Available online at www.sciencedirect.com anteal ScienceDirect Jews Journa. ournal of Taibah University for Seience 11 (2017) 648-683 wwivelsevienconVlocatelitusci Full Length Article Thermal, structural and morphological properties of High Density Polyethylene matrix composites reinforced with submicron agro silica particles and Titania particles Oluyemi O. Daramola‘*, Isiaka O. Oladele“, Benjamin 0. Adewuyi", Rotimi Sadiku”, Stephen C. Agwuncha” * Deparment of Metallurgical and Materials Engineering, Federal University of Technolo, PMB 70, Alure, Ondo Stat, Nigeria * Division of Polymer Technology, Department of Chentcel, Metallurgical, and Material Engineering, Tshwane University of Technology, Bag ‘X680, Pretoria 0001, South Africa Received 20 February 2016; received in revised form 10 August 2016; acepted 29 August 2016 Available online S November 2016 Abstract HDPE—based composites samples filled with 2, 4, 6, 8 and 10.wi.% submicron agro-waste silica particles extracted from rice husk ash (RHA) at constant 0.3 wt,% Titania loading were prepared using rapra single serew extruder at temperature of 200-230°C. ‘The extrudates were compressed with a laboratory carver press at a temperature of 230°C for 10min under applied pressure of 0.2 kPa and water cooled at 20°C min“, Thermal, structural and morphological properties of the composites were studied. The results ofthe thermogravimetric analysis (TGA) revealed that the composites with 10 wt.%e SiOz have the best maximum thermal degradation temperature of 438.73 °C. The erystal structure of neat HDPE, and the siliceous composites developed revealed two ‘obvious diffractive peaks of about 21.3° and 23.7° corresponding to typical crystal plane (I 10) and (200) of orthorhombic phase respectively. The diffractive peaks do not shift with the addition of silica particles; this clearly indicates that the addition of silica particles did not exert much effect on the crystalline structure of HDPE. There is no much difference in the interplanar distance (devalue). Lamellar thickness (L) of HDPE increases with the addition of silica particles, which implies that silica particles aid the formation of more perfect crystals. Scanning electron microscopy studies indicated that there were chains inter diffusion and entanglement between HDPE matrix and the silica particles at lower weight fraction (24 wt.%) of submicron silica particles which resulted into homogeneous dispersion of the particles within the matrix, © 2016 The Authors. Production and hosting by Elsevier B.V. on behalf of Taibah University. This is an open access article under the CC BY-NC-ND license (htip//ereativecommons.org/licenses/by-ne-nd/t.0). Keywords: High Density Polyethylene; Rice husk ash; Submieron agro waste silica particles © Corresponding author Exmail cuddresse ojaythompsoms@yahoo.com, cengryemidaramola@ pail com (0.0, Daramls). Peer review under responsibilty of Tabah University me aiviet_| Production and hosting by Elsevier hiap/4ds.do.org/0,1016,jtsei.2016.08,006 1658-3655 © 2016 The Authors. Prodlction and hosting by Elsevier B.V. on behalf of Taibah University, Tis i an open access article under the (CC BY-NC-ND license (htp//ceativecommons.oricensesby-ne-nd/.00,646 0.0. Daramola etal. / Journal of Taibah University for Science 1] (2017) 645-653 1, Introduction Siliceous particulate composites are used in a vari- ty of applications to isolate components, areas, or other materials from potentially stressful conditions that can adversely affect the performance of a device. For exam- ple, the performance of photovoltaic (PV) modules may decrease over a time as the waler penetrates the mod- ule and corrodes the metallic components essentially for module function, In the absence of water, corro- sion occurs relatively slowly because by-products are less able to diffuse away from a surface to allow the cottosion process to progress [1,2] The PV industry has long—recognized the dramatic effect that corrosion has on module performance. Today PV modules typically include a polymeric