotubes nanocomposites, favoring filler dispersion when using polyvinyl acetate-carbon nanotube nanocomposites (PVAc) (Peeterbroeck et al., 2007). Figure 2.7: AFM images of EVA with 3% MWNTs (Peeterbroeck et al., 2007). Rheology of the nanocomposite is a very important indicator to produce defect-free products as inclusion of nanofillers in them causes significant changes on the viscoelastic properties (S. K. Singh et al., 2018). This was later proven from a study by Vishwa Pratap Singh et. al. on the compatibilizer polarity of polyethylene/sepiolite clay nanocomposites, consequently affecting the rheological behavior. Although molecular weight is the major influence, sepiolite fibers do incorporates better with a polymer matrix containing more polarity (V. P. Singh et al., 2017). Similar claim also been highlighted by Marek Weltrowski et. al. on polarity parameters as a prediction for the nanofillers dispersion in the nanocomposite. Compatibilizer polarity further influenced by three other polarity parameters from the polar groups which are the acid value, mole fraction and weight fraction (Weltrowski & Dolez, 2019). Apart from that, ion transport occurred within the system are also heavily influenced by the polymer polarity. Replacing small molecule electrolytes with a polymer-based hosts requires extensive balance on the host polymer polarity as incorporation of high and low dipole moments will be affecting the ionic aggregation and transportation of ion (Wheatle et al., 2018). Utilization of nanoscale fillers into the electrolytes was studied by Santosh Mogurampelly et. al.. Diffusivity of ion in the polymer were affected by two major factors which is temperature and presence of interfacial layer. The interfacial area further influences the ion-nanoparticle interactions. As a result, conductivity of ion decreased when a low temperature is applied and both residence time and relaxation time increases following the addition of nanoparticles (Mogurampelly & Ganesan, 2015). 21 2.5 Polypropylene (PP)/Titanium Dioxide (TiO2) Nanocomposite. An inclining interest to promote better dielectric material has influence the ongoing polymer development on nanocomposite using a PP. PP is a linear and saturated hydrocarbon polymer with a chemical structure of (C3H6)n. Year 1954 marks the discovery of PP by an Italian chemist named Giulio Natta and his assistant, Paulo Chini (Sivaram, 2017). Since then, the manufacturing process of PP has escalated in the world market that 30 million tons was developed in the year of 2000 and considered as the fastest commodity plastic produced (Vogl, 1999). PP is developed by polymerization process and can be categorized to slurry polymerization, bulk polymerization process and gas phase polymerization process. Among all, gas phase polymerization process is the current industrial application to produce desired PP. The production involves the PP and a catalyst to be contacted in the fluidized bed reactor. A preliminary step to control the reaction times and temperature is essential to the operation as such reduction could lower the energy consumption and prolong the lifespan of the equipment. This could be done by allowing crystal fragments to be isolated and covered entirely with a thin film of prepolymer (Martins et al., 2017). The process involves two categories which is polymerization area and extrusion area. Introduction of propylene and catalyst to the reactor are accompanied by co-catalyst, hydrogen and silane which often called as cyclohexyl methyl dimethoxy silane. Each of them has designated purpose with co-catalyst as the catalyst activator, hydrogen usage to regulate the molecular mass of polymer and silane as stereomodifier (Saravanan & Sulaiman, 2014). The powder reactor effluent will then pass through a discharge vessel for separation of carrier gas (hydrogen) and PP product before passing through a purge vessel. Purge vessel utilizes nitrogen to purge the powder of residual monomers before temporarily stored in silo as temporary storage upon entering the extrusion area (CHAMAYOU, 2015). Additives are mixed with the effluent beforehand by feed hoppers. PP is melted in contra-rotating screw extruder, forming a homogenized composite. Pelletized PP is conducted by using an underwater pelletizer due to its hot properties after the die plate section (Alastalo, 2001). Further removal of off-gas is conducted in degassing unit before packed and transported. 22 PP is a non-polar polymer with high superior insulating properties due to its large band gap (Kilic et al., 2017). Its common application in nanocomposite is often associated with its low cost, different physical properties and relatively high heat distortion temperature (Zaferani, 2018). In addition, researchers often sought for PP improvement in all properties such as thermal, mechanical, rheological, gas permeation as well as dielectric performance (Pérez et al., 2010). Although it exhibit a low polarity (Ferreira et al., 2011) and low dielectric constant, PP do have good balance stiffness as well as processibility, ensuring its application in electronics (Ammar, 2020). By introducing PP as the host polymer matrix for mixing with an inorganic filler, analysis shows that it has the potential for improved properties, mainly in automotive industry (Watanabe et al., 2020), dielectric efficiency (Nasrin et al., 2018) and packaging sector (Khalaj et al., 2016). Hence, these elements influence its vast application on recent nanocomposite analysis and will be further discussed in this review. Incorporation of nanofillers are expected to improve most of the host polymer properties and enables them to be structurally modified for better use. Although commonly used fillers for PP are clay and calcium (Zhou et al., 2005), TiO2 also shows improvement on properties of composite (Ramazanov et al., 2018). TiO2 is an oxide ceramic with three different structure namely rutile, anatase and brookite form (PARVIZI-MAJIDI, 2000). Nanoscale TiO2 can be produce from various processing methods such as deposition methods, oxidation methods, sonochemical and microwave-assisted methods, hydro/solvothermal methods, sol-gel methods, template-based methods, electrochemical anodization. Above all, sol-gel method is the commonly used approach to synthesize TiO2 (Ullattil & Periyat, 2017). Figure 2.8: Sol-gel processing for TiO2 (Ullattil & Periyat, 2017). 23 In general perspective, sol-gel method is conversion of solution by using polymerization which influenced by water. This method is preferable due to its ability to process at low temperature and produce a homogenous composite. The process begins with mixing of precursor with water in an organic solvent (Araoyinbo et al., 2018). After that, the homogenous solution is converted into a sol by using a reagent. Self-polymerization and condensation method were used to convert sol into the gel. Aside from its easy requirement for simple equipment, sol- gel method assures high chemical purity as no grinding nor pressing steps are required . Choosing an appropriate method for TiO2 is crucial as morphology and anatase-rutile formation influence nanofillers dielectric properties (A. Wypych et al., 2014). 2.6 Additives for polymer composites Alternatives to improve polymer composites properties consists of combustion modifiers, release agents, lubricants, anti-block additives, catalysts, UV stabilizers, optical brighteners, plasticizer and coupling agent. 