encapsulant ‘material to isolate the components from the ever-present potentially adverse conditions created by various sources of water, including rain, snow and condensation. The isolation created by the encapsulant protects the PV com- ponents from corrosion and provides additional benefits, including mechanical support, electrical insulation and protection from mechanical damage [34] Polymeric encapsulants provide the desired isola- tion by bonding to a surface and limiting access to the protected areas or components. For example, encapsu- lants used in PV modules are typically bonded to one or more glass sheets to isolate the solar cells, or cell strings, from water in the module environment. The abil- ity of a polymeric material to protect a surface is thus highly dependent on its ability to bond to a surface and limit access to corrosion sites. A strong correla- tion exists between corrosion protection and adhesive strength [5,6] The dominant encapsulant used in the PV industry is based on a random copolymer consisting of about 67 wt.% polyethylene and 33 wt.% polyvinyl acetate [7]; Polyethylene was chosen because it is very simple and inexpensive polymer. When used alone, however, it is typically an opaque or translucent (depending on the polymerization conditions) semicrystalline polymer with a thermal property too low to protect a PV device. Polyvinyl acetate is a transparent, amorphous polymer, but it has a glass transition temperature (Tg.) of about 35°C; making it too brittle or non-compliant under typ- ical environmental exposure [8], Small amount of vinyl acetate is added to polyethylene to break up the crys- tallites, producing a semicrystalline, highly transparent material The adoption of Ethylene Vinyl Acetate (EVA) as a defacto standard occurred not because it had the best combination of properties, but because it was inexpen- sive and readily available, EVA was designed to be used on the front side of cells where high light transmission is required. It is also routinely on the back side of cells where light transmission is not necessary. In these appli- cations, a white sheet of tedlar (or another reflective material) is commonly laminated to the back to improve performance by reflecting back the light that initially shines between the cells. Over the last several decades EVA has emerged as the dominant encapsulant material used in PV devices; carly modules constructed with EVA demonstrated severe failure within a few years of putting the mod- ules in use because of yellowing of the encapsulant [9]. Improvement to EVA have been developed, includ- ing formulations with antioxidant and ultraviolet (UV) absorbers, that provide encapsulant materials that will not significantly yellow over the 20- to 30-lifeline of a module [10] Despite all these improvements, EVA still has several drawbacks that affect its performance as an encapsulant material, particularly in PV module; for example, EVA suffers from non-ideal mechanical and thermal proper- ties, a high diffusivity of water, and acetic by-product production [11]. The newer thin-film technologies that are rapidly being developed in the PV industry may be more sensitive to the shortcomings of EVA. As crystalline silicon wafers become thinner, the mechan- ical properties of EVA may also prove insufficient. An alternative option would be to use an optically clear sil- ica encapsulant with wide operating temperature range, repairable, ultraviolet stable, weather resistant, flexible and casy to use. As the ability to isolate components and areas from potentially adverse condition is not absolute, there is a continuing need for improved encapsulant materials. A siliceous encapsulant providing even a minimal cost savings is expected to be well-received in the current environment, particularly if the encapsulant also pro- vvides beneficial technical properties. However, since the development of polymer based siliceous particulate com- posite ftom rice husk for solar cell applications looks feasible, a detailed investigation in this