2.6.1 Fillers As described previously, dispersing a nano-scale fillers brings huge potential in the industry as compared to conventional single polymer composite. Since major application of nanocomposites is for capacitors, the ionic interaction and electrical conductivity are an important performance factors. Regardless of distinct type of nanofillers, the dielectric properties such as permittivity, dielectric constant, dielectric loss and breakdown strength are significantly improved (Sudha et al., 2017). Apart from dielectric enhancement, the mechanical properties consisting of flexural, impact, stiffness and Young’s modulus of elasticity also shows rigidity in performance upon tested (Abdul Majid et al., 2019). Besides that, each addition of nanofillers also will increase the particle weight ratio, improving the thermal conductivity (Tessema et al., 2017). Consideration should be taken on the polymer polarity as it will affect the phase morphology of the nanocomposite (J. W. Lim et al., 2008). The interfacial area between the components will signify the interaction between them, causing different end properties for each fillers. 24 2.6.2 Combustion modifiers Applications of polymers in electrical and medical housing requires the component to be retardants towards flame. This is to allow for safe use whenever there is any significant fire hazard present (Zweifel , Maier, 2009). A research conducted by Liming He et. al. focuses on various type of combustion modifiers on polymer-based propellant. Additives uses in the analysis are lead phthalate, lead oxide, copper adipate and cupric oxide. After curing reaction has been carried out, lead phthalate emerges as the most prominent combustion additives on polyurethane (polymer). For other three components, there are no significant changes on the activation energy. The metal cations in the catalyst influenced the performance of modifiers (He et al., 2019). 2.6.3 Release agents Coefficient of friction can be reduced by using release agents. In addition, it also allows the polymer to stay unattached with their own surfaces or others, for instance, processing machineries (Stevens, 1993). There are two types of release agents; mold-release agents and slip agents. Mold-release agents refers to agents that is used to prohibit adhesion in both compression and injection molding (Kent, 2002). Slip agents on the other hand, is agents used in calendaring and extrusion process (Kloziński & Jakubowska, 2019). Since the additives properties are yet to be explored, there are limitation on the idea of release agents identity (McKeen, 2012a). 2.6.4 Lubricants Operation of polymer happens at high temperatures and beyond its crystalline melting points. Heat generated from the process increases reactions of degradation to occur, causing higher tendency of multiphase dispersion (Zweifel , Maier, 2009). Generally, alteration on the polymer’s melt rheology during molding is controlled by lubricants. Two types of lubricants are external lubricants and internal lubricants. External lubricants is added to manipulate the degree of friction as well as adhesion whereas internal lubricants is imposed to lower the melt viscosity while simultaneously increase the heat dissipation (Hunt, 2000). Internal lubricants are influenced by both thermal diffusion and deformation (Samyn & Schoukens, 2008). Efficiency of lubricant as additive is studied on a research article by S.I. Shara et. al.. It can be concluded that with an addition of ethylene propylene diene monomer (EPDM) as the lubricant, viscosity index and 25 thermal stability properties of polymer records an increment trend (Shara et al., 2018). As a result, polymerization process is conducted at a more efficient condition. 2.6.5 Anti-block additives By definition, anti-blocking is a term for signifying ways to prohibits the film sheets from sticking to themselves (Zweifel , Maier, 2009). In order to achieve the objectives, there are two possible ways for polymer adjustment. One of them is by adding mineral particles into the polymer for roughness boosts, subsequently affecting low interaction in the contact area. Another alternatives would be utilizing slip additives for easy glide when the particles slide against one another (Zilles, 2016). Its application has been commercialized since the earliest patent issued by James A. Allen in 1983 on addition of slip and anti-block agents to decrease the blocking characteristics of olefin polymer, low-density polyethylene (LDPE) (Knight, 1983). In total, a polyester polyol, polycaprolactone (PCL) is suggested to be the most effective additive for interaction reduction (Smith, 2006). 2.6.6 Catalysts Generally, catalyst aids the polymer process by promoting the rate of chemical reaction without affecting the final product composition. During polymerization process, catalyst used may influence the operating parameters as well as residence-time distribution in the reactor (Németh et al., 2006). Choices of catalyst is crucial a study conducted by M. V. Pandya et. al. claims that the choice of additives causes decrease in the reaction rate. This is because of the complex formation between the chosen polymer and additive, causing low rate of polymerization reaction (Pandya et al., 1982). Before inclusion of stabilization packages, the catalyst residue formed will affect the color (Terzopoulou et al., 2017), oxidation and degradation trait (Del Teso Sánchez et al., 2016). Last but not least, addition of catalysts also affects the morphology and functionality of polymer (Ardila-Suárez et al., 2015). 26 2.6.7 UV stabilizers Polymer degradation from ultraviolet (UV) energy can be prevent by using a UV stabilizers. Common additives such as absorbers and free-radical scavengers causes polymers to have high resistance towards the fluorescent and daylight exposure (Alfredo Campo, 2008). Chemical interaction of the stabilizers occur through covalent bond in the polymer chain, giving resistance ability towards extraction as well as evaporation (Konstantinova et al., 1994). In recent years, there have been some efforts pertaining to formulation of new non-toxic additives which could potentially provide high resistance to UV irradiation with the same thermal stability and pollution prevention measures (Huang et al., 2016). Apart from that, harsh environments that could potentially affecting the polymers was studied by Ikram Hussain et. al. using hindered amine light stabilizer (HALS). Results shows that HALS able to assists the polymer by promoting the oxidation functional groups, hence increasing both photooxidative reactions and prolong lifespan of the films (Hussain & Redhwi, 2002). On a similar note, HALS is proven to provides more stability with better surface smoothness (Brostow et al., 2020). 2.6.8 Optical brighteners Optical brightness or commonly called as fluorescent whitening agent is an additive used to manipulate the visual physical properties of polymers. They encourage the plastic to look brighter, for instance, from white to yellow. When exposed to UV light, the additives will transform the light into a visible blue spectrum which enables precision of quality control measures (A Shrivastava, 2018). Brighteners possess good melting points property, heat stability and dissolution in plastics (Jervis, 2003). Two commonly used additives are bis-benzoxazolyl-stilbene and bis-benzoxazolyl-thio-phene. The configurations and properties of those agents are described in Figure 2.9. In addition, brighteners are usually combined with other components such as pigments and dyes to achieve the desired shade requirements (Muller, 2011). 27 Figure 2.9: Properties of bis-benzoxazolyl-stilbene and bis-benzoxazolyl-thio-phene (Jervis, 2003). 2.6.9 Plasticizers Plasticizers is an additive used to control the flexibility of polymer. By using a different application of plasticizer agent, the mechanism gives different performance. Generally, the process is conducted by heating and mixing method until the resin has been completely dissolved. The plasticizer weaken the polymer-polymer interaction and prohibit from a rigid network to be formed. As a result, van der Waals forces increases as well as other properties such as flexibility, elongation and softness (Godwin, 2000). According to a study by George Wypych, using plasticizers on polymers give substantial of effect towards the mechanical properties as well. It is observed in Figure 2.10 that with an addition of plasticizer, both elongation and impact strength increased whereas hardness and tensile strength decreased (G. Wypych, 2017). In addition, zinccontaining additive can be used if polymer degradation is likely to occur due to biological influence (Vikhareva et al., 2021). Other than that, a novel amphiphilic polymer, Soluplus® can be utilized to improve the polymer films (H. Lim & Hoag, 2013). Figure 2.10: Tensile strength and elongation study on plasticizer effect (G. Wypych, 2017). 28 2.6.10 Coupling agents By definition, coupling agents is a reactive and low molecular weight additive that will react with a filler, fiber or polymer to increase the mechanical properties and compatibility between them (Pfaendner, 2010). Cooperating fillers or other reinforcement on the polymer could weaken the composite. By using coupling agents, the objectives of prolong the time taken for dissimilar materials to separate from one another can be successfully achieved (Coleman, 2017). Among all, silane chemistry is the best coupling agents for most polymers. A study by Liu Jiesheng et. al. concluded that silane interferes with the crosslinking action, giving high tensile strength and hardness properties (Jiesheng et al., 2013). Similar performance could also be observed from coupling agent research on the bio-composite (Pisanu et al., 2019) and bio-fillers (Alsewailem & Binkhder, 2014). 2.7 Nanocomposites and its potential Nanocomposites possess numerous upbringing potential for various industry, offering significant boost to their chemical and physical properties. This leads to rising numbers of publications on nanocomposite and its significance for the past few years (Broitman, 2018). Other than venturing new innovations in dielectric and packaging application, nanocomposite also has been utilized in other field such as prosthetic devices in medical industry. By using nanocomposite as prime substance for the development of technology, it enables consumers to achieve great flexibility and durability (Hasnain et al., 2018). On the other hand, it is also heavily applied on aerospace applications which consists of electromagnetic (EM) shielding, tribology, coatings and structures (Rathod et al., 2017). Despite its vast application, usage of nanofillers for the polymer at a large volume are not favorable towards cost efficiency (Bhattacharya, 2016). A high demand is necessary to ensure that the operation have to be economically advantage while simultaneously producing the desired volume and quantity of nanofillers. In addition to their undesirable process cost trait, the green engineering objective and redispersion of nanofillers into the polymer matrix are yet to be achieved (Rothon, 2017). Although it can be used as a packaging end-product, consideration should also be taken as it may give safety issues to human health because of their physiochemical properties (Honarvar et al., 2016). 29 3. CHAPTER THREE: METHODOLOGY 3.1 Materials Preparation 3.1.1 In-situ intercalative polymerization In-situ polymerization involves either a solvent-free system or solvent-based system (Pielichowski & Michalowski, 2014). Generally, this method consists of three steps which is later shown in Figure 3.1. Its extensive used is promoted during Toyota’s initial discovery on nanocomposite application. The reaction occurred is initiated from three different factors, which is radiation or heat, cationic exchange by catalyst or initiator dispersion (H. Roy et al., 2018). The polymer produced from the process is either a delaminated structure or an exfoliated polymer. Detailed study is conducted by Sharanabasamma M Ambalagi et. al. which utilizes the concept on polyaniline (PANI) and copper dioxide (CuO) nanocomposite preparation. Based on a comparison of nanocomposite with a single nanoparticles X-ray diffraction figure, it is concluded that there are no significant effect towards the crystalline structure and dispersion of nanofillers is achieved (Ambalagi et al., 2018). In total, in-situ intercalative polymerization can be considered as an option for materials preparation due to its interlayer spacing improvement well-exfoliated nanoplatelets formations. Apart from refractive index consideration, concerns also arises from unreacted educts affecting the end product (Q. Guo et al., 2014). Pretreatment of nanoscale additives by using modifiers. Dispersion of additives on the monomers. Bulk or solution polymerization is conducted. Figure 3.1: General process flow 30 3.1.2 Template synthesis (sol-gel technology) Sol-gel technology uses a different approach to produce the desired nanocomposite. The formation comprises of two general steps which is hydrolysis followed by a polycondensation reaction (Guglielmi & Martucci, 2017). The kinetic reactions occurred in the process is influence by silane to water ratio, temperature, catalyst and many more (Kesmez et al., 2011). Since morphological structure plays an important role in the synthesis of nanocomposite, sol-gel is favored in comparison to other traditional blending alternatives . After the sol-gel reactions has been successfully achieved, equations generated below is the general summary that could be concluded from the process. Base-catalyzed and acid-catalyzed have distinct effect on the end materials. Although the process is easier to construct, using based-catalyzed reaction could potentially produce undesired nanocomposite dimension quantity, hence failing the objectives of the research analysis (Zou et al., 2008). With such limitation on the choices of catalyst, only acidcatalyst reaction brings better results, particularly in terms of structural organization. Figure 3.2: Sol-gel complete equation (Zou et al., 2008). 3.1.3 Melt intercalation Melt intercalation is a mechanical approach which does not use solvent in producing a nanocomposite. General approach of melt extrusion involves the compound to be exposed and mix at high temperature followed by a series of cold and hot stretching (Castejón et al., 2018). In order to maintained the performance at its peak, it is necessary to reduce the modifier effect on the crystalline morphology film as high as possible (Wang et al., 2017). Competitive degradation and crosslinking reaction is expected to improve the morphological performance of blended nanocomposite (Jones, 2017). Concept of shearing stresses is heavily applied as aggregation factor can be break and retained (Ivanoska-Dacikj & Bogoeva-Gaceva, 2019). It is later proven that there are distinct morphologies produced from a conventional injection molding and non-conventional injection molding. According to results obtained from a study by Alejandra Constantino et. al., the 31 non-conventional injection moldings leads to high degree of crystallinity of the skin layer although data from X-ray diffractometer shows small differences (Costantino et al., 2012). Table 3.1: Comparison of nanocomposite synthesis Type Advantages In-situ • High interlayer spacing. intercalative • Ease of operation. polymerization • High process performance. Disadvantages • availability of monomers • method Sol-gel Low and inconsistent Formation of unreacted educts at the final material. • process Compatibility with a wide • precursors. • Easily operated. • Only mild conditions required to In application of silica, it gives poor reactivity. • Formation of composites with more than 100nm. operate. Melt- • More economical or inexpensive. intercalation • More flexible for formulation. method • High compatibility in commercial applications. • Not feasible for highperformance polymers. • Difficult to obtain the high dispersion level. Based on general analysis described in Table 3.1, melt blending is the most practical and broadly applicable method, which will be further discussed in this report analysis. The goals of our research analysis is to produce the highest homogenous dispersion between the polymer (PP) and the nanoscale filler (TiO2). The two feedstocks need to be obtained beforehand. The procedure of operation begins with a drying process for 24 hours in order to remove the moisture content, which could interfere with the mixing efficiency between the host and the fillers (dal Lago et al., 2020). Next, the composites with designated ratios of 10,20,30 and 40 wt.