direction is there~ fore considered worthwhile. In the previous work [12], sol-gel process for the ‘manufacturing of submicron silica particles from rice husk ash (RHA) was described and the influence of the silica particles on the mechanical properties of High Density Polyethylene was also presented. Energy dis- persive x-ray spectrometer (EDX) as well as scanning electron microscope (SEM) were used to determine the elemental composition and the morphology of the0.0. Daramola etal. / Journal of Taibah University for Science 1] (2017) 645-653, 647 192 3 4 § 6 7 8 8 1 FulScal 10167 cs Crs 1000 ) Fig. 1. EDX spectromettic data of silica extracted from RHA with 20M NOH, powder respectively. The EDX analysis confirmed the presence of silica in the composite to be 96.1%. The powder particle size was also verified by Horiba dynamic particle size analyzer. The average particle size was 0.5 um. The silica powder causes enhancement in the mechanical properties of HDPE up to 4 wt.% This paper presents the influence of agro waste silica particles on the thermal, structural and morphological properties of High Density Polyethylene matrix com- posites 2, Materials and methods 2.1. Materials Fine Silica powder of S00nm average particle size produced from rice husk ash by sol-gel process as described by Daramola et al. [12] were used in this research. The EDX spectrometric data of the silica extracted from RHA with 2.0M NaOH is presented in Fig. 1, Submicron Titania powder particles supplied by Table 1 Proportion ofthe constituents added in gram ‘Alfa Aesar High Purity Research chemicals, Vorna Val- ley, Republic of South Africa (RSA) were utilized as ultraviolet absorber. Maleic anhydride-grafted polyethy- ene (Mape) supplied by Sasol Chemicals, Sasolburg RSA was used as compatibilizer. High Density Polyethy- Tene (HDPE) was supplied in Pellet form by DOW Chemicals, RSA; It has a melt flow index (MFI) of 8 g/10 min (XZ 89712-00 RD, 10140182040), a molec- ular weight of 168,000gmol-", a melting point of 130°C, and a density of 0.954 gem™>. Ethylene-vinyl acetate (EVA), Elvax-220W, with a melt flow index of 150 g/10 min, vinyl acetate content of 30% and density of 0.951 gicm’, supplied by DuPont chemical company was used in this work. 2.2. Method 2.2.1. Compounding of the composite materials Predetermined proportion of HDPE, Silica powder, Titania powder and gafted maleic anhydride polyethy- Jene (Mape) were mixed together in a tumbler mixer for 20min in other to obtain homogeneous mix- ture, Table 1 shows the proportion of the constituents added in grams. Each mixed samples, neat HDPE and EVA (65% HDPE) were melt-blended using a Rapra Single-Screw Exiruder at a temperature of 200-230 °C; (Zonel = 200°C, Zone2=210 °C Zone 3=220°C, Zone 4=230°C) and rotor speed of 40rpm. The extrudates were ground with a grinding machine. 2.2.2. Composites production The ground extrudates were poured in a rectangular mould of dimension 150 x 100 x 4mm. 60 g was used for the rectangular samples. The filled mould was placed in between the lower and the upper plates of the Carver laboratory press at 230 °C for 10 min under applied pres- sure of 0.2 kPa. The materials were then water cooled at 20°C min. In this way, neat HDPE, neat EVA and sub- ‘Sample designation WL OFMAPEG%) wis of TIO; WH Of SiO; Wim of VA HDPE (03%) 468 and 10%) GO) Neat HDPE = = = = 1000 EVA (HDPE/VA) 50g - - 300g 6508 2 wh.% Si0,/TI0,/HDPE. 50g. 3g 20¢ - 9278 4% Si 508, 3g 408 - 907g 6. Si 50g. 3g 608 - 887g 8 wt.% Si02/TI02/HDPE 50g 3g 80g - 867g 10We% Si0p/MOYHDPE 50g 3g 100g = site68 0.0. Daramola etal. / Journal of Taibah University for Science 1] (2017) 645-653 Fig. 2. Plot of TGA Thermograms of neat HDPE, EVA and $i03/T10,/HDPE composites. micron composite samples filled with various volume of silica (2, 4, 6, 8 and 10 wt.%) at constant 5 wt. % Mapp and 0.3 wt.% Titania loading were prepared. Teflon sheet was used to cover the surface of the samples at the top and bottom part of the mould while silicone was sprayed at the inner edges of the mould for easy release after moulding. 