% nanofillers are passed into a twin screw extruder at 100rpm at three different temperature profile, 220oC, 230oC and 240oC. Twin screw extruder are preferred because of its high efficient performance in producing a maximum dispersion of nanocomposite (Anshuman Shrivastava, 2018b). The working principle of an extruder is the plastic would be melted and simultaneously forced to passed through a die with a fixed opening. 32 The molten product from the process is later cooled at normal room temperature, forming a long rod-chain of extrudates (Nasrin et al., 2018). After the formed nanocomposite is cut into small pieces by a pelletizer (Wang et al., 2017), it is later then melt-pressed by an injection molding machine at 180oC with a load of 100kN (Cabello-Alvarado et al., 2019). The pelletized material is later then fed to a heating chamber by using either a plunger or a screw. The hot mixture is injected into the mold and produces cavities of the shape. Hence, the mold opened and the products are ejected and collected (Koppens, 1991). Figure 3.3 shows the internal component of injection molder for a clearer in-depth understanding. The nanocomposite is later studied by thermal and dielectric studies. Figure 3.3: Injection molding machine (Koppens, 1991). 3.2 Analysis 3.2.1 Microscopic analysis Micro-structural analysis often use electron microscope as the equipment in research laboratories regards to any processing methodologies. It is widely used in many industries to characterize certain materials although it is an expensive unit and frequently bought by large organization. There are several advantages and disadvantages associating with usage of electron microscope. First of all, electron microscope provide a high-resolution image at a high magnification range. As a result, the electron-emitting device able to also produce the chemical and structural identification at a very specific area. However, its requirement for vacuum operations could interfere with the nature of the material, damaging them at an atomic level (Inkson, 2016). 33 In recent technology, there are two types of electron microscopy which is transmission electron microscopy (TEM) and scanning electron microscopy (SEM). TEM can be defined as an electron microscope which uses electron beams on a specific area by passing through an ultrathin specimen to identify the object (nanomaterials), hence acquiring the chemical as well as physical structure (Karak, 2018a). The electron energies emitted were later then received by a detector and an image is later formed. Although TEM is known for its high details and high magnification as compared to conventional light microscope, the sample preparation is highly time consuming as the process requires a vacuum state operation, making it undesirable for living specimen identification (Raghavendra & Pullaiah, 2018). Despite its high consideration, it has been utilized to identify the microstructure of clay nanocomposite (Morgan & Gilman, 2002) and polyethylene nanocomposite (B. L. Silva et al., 2014). SEM, on the other hand, is an electron microscope which produces an image of a material by focusing beam of electrons to a spot, without having to pass through an ultrathin sample (Raghavendra & Pullaiah, 2018). The signals are detected after the electrons and atoms interact against each other. In this research analysis, SEM will be used due to its simple operation as well as faster sample preparation (Karak, 2018a). Electrons theoretically flows at 1-30 kV accelerating voltage, with different analysis shows chosen voltage at 2 kV (Wang et al., 2017), 3 kV (CabelloAlvarado et al., 2019), 5 kV (Aydemir et al., 2016), 10 kV (Mohanapriya et al., 2016), 15 kV (Nasrin et al., 2018) and 20 kV (Ercan et al., 2017) for their microscopic analysis. 15kV of electron voltage is chosen as it shows similar approach by A. Maharramov et. al. on the structural analysis (Maharramov et al., 2016a). Figure 3.4 signifies the internal component of SEM microscope for clearer view. Electron gun consists of the first two unit in the diagram which is electron source as well as accelerating anode. Electron source is the component that will provide an electron beam throughout the process. The electrons will pass through series of lenses to encompasses the electrons on a specified area, increasing the efficiency of material identification. The interaction between the electron and the specimen will also be detected by multiple detectors before the signals are portrayed in the computer for researchers further actions. The vacuum pressure inside the equipment is kept at 0.110-4 Pa to prevent from release of volatile components (Inkson, 2016). 34 Figure 3.4: SEM microscope (Inkson, 2016). 3.2.2 Thermal measurement Understanding the thermal properties of material is essential on providing detailed assumptions on its possible lifetime (Saisy Kudilil Esthappan et al., 2012a). Numerous factors influencing the thermal response of a nanocomposite includes the thermal properties of fillers, coefficients of thermal expansion (CTE), moisture content and many more (Sauerbrunn et al., 2015). Thermogravimetric analysis (TGA) is a common approach to acquire the thermal image of material because of its fast, less expensive and easy technique (Gomes et al., 2018). TGA can be defined as a method of thermal monitoring when a substance is exposed to a controlled temperature environment within a timeframe (Elmer, 2010). Other than investigating on the decomposition and loss of volatiles, it can be used to acknowledge the thermal stability, moisture content and oxidation properties (Polini & Yang, 2017). 35 TGA can be broken down into several compartments as shown in Figure 13. Generally, the thermogravimetric analyzer (TA) aims to study the changes in weight as the temperature value increases. There are two main components heavily required for the unit operation, which is a furnace and a weighing scale. The highly sensitive weighing scale is placed on top of furnace and isolated away from the heat to maintain the high sensitivity and precise weighing measures (Ebnesajjad, 2006). The furnace, on the other hand, is a programmable unit for heat control with different material as the heating element. Heating elements such as platinum and alloy associates with the thermal capability of the furnace. Figure 3.5: Thermogravimetric analyzer (Unapumnuk et al., 2006). Experimentation using TA requires controlled parameter for nanocomposite. As shown in Figure 3.5, the nitrogen gas will be supplied at the top section to purge any remaining oxygen inside the area (Unapumnuk et al., 2006). According to several researchers, the flow of heat vary from 10 oC/min (Awad & Khalaf, 2019) to 20 oC/min (Saisy Kudilil Esthappan et al., 2012a). Difference in temperature range also can be observed such as 15oC to 600oC (K. Ahmed et al., 2016), 20oC to 800oC (Saisy Kudilil Esthappan et al., 2012a), 25oC to 550 oC (Maharramov et al., 2016b), 30oC to 500oC (Awad & Khalaf, 2019) and 30oC to 700oC (Nasrin et al., 2018). In conclusion, the heat for the analysis will flow at 20oC/min at a temperature range of 25oC to 700oC due to similar approach by several studies. As a result, the thermogram as shown in Figure 3.6 will be generated indicating the point where the weight loss. 36 Figure 3.6: TGA thermogram (Awad & Khalaf, 2019). 3.2.3 Dielectric properties There are different variety of dielectric measurement unit. This includes impedance analyzer (Nasrin et al., 2018), immittance meter (Ramazanov et al., 2018), capacitance-voltage measurement system (Yu et al., 2016), dielectric analyzer (T. I. Yang & Kofinas, 2007), ALPHA analyzer (Ju et al., 2014). Since LCR meter is use in several other articles, it will be used as the equipment in this article with a frequency from 25Hz to 1 MHz. In addition, there are several methods worth mentioning concerning on dielectric measures. First of all, two methods are the usual practical or standard applied to identify the dielectric breakdown strength. Both are Standard Test Method for Dielectric Strength of Solid Electrical Insulating Materials at Commercial Power Frequencies (ASTM D149-20) and Electric Strength of Insulating Materials (IEC 60243-1) (Anshuman Shrivastava, 2018a). To test different dielectric constant properties, two standard test is used. Both of them are Standard Test Methods for AC Loss Characteristics and Permittivity of Solid Electrical Insulation (ASTM D150) and Recommended Methods for the Determination of the Permittivity and Dielectric Dissipation Factor of Electrical Insulating Materials at Power, Audio and Radio Frequencies Including Meter Wavelengths (IEC 60250) (Anshuman Shrivastava, 2018a). Last but not least, to calculate the both the surface and volume resistivity, both ASTM D57 and IEC 60250 are the applicable method. 37 4. CHAPTER FOUR: RESULTS AND DISCUSSION 4.1 Surface Morphology Presentation of surface morphology findings are as follows. Table 4.1: Morphological structure of PP/TiO2 nanocomposite. No 1 Synthesis method Structure analysis Melt intercalation Scanning electron TiO2 Result References 0 wt.% No significant (Saisy Kudilil changes. Esthappan et microscopy (SEM) al., 2012a) 2 Melt intercalation Scanning electron 0 wt.% microscopy (SEM) No significant (Saisy Kudilil changes. Esthappan et al., 2012b) 3 Melt intercalation Scanning electron 0 wt.% microscopy (SEM) 4 Melt intercalation Scanning electron changes. 0 wt.% microscopy (SEM) 5 Melt intercalation Scanning electron Melt intercalation Scanning electron 0.25 wt.% Melt intercalation Transmission Less agglomeration. 0.5 wt.% microscopy (SEM) 7 No significant changes. microscopy (SEM) 6 No significant Less agglomeration. 0.5 wt.% electron Less agglomeration. (Nasrin et al., 2018) (Soares et al., 2015) (Soares et al., 2015) (Soares et al., 2015) (Soares et al., 2015) microscopy (TEM) 8 Melt intercalation Scanning electron 0.5 wt.% microscopy (SEM) 9 Melt intercalation Scanning electron agglomeration. 1 wt.% microscopy (SEM) 10 Melt intercalation Transmission electron Less Less agglomeration. 1 wt.% Less agglomeration. (Aydemir et al., 2016) (Soares et al., 2015) (Soares et al., 2015) microscopy (TEM) 38 11 Melt intercalation Scanning electron 1 wt.% microscopy (SEM) 12 Melt intercalation Scanning electron Less agglomeration. 1.5 wt.% microscopy (SEM) (Aydemir et al., 2016) Homogenous (Saisy Kudilil dispersion. Esthappan et al., 2012a) 13 Melt intercalation Scanning electron 2 wt.% microscopy (SEM) 14 Melt intercalation Scanning electron Less agglomeration. 3 wt.% microscopy (SEM) (Aydemir et al., 2016) Uniform (Saisy Kudilil dispersion. Esthappan et al., 2012b) 15 Melt intercalation Scanning electron 3 wt.% microscopy (SEM) Small aggregation of (Zohrevand, 2013) particles. 16 Melt intercalation Scanning electron 4 wt.% microscopy (SEM) Larger agglomeration (Aydemir et al., 2016) formed. 17 18 In-situ Scanning electron intercalative microscopy (SEM) Melt intercalation Scanning electron 5 wt.% 5 wt.% Uniform (Ramazanov distribution. et al., 2018) TiO2 (Zohrevand, aggregation microscopy (SEM) 2013) tendency increases. 19 In-situ Scanning electron intercalative microscopy (SEM) 10 wt.% Coagulation of (Ramazanov nanoparticles et al., 2018) occurred. 20 21 Melt intercalation Melt intercalation Field emission Homogeneous (Wang et al., scanning electron dispersion with 2017) microscope lower (FESEM) agglomeration. Scanning electron microscopy (SEM) 10 wt.% 20 wt.% High agglomeration. (Nasrin et al., 2018) 39 22 Melt intercalation Scanning electron 20 wt.% microscopy (SEM) Lesser (Forhad Mina agglomerates et al., 2009) than 40 wt.%. 23 24 Melt intercalation Melt intercalation Field emission 40 wt.% Homogenous scanning electron dispersion with microscope higher (FESEM) agglomeration. Scanning electron 40 wt.% microscopy (SEM) Lumps (Wang et al., 2017) (Nasrin et al., formation on 2018) the surface. 25 Melt intercalation Scanning electron 40 wt.% microscopy (SEM) High (Forhad Mina agglomerates et al., 2009) formed. Table 4.2: Summary of morphological structure of PP/TiO2. No Synthesis method TiO2 Result 1 Melt intercalation 0 wt.% 2 Melt intercalation 0.25 wt.% Smooth surface with least agglomeration. 3 Melt intercalation 0.5 wt.% Smooth surface with least agglomeration. 4 Melt intercalation 1 wt.% Agglomeration occur at low level. 5 Melt intercalation 1.5 wt.% Agglomeration occur at low level. 6 Melt intercalation 2 wt.% Agglomeration occur at low level. 7 Melt intercalation 3 wt.% Agglomeration occur at low level. 8 Melt intercalation 4 wt.% Agglomeration increases. 9 Melt intercalation 5 wt.% Agglomeration increases. 10 Melt intercalation 10 wt.% High rate of agglomeration. 11 Melt intercalation 20 wt.% High rate of agglomeration. 12 Melt intercalation 40 wt.% High rate of agglomeration with lumps No significant changes. formation. 40 Tabulation of data shown above comprises of research findings from distinct articles mentioning on the morphological structure involving PP as the host polymer matrix and TiO2 as the nanoscale filler. In general view, there are two approaches used by the researchers to produce the nanocomposite. Melt intercalation is the widely used method instead of in-situ intercalation. This is because melt intercalation gave lesser impact to environment as well as providing high compatibility for bigger industrial application. Scanning electron microscopy is the most favored method to interpret the interaction between the compound. The addition of TiO2 content ranges from 0 wt.% until the maximum value recorded which is 40 wt.%. The trend shown describes the agglomeration rate increases as the concentration of TiO2 increases. (a) (b) Figure 4.1: SEM micrographs of neat PP (0 wt.% TiO2) (a) (Nasrin et al., 2018) (b) (Saisy Kudilil Esthappan et al., 2012b). Neat PP is used as the standard measure for comparison of structure before and after the addition of nanofiller. The morphological structure of neat PP is as shown in the Figure 4.1 which clearly portray the surface of composite at a microscale. Figure above shows the structure of PP with a smooth surface without any addition of TiO2. In order to improve the properties of PP and increases the desire on dielectric application, addition of nanofillers is crucial to boosts the performance of composite. 41 (a) (b) Figure 4.2: SEM micrographs of PP/TiO2 (a) 0.5 wt.% (Soares et al., 2015) (b) 1.5 wt.% (Saisy Kudilil Esthappan et al., 2012a) Addition of nanofillers less than 1 wt.