2.2.3, Thermogravimetric analysis The thermal stability of neat polymer, EVA and sub- micron composites weighing approximately 10mg were investigated using a thermogravimetric analyzer (TGA). The TGA (Model Q500, TA Instruments, USA) was operated in air at a heating rate of 10°C/min from room temperature to 800°C. 2.2.4, X-ray diffraction spectroscopy (XRD) The crystal structures of neat polymer, EVA and sub- micron composites were studied using wide-angle-X-ray diffraction (WAXD, Pan Analytical Xpert Pro Diffrac~ tometer, The Netherlands) using Cu Ka radiation; with a wavelength of 0.154 nm, at a voltage of 4SKV and a current of 40mA. 2.2.5. Scanning electron microscopy (SEM) The surface morphology of the samples was stud- ied using an AURIGA scanning electron microscopy (SEM) (Carl Zeiss, Germany) with an accelerating volt- age of ISKV. The notched impact fractured surfaces were mounted on aluminium stubs and were sputter coated with gold using EMITECH K950X sputter coater and were subjected to SEM analysis. man Neat nore 5 Soateznore Fig. 3. Plot of 5% degradation temperature of neat HDPE, EVA and, he developed composites. 3. Results and discussion 4.1. Thermogravimetric analysis (TGA) of the composites The results of the thermal-oxidation degradation anal- ysis of the neat HDPE, EVA and the siliceous HDPE composites are presented in Figs. 2-6 while Table 2 shows the thermo-oxidative parameters of all samples calculated from TGA and presented as a function of SiO» which summarizes the TGA data which include degradation temperature, Ts, at which 5% weight loss occurted, Tyo, at which 10% weight loss occurred, Tmax, ‘maximum temperature at which maximum degradation (50%) occurred and the percentage char at 500°C which is the residue/left over of the materials. At a tempera-0.0. Daramola etal. / Journal of Taibah University for Science 1] (2017) 645-653, 649 Table 2 ‘Therme-oxidative parameters ofall samples calculated from TGA and presented as a function of % SiO. ‘Sample designation Beo, TCO Ths CO) Wise Neat HDPE 364 3500 389.09 429.2700 2.8740 EVA 282.5000 29458 413.1600 0.0000 2w1.%$103/T102/HDPE 360.2100 383.78 415.5600 5.5390 491. %8102/T102/HDPE 378.0800 399.91 430.3400 68510 6 wt. %8102/T1O,/HDPE 365.3100 394.37 430.5300 6.7760 8. %8i0,/T10,/HDPE 382.3800 405.21 434.6800 6.0030 10 we %Si02/1103/HDPE 377.0500 40082 438.7300 12,3000 ‘Ty is the degradation temperature at 5% weight los, To is the degradation maximum degradation rate occuss, and Wer i the % ash at 500°C, Fig. 4, Plot of 10% degradation temperature of neat HDPE, EVA and, the developed composites. Nest HDPE Fig. 5. Plot of 50% degradation temperature of neat HDPE, EVA and, the developed composites. ture of 282.50°C, EVA have degraded by 5%, HDPE degraded by 5% at 360.21 °C; the optimum 5% degra- dation temperature of the developed siliceous composite Temperature at 10% weightloss, Tyra is the temperature at which the ZZZZLL WLLLLLLLLA Fig. 6. Plot of percentage char of neat HDPE, EVA and the developed, composites. is 382.38 °C which is a composite with 6 wt% silica, The residue left after combustion of neat HDPE and EVA are 2.874% and 0% respectively. Fig. 2 presents the plot of the thermograms of EVA, Neat HPDE and SiO;/TiO:/HDPE Composites which shows the degradation patterns of the materials in each ‘gtoup, with those of neat HDPE and EVA included. The results presented in Figs. 3 and 4 show the plots of 5% and 10% degradation temperature of neat HDPE, EVA and the developed composites respectively which indi- cate that the siliceous composites developed exhibited higher thermal stability than the neat HDPE and EVA. ‘The better thermal stability observed in the composites developed is as result of the presence of silica which is a material that can operate over a wide range of temper- ature [13] The results presented in Fig. 5 is the plot of maxi- ‘mum degradation (50%) of neat HDPE, EVA, and the developed composites which indicates that the thermal stability of the composites increase linearly with increase in silica content for Si0;/HDPE composites. One expla- nation for this is that inorganic substances possess high thermal stability; they act as heat barriers and retard volatilization [14,15]. Therefore, the addition of silica650 0.0. Daramola etal. / Journal of Taibah University for Science 1] (2017) 645-653 Intra fas) 2 theta) Fig. 7, XRD pattems of neat HDPE, EVA and SiO,/Ti0,/HDPE com- posites. particulate clearly improved the thermal stability of the materials. The maximum degradation temperature of the siliceous composites is at 10 w1.