% shows a very small effect on the morphological structure. Despite small TiO2 content is dispersed in the polymer matrix, Igor Lopes Soares concluded that the nanofillers are well distributed. On top of that, it is later observed that TEM analysis differs with the SEM conclusion. The addition of nanofillers does distributed on the polymer surface, however, the dispersion objective are not achieved since aggregation forms two types of crystal in the nanocomposite. As shown in Figure 4.2 (b), upon addition of TiO2 reached a 1.5 wt.%, the structure shows better dispersion with insignificant agglomeration formation as opposed to previous measure. Figure 4.3: SEM micrographs of PP/TiO2 at 4 wt.% (Aydemir et al., 2016). Continuation of the analysis is addition of 2 wt.% and 3 wt.%. Similar to previous approach on 1.5 wt.% of TiO2, 2 wt.% and 3 wt.% addition of TiO2 also indicate a good dispersion with minimal rate of agglomeration. However, once 4 wt.% of TiO2 is added, formation of agglomerates increases significantly, forming an increase in its volume. Agglomerations at high level are not favored due to its ability to weaken the upbringing traits of nanocomposites (Ashraf et al., 2018). 42 (a) (b) Figure 4.4 SEM micrographs of PP/TiO2 (a) 10 wt.% (Wang et al., 2017) (b) 40 wt.% (Nasrin et al., 2018) Following that, addition of the 5 wt.% TiO2 content shows similar trend as 4 wt.% of TiO2 content. Higher content of TiO2 also signifies large coagulation of TiO2 nanoparticles and changes of nanoparticles sizes. It is observed that 5 wt.% of TiO2 changes the size from 10nm to 30nm and 10 wt.% of TiO2 gives 50nm to 60nm (Ramazanov et al., 2018). This meets with the desired particle’s diameter range provided by manufacturers (Masoudifar et al., 2018). With each addition of nanofillers starting from 10 wt.% the number of particles on the polymer surfaces increases with distance between them decreases. 40 wt.% is the highest TiO2 content in all of the research analysis conducted. At this state, hole will be formed in the surfaces, developing roughness as well as darkness feature to the nanocomposite, making them no longer compatible against one another (Nasrin et al., 2018). This results in low interfacial bonding and reduce its performance when exposed to external stress (Wang et al., 2017). Surface morphology plays a major role in determining both dispersion as well as distribution of PP/TiO2 as the mobility further indicates the transport traits used in energy applications particularly electronics and automotive industry. A high content of nanocomposite shows unfavorable results because of covalent bonded chained to the surface of TiO2. Formation of aggregation on the surface causes weak accessibility of TiO2 to the matrix surface and causes the material’s weak ability to transmit energy (Ashraf et al., 2018). In addition, interaction between the chosen TiO2 and non-polar properties of PP significantly affect the transition region, causes molecular polarizability hence simultaneously affects the dielectric constant. 43 Apart from utilizing PP as the main source of host polymer matrix, other researchers also uses reinforced PP to be paired with TiO2 for nanocomposite. Among them are polypropylenereinforced rice husk (P-RH) composite, polypropylene- carbon nanotube (P-CNT) and polypropylene-polyethylene terephthalate (P-PET). Based on the tabulation of data in Table 4 and Table 5, it can be concluded that dispersion is achieved between 3-5 wt.% of TiO2. Including nanofillers in the composite enables the interaction of modified composite to increase and the gap between them can be minimized (Awang, 2017). As a result, agglomeration decreases and the nanocomposite is produced at desired condition. Table 4.3: Morphological structure of reinforced PP/TiO2 nanocomposite No 1 Nanocomposite P-RH composite Analysis TiO2 Scanning electron 0 wt.% microscopy (SEM) 2 P-RH composite Scanning electron Result No significant References (Awang, 2017) changes. 10 wt.% microscopy (SEM) Gap between (Awang, 2017) the polymer matrix and RH is reduced. 3 P-RH composite Scanning electron 40 wt.% microscopy (SEM) 4 P-CNT composite Scanning electron P-CNT composite Scanning electron (Awang, 2017) formation. 1 wt.% microscopy (SEM) 5 Bundle 5 wt.% microscopy (SEM) Least (Cabello- agglomeration Alvarado et al., with less filler. 2019) Less agglomeration. (CabelloAlvarado et al., 2019) 6 P-CNT composite Scanning electron 10 wt.% microscopy (SEM) Agglomeration increases. (CabelloAlvarado et al., 2019) 7 P-PET composite Scanning electron microscopy (SEM) 3 wt.% TiO2 is well dispersed. (Matxinandiarena et al., 2019) 44 8 P-PET composite Scanning electron 7 wt.% microscopy (SEM) Particle size dispersion (Matxinandiarena et al., 2019) decreases. 9 P-PET composite Scanning electron 12 wt.% microscopy (SEM) Reduction in (Matxinandiarena PET particle et al., 2019) size. 10 P-PET composite Transmission 3 wt.% electron Small changes (Matxinandiarena on the surface. et al., 2019) microscopy (TEM) 11 12 P-PET composite P-PET composite Transmission 7 wt.% Coating of (Matxinandiarena electron nanoparticles microscopy (TEM) increases. Transmission 12 wt.% et al., 2019) Interface almost (Matxinandiarena electron completely microscopy (TEM) covered by et al., 2019) TiO2. Table 4.4: Summary of morphological structure of PP/TiO2 nanocomposite. No Composite TiO2 Result 1 Polypropylene-reinforced rice husk (P- 3 wt.% TiO2 well dispersed. 5 wt.% TiO2 well dispersed. 3 wt.% TiO2 well dispersed. RH) composite 2 Polypropylene- carbon nanotube (PCNT) 3 Polypropylene-Polyethylene Terephthalate (P-PET) 45 4.2 Thermal Analysis Presentation of thermal findings follows the following terms: • OD = Onset of degradation temperature • MD = Maximum degradation temperature • - = Not available Table 4.5: Thermogravimetric analysis (TGA) of PP/TiO2 nanocomposite. No 1 Method TiO2 OD MD Rate Residue (wt.%) (oC) (oC) % % Melt intercalation References (Saisy Kudilil 0 391.00 472.00 56.30 1.40 Esthappan et al., 2012a) 2 Melt intercalation 3 0 370.00 458.70 - 0.04 Melt intercalation (Aydemir et al., 2016) (Saisy Kudilil 0 324.90 433.56 30.13 0.39 Esthappan et al., 2012b) 4 In-situ intercalative 5 Melt intercalation 6 0 256.83 4479.77 - - 0 350.00 457.00 - - Melt intercalation (Ramazanov et al., 2018) (Alghamdi, 2016) (Saisy Kudilil 0.5 419.00 474.00 52.00 1.50 Esthappan et al., 2012a) 7 Melt intercalation 8 0.5 380.00 458.90 - 0.05 Melt intercalation (Aydemir et al., 2016) (Saisy Kudilil 0.5 377.84 470.58 37.64 0.68 Esthappan et al., 2012b) 46 9 Melt intercalation 10 In-situ intercalative 11 1 390.00 459.20 - 0.06 1 310.81 502.67 - - Melt intercalation (Aydemir et al., 2016) (Ramazanov et al., 2018) (Saisy Kudilil 1.5 421.00 477.00 49.30 2.10 Esthappan et al., 2012a) 12 Melt intercalation (Saisy Kudilil 1.5 373.72 469.75 40.49 1.33 Esthappan et al., 2012b) 13 Melt intercalation 14 2 395.00 459.40 - 0.14 Melt intercalation (Aydemir et al., 2016) (Saisy Kudilil 3 416.00 477.00 50.20 3.40 Esthappan et al., 2012a) 15 Melt intercalation (Saisy Kudilil 3 372.18 469.53 42.26 2.81 Esthappan et al., 2012b) 16 Melt intercalation 17 In-situ intercalative 18 Melt intercalation 19 Melt intercalation 20 Melt intercalation 4 400.00 461.10 - 0.44 5 281.32 483.35 - - 10 432.00 468.00 - - 20 440.00 475.00 - - 30 445.00 479.00 - - (Aydemir et al., 2016) (Ramazanov et al., 2018) (Alghamdi, 2016) (Alghamdi, 2016) (Alghamdi, 2016) 47 Table 4.6: Summary of thermogravimetric analysis (TGA) of PP/TiO2 nanocomposite. No TiO2 content (wt.%) OD (oC) MD (oC) References 1 0 324.90 433.56 (Saisy Kudilil Esthappan et al., 2012b) 2 0.5 380.00 458.90 (Aydemir et al., 2016) 3 1 390.00 459.20 (Aydemir et al., 2016) 4 1.5 421.00 477.00 (Saisy Kudilil Esthappan et al., 2012a) 5 2 395.00 459.40 (Aydemir et al., 2016) 6 3 416.00 477.00 (Saisy Kudilil Esthappan et al., 2012a) 7 4 400.00 461.10 (Aydemir et al., 2016) 8 5 281.32 483.35 (Ramazanov et al., 2018) 9 10 432.00 468.00 (Alghamdi, 2016) 10 20 440.00 475.00 (Alghamdi, 2016) 11 30 445.00 479.00 (Alghamdi, 2016) Temperature (oC) SUMMARY ON OD VALUES ON TIO2 CONTENT 500 450 400 350 300 250 200 150 100 50 0 Titanium Dioxide Nanofiller Content (%) 0 0.5 1 1.5 2 3 4 5 10 20 30 Figure 4.5: Graph on different OD values (oC) versus the TiO2 content (wt.%). 48 SUMMARY ON MD VALUES ON TIO2 CONTENT 490 480 Temperature (oC) 470 460 450 440 430 420 410 400 Titanium Dioxide Nanofiller Content (%) 0 0.5 1 1.5 2 3 4 5 10 20 30 Figure 4.6: Graph on different MD values (oC) versus the TiO2 content (wt.%). Analytics that have been obtained summarizes distinct findings from various researchers on the PP/TiO2 nanocomposite. The analysis conducted aims to study on the four aspects that could be obtained directly from TA. The onset of degradation (OD) temperature describes the temperature which thermal degradation begin to occur whilst the maximum thermal degradation (MD) temperature signifies the maximum decomposition of material (Bavya et al., 2019). The heating rate describes the intensity of heating along the decomposition period. After the process, the final composition of the material is collected and recorded as the final residue at chosen temperature. Previous research uses TiO2 content ranges from neat PP (0 wt.%) to 30 wt.% for precise comparison. Other than that, the summary also has been categorized with synthesis method categories, which predominantly dominates by melt intercalation method. Based on summary in Figure 4.5 and Figure 4.6, the values obtained slightly differs as the synthesis method is differ by certain parameter and external factors such as temperature during extrusion process, the rotation of the twin screw extruder, rapid cooling criteria and injection molding process. However, identification on the results can be concluded from comparison with other TiO2 content materials. 49 Based on Figure 4.5, the pattern shows a slight increase in trend, indicating an improvement on onset of degradation temperature. A summary of values is used to portray the performance of material at the said temperature with different TiO2 content. The value of 0 wt.% TiO2 content for OD begins at 324.90oC with a MD readings of 433.56oC. This value has been taken from Saisy Kudilil Esthappan article which focuses on the thermal effect on PP/TiO2 nanocomposite. The highest reading can be recorded at 30wt.% of TiO2 content, which shows significant boosts on the thermal properties. However, in Figure 4.6, the highest maximum degradation temperature is recorded at 10 wt.% of TiO2 content. This further signifies improvement in thermal stability from the inhibition of thermal motions in the polymer chains (Saisy Kudilil Esthappan et al., 2012a). Figure 4.7: Thermogram of PP/TiO2 nanocomposite (Saisy Kudilil Esthappan et al., 2012a). The performance of low TiO2 content can be further analyzed from thermogram obtained. Based on Figure 4.7, there is an improvement on the onset as well as endset degradation temperature. At 0.5%, the endset of degradation increased to 499oC from 497oC. The increase in endset degradation temperature also gave an indication on the improvement of thermal stability (Saisy Kudilil Esthappan et al., 2012a). Similar improvement can be observed on 1.5 wt.% at both onset and endset of degradation. However, higher temperature stability tend to produce higher residue content. In addition, using 3 wt.% of TiO2 records a decrease value in both onset and endset degradation temperature with further increment of residue content. Hence, using higher than 1.5 wt.% have the potential to produce weaker thermal properties. 50 Figure 4.8: Thermogram of PP/TiO2 nanocomposite (Aydemir et al., 2016). The claim is further proven from Deniz Aydemir et. al., which shows similar trend on the thermogram. Based on the analysis conducted, T10% and T50% are used to indicate the temperature at which the content decreases. The neat PP has a 454.8oC for T50%whereas 4 wt.% TiO2 records a 457.3oC. From the analysis, there is constant increment on the maximum degradation temperature with reduction in mass loss along the addition of TiO2 content. Contrary to previous research analysis, the 4 wt.% does not show any significant decrease on onset as well as endset degradation temperature. However, there is close proximity of the values between one another. Figure 4.9: Thermogram of PP/TiO2 nanocomposite (1) 0 wt.% TiO2 (2) 1 wt.% TiO2 (3) 5 wt.% TiO2 (Ramazanov et al., 2018). 51 Based on Figure 4.9, M. A. Ramazanov et. al. also concluded that using 1% TiO2 content do provides positive thermal properties trait. This is mainly associated with the low TiO2 content, which utilizes reduce energy for the melting process (Soares et al., 2015). However, the declining performance can be observed on 5 wt.% from the thermogram which clearly indicates the reduction in all factors, particularly onset, endset and maximum degradation temperature. To compare, a 1% TiO2 have a 310.81oC maximum degradation temperature and 502.67oC endset degradation temperature whereas 5 wt.% TiO2 decreases to 281.32oC maximum degradation temperature and 483.35oC. The data shows a huge reduction in terms of performance although there is 2wt.% difference from the proposed TiO2 content which is 3 wt.%. Based on the significance from both article so far, it can be induced that using more than 4 wt.% of TiO2 could produce a low thermal stability and reduce its long-term performance for any heat application on end-product. For large content of TiO2 on the nanocomposite, different theoretical value are expected according to previous claims by Saisy Kudilil, Ramazanov and Deniz. Readings from Mohammed N. Alghamdi shows that although the addition of nanofiller already exceed 4 wt.%, the thermogram indicates a linear trend for each values, 10 wt.%, 20 wt.% and 30 wt.%. It is also proven by Md. Forhad Mina which shows the increment of value by using the same approach as Alghamdi. It is also believed that a good dispersion produces such high performance although the composite is exposed at high temperature (Alghamdi, 2016). The dispersion during the synthesis able to produce a residue with low degradation at 500-600oC . It is also correlated with the higher polymer chains flexibility, which tend to degrade easily at low temperature (Abdelrazek et al., 2018). Therefore, a thermal stability of nanocomposite needs to be highlighted on the dispersion, which further correlates with previous issue, compatibilization, nanocomposite surface morphology and blending properties. In addition, degradation temperature indication is crucial for the operation since the processing temperature should allow the nanocomposite to melt and flow. However, the maximum degradation temperature will be used as the limitation to prevent complete deterioration (Mat-Shayuti et al., 2016). In total, there is huge relationship between the thermal degradation and polymer chains flexibility. At lower temperature, the polymer tend to harden due to better interfacial interaction and restriction of polymer chain movement. A higher matrix polarity possess better density at the interface and thermal conductivity, potraying significant impact between heat transfer ability and interfacial interaction. 52 4.3 Dielectric Properties 4.3.1 Dielectric loss (a) (b) (c) (d) Figure 4.10: Frequency dependent dielectric loss tangent (a) 10 wt.% TiO2 (b) 20 wt.% TiO2 (c) 40 wt.% TiO2 (d) 50 wt.% TiO2 (Nasrin et al., 2018). Analysis shown describes the dielectric loss tangent trend for each TiO2 content, ranging from 10 wt.% to 50 wt.