% silica with a value of 382,38°C, The plot of the percentage char of EVA, neat HDPE, and the developed composites which is the residue left after combustion of the composite at 500°C is presented in Fig. 6, The results clearly showed that EVA had totally degraded at this temperature while neat HDPE was left with 2.874%. The optimum percentage char is 12.30% which is the composite with 10 wt.% silica. The values of percentage char for other composites are shown in Table 2, 3.2. Crystal structure based on wide angle X-ray diffraction (WAXD) analysis The XRD pattems of neat HDPE, EVA and SiO,/Ti02/HDPE composites are shown in Fig. 7. The diffraction angles, the corresponding interplanar dis- tance of EVA, neat HDPE and the composites together with their lateral crystal size are shown in Table 3. ‘Two obvious diffractive peaks of about 21.3° and 23.7° corresponding to typical crystal plane (1 1 0), and (2.00) of orthorhombic phase respectively were discov ered, There is no much difference in the interplanar distance (d-value) which represents the lattice param- eter of the neat HDPE and the developed composites which proves that the lattice parameter is not affected by the presence of silica particles. Moreover, the diffractive peaks do not shift with the addition of silica particles. This clearly indicates the unchanged crystal structure of HDPE which shows that the addition of silica particles did not exert much effect on the crystalline structure of HDPE Lamellar thickness (L) of HDPE increases with the addition of silica particles, which implies that silica aid, the formation of more perfect crystals. This can be attributed to the fact that silica particles act as heteroge- neous nucleating agent inducing HDPE to form perfect and stable crystals [16] 3.3. SEM images of the composites A detailed investigation of the filler morphology within the matrix is a key parameter to impart desired mechanical properties of polymer-based composites. To have a clear images of the fractured patterns of the com- posites, SEM images of the notched impact fractured surfaces of neat HDPE, EVA and the developed compos- ites at different filler contents are shown in Fig. 8(a-g). Fig. 8(@) revealed the notched impact fractured surface image of neat HDPE which has a relatively smooth fractured surface in association with terraced markings, indicating weak resistance to crack propagation [17] Some agglomerated particles were seen on the SEM image of EVA. In the case of SiOz/TiOz/HDPE compos- ites with silica content of 2-4 wt.%, it is very clear that there is good dispersion of filler in HDPE matrix. The particles were uniformly distributed in the matrix with little agglomerates as shown in Fig. 8(cand d). When the content of submicron silica approaches 6 wt.%, the mor- phologies of the composites fractured surfaces become somewhat different as shown in Fig. 8(e-g); a number of cavities appear on the surface of SiO,/TiO;/HDPE composites. These cavities as illustrated by the arrows in Fig, 8(¢-g) are produced due to the debonding of the silica particles [18]. In general, an increased content of SiOz would lead to a larger agglomerates because of the formation of hydrogen bonds among the abundant hydroxyl groups and adsorbed water on their surface and hence greater probability of debonding due to the poor interfacial adhesion |15.19] as there is not enough time for inducing matrix yielding after excessive parti- cles debonding, the matrix beside the cavities seems tobe rather flat; this coincides with the reduction of toughness of Si0;/HDPE composites at high SiO> loading 4. Conclusion The following conclusions are drawn from the present work: i, The siliceous composites developed exhibited higher thermal stability than the neat HDPE and EVA.0.0. Daramola etal. / Journal of Taibah University for Science 1] (2017) 645-653 651 Agglomerated lad lall cy Taeiarlac} iw a Ce Rie Pd gittecias ; debonding at the interface Fig. 8. SEM images of (a) neat HDPE, (b) EVA, (¢) 2wt.