% by using an Agilent Impedance Analyzer. Study signifies that each of the filler content signifies distinct dielectric performance when exposed to a certain frequency. As the frequency increases, the loss tangent also increases until it reach a maximum peak before a decrease in value is observed. The reduction after the maximum peak is often associated with the lagging of the dipoles, hence reducing the participation of particles in the polarization (Magerramov et al., 2013). It is also can be observed that 20 wt.% TiO2 shows high dielectric loss and small differences between each temperature applied. As opposed to other TiO2 content, the trend only can be observed on the highest temperature which yields the highest maximum peak of loss tangent. 53 Figure 4.11: Frequency dependent dielectric loss tangent (1) neat PP (2) 0.5 wt.% TiO2 (3) 1% TiO2 (4) 4 wt.% TiO2 (Ramazanov et al., 2018). Figure 4.12: Volume content dependent dielectric loss tangent (Ramazanov et al., 2018). Another study by Maharramov on the dielectric loss can be observed in Figure 4.11 as well as Figure 4.12. Figure 4.11 shows an increase in dielectric loss tangent in 0.5 wt.% TiO2 and 4 wt.% TiO2. However, a significant drop occurs in 1% wt.% which it reach the minimum value compared to others. Similar trend is observed by Rahima Nasrin previously and it is mostly often associated with the destruction of conductive path because of mobility by the polymer chains (Zhao et al., 2014). It is clear from Figure 4.12 that the dependence of dielectric loss tangent only increases starting from 1 wt.%. This escalates until the maximum approach taken by Maharramov, which is 10 wt.% of TiO2 content. 54 4.3.2 Dielectric constant (a) (c) (b) (d) Figure 4.13: Frequency dependent dielectric constant (a) 10 wt.% TiO2 (b) 20 wt.% TiO2 (c) 40 wt.% TiO2 (d) 50 wt.% TiO2 (Nasrin et al., 2018) Figure 4.13 portrays distinct dielectric constant with frequency ranging from 1 x 102 Hz until 1 x 105 Hz. It is shown that the dielectric constant decreases as the value of frequency increases. Initial value at 100 Hz is marked to be the highest peak among all frequency. This is due to the dipoles inability to keep up with the electric field, thus resulting in reduction as described. It is also reported that the dielectric constant value decreases as the TiO2 content increases. 10 wt.% TiO2 content records the highest dielectric constant at 770. However, the numbers decreases as the filler content went from 20 wt.%, 30 wt.% and 40 wt.% TiO2 content. 20 wt.% and 40 wt.% of TiO2 content records a steep decrease before reaching a consistent state. This is because of the strong polarity of nanofiller which also has been highlighted by other nanocomposite study (Y. Cheng et al., 2020). 55 4.3.3 Dielectric permittivity Figure 4.14: Volume content dependent dielectric permittivity at different TiO2 concentrations (Ramazanov et al., 2018). Figure 4.15: Dielectric permittivity at different TiO2 concentrations (Zaharescu et al., 2008). Figure 4.14 shows a volume content dependent dielectric permittivity performance of the nanocomposite at various TiO2 content. There is an increase trend in dielectric constant when it reaches the maximum peak at 1 wt.% before readings at 3 wt.%, 5 wt.% and 10 wt.% shows a slight reduction. It is also observed with a temperature dependent figure and commonly escalated from the interfacial polarization between the filler and polymer matrix (Abouhaswa & Taha, 2020). However, different performance is also observed at 3D representation in Figure 4.15, which each addition of TiO2 results in increases dielectric permittivity. This results from higher tendency of dipoles detachment from the particle surface (Zaharescu et al., 2008), hence proving low permittivity properties of non -polar PP. 56 4.3.4 Dielectric resistivity Figure 4.16: Volume content dependent electrical resistivity (a) 25oC, (b) 50oC (c) 75oC (d) 100oC (Forhad Mina et al., 2009). Figure 4.16 signifies the trend of electrical resistivity upon application at different temperatures. The component that has less than 10 wt.% shows a sudden drop in resistivity. However, larger TiO2 content only shows a linear decrease at all temperature application. Since exploration of TiO2 effect on electrical resistivity is not entirely explored, the reduction along with increase of TiO2 content often associates with high immobile nanolayers. It theoretically signifies as ion traps, hence blocking the ion mobility from occurring (Singha & Thomas, 2008). Hence, it prevents from accumulation of charges on the surface. 4.3.5 Dielectric conductivity Figure 4.17: Frequency dependent dielectric conductivity of nanocomposites (a) 10 wt.% TiO2 (b) 20 wt.% TiO2 (Nasrin et al., 2018). 57 Rahima Nasrin et. al. shows a conductivity trend on different nanofiller content. The frequency effect is observed for temperatures ranging from 300, 325, 350 and 375 K as shown in Figure 4.17. The graphical trend shows a linear increase as the frequency increases. This is resulted from the interfacial polarization occurring between the host polymer PP and the nanoscale TiO2 (Nasrin et al., 2018). Although application of temperature is used in this study, there is no significant difference between each measures as the trend shows nanocomposite low dependency on the temperature. Such results also gave an indication that the bond is occupied and separation has occurred from the conduction phenomenon, hence prohibiting electrons from transportation of charge in the electrical field. 4.3.6 Electrolyte uptake capability Figure 4.18: Volume content dependent electrolyte uptake capability (Wang et al., 2017). Electrolyte uptake capability is another alternative by Shan Wang et. al. on observing the properties as it commonly applied for utilizing nanocomposite in boosting battery performance. Figure 4.18 shows an increase trend of uptake capability as the TiO2 content increases. The value went from 56% at 0 wt.% and reach a maximum peak of 104% at 40 wt.%. This occurs predominantly by two factors which are the hydrophilic traits of TiO2 and the presence of large micropores (Wang et al., 2017). As a result, the performance of nanocomposites shows better electrolyte uptake as compared to neat PP. 58 5. CONCLUSION Polymer development has brought many attention to enhance the properties especially for the dielectric applications. Significance improvement on the polymer can be observed by using nano scale filler, for additional boosts to the nanocomposite’s performance. There are several limitation of polymer, mainly PP such as low thermal properties and inability to perform at harsh conditions which enables studies of nanocomposite increases over the years. Therefore, a nanoscale filler which is TiO2 is used in this research study and reactions between the host polymer and the filler are observed through three significant parameter. Parameters include thermal, dielectric and morphological properties. PP production was developed by gas-phase polymerization process while TiO2 is produced from sol-gel process. Following that, both of them can be mixed through three different pathway such as in-situ intercalative polymerization process, sol-gel technology and melt intercalation process. Although in-situ intercalative polymerization process provides better interlayer spacing and formation of well-exfoliated platelets in polymer matrix, melt intercalation is the most preferable method by various researchers due to its low cost and low environmental effect, hence ensuring its readily applicable to the industrial application. The nanocomposite is produced by mixing both of them in a twin-screw extruder before pelletized and melted in an injection molding at high temperature. Following that, analysis on the nanocomposite is performed by SEM, TGA and LCR meter. Morphological structure results indicates formation of agglomeration beginning from 4 wt.% of TiO2 content. 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