% Si03/TIO3/HDPE, (8) 4 wt.% Si03/TIOs/HDPE, (¢) 6 wt. % Si03/TIO3/HDPE, (f) 8% SiO2/TOy/HDPE, (g) 10 we % Si0,/TIOy/HDPE, The better thermal stability observed in the com- posites developed is as result of the presence of silica which is a material that can operate over a wide range of temperature. The thermal stability ‘of the composites increase linearly with increase in silica content for $i0;/TiO/HDPE composites; this is as result of the presence of inorganic sub- stances which possess high thermal stability; they act as heat barriers and retard volatilization. The addition of silica particulate clearly improved the thermal stability of the materials. The optimum, degradation temperature of the siliceous compos-652 0.0. Daramola etal. / Journal of Taibah University for Science 1] (2017) 645-653 ‘Table 3 Diffraction angle and the corresponding interplanar distance and lateral crystal sizeof the Composites ‘Sample designation 28 Ono 20 haw auo(am Pe) atom) Lot) Neat HDPE 21227 23.576 oais was 0377 40.880 EVA 23578 25.401 0377 39.618 0350 37300 2wit.568i0/T0,/HDPE 21282 23.635 ois 44.340 0374 37708 44. 9810/T10,/DPE 21573 2392 oais 53.788 0374 42282 60. $810,710 /HDPE 21174 23527 019 53.990 0379 47.670 {. 968i0,/T10,/HDPE 21.399 23.783 oa 57.000 oan 49732 10wt.%8i0,/T10,/HDPE, 2uaiT 23.768 oat 62.690 0376 52.636 ites is at 10 wt.% silica with a value of 438.73°C. ‘The percentage char of the composites which is the residue left after combustion of the compos- ite at 500°C clearly showed that EVA had totally degraded at this temperature while neat HDPE was left with 2.874%. The optimum percentage char is 12.30% which is the composite with 10wt.% sil- ica fi, The crystal structure of EVA, neat HDPE, and the siliceous composites developed were investigated Fig. 7 shows the XRD Patterns of Neat HDPE, EVA, and the siliceous Composites. The diffraction angles and the corresponding interlayer spacing and lat- eral crystal sizes of the composites are shown in ‘Table 5, The erystal structure of EVA, neat HDPE, and the siliceous composites developed revealed two obvious diffractive peaks of about 21.3° and 23.7° corresponding to typical erystal plane (110), and (2.00) of orthorhombic phase respectively. There is no much difference in the interplanar distance (d- value) which represents the lattice parameter of the neat HDPE and the developed composites which proves thatthe lattice parameter is not affected by the presence of silica particles. Moreover, the diffractive peaks do not shift with the addition of silica par ticles. This clearly indicates the unchanged crystal structure of HDPE which shows that the addition of silica particles did not exert much effect on the crys- talline structure of HDPE, Lamellar thickness (L) of HDPE increases with the addition of silica parti- cles, which implies that silica aids the formation of more perfect crystals. This can be attributed to the factthat silica particles act as heterogeneous nucleat- ing agent inducing HDPE to form perfect and stable crystals. iii, From fracture surface analysis, it is clear that sil- ica submicron particles, homogeneously dispersed inHDPEat lower weight percent loading as observed from white zones on the SEM images of the notched impact fractured surfaces of the compos- ites. Acknowledgements We appreciate the following organizations for their support and contributions. They are; (a) Tertiary Education Trust Fund (TETFUND), Nigeria. (b) The Federal University of Technology, Akure, Nigeria. 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