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PublicationBonding strength characteristics of FA-based geopolymer paste as a repair material when applied on OPC substrate( 2020)
;Warid Wazien Ahmad Zailani ;Aissa Bouaissi ;Sorachon Yoriya ;Mohd Remy Rozainy M. A. Z.Hamzah FansuriThis investigative study aims to study the mechanical and morphological properties of fly ash (FA)-based geopolymer paste as a repair material when applied on ordinary Portland cement (OPC) overlay concrete. The first part of this study investigates the optimal mix design of FA-based geopolymer paste with various NaOH concentrations of 8, 10, 12, and 14 M, which were used later as a repair material. The second part studies the bonding strength using a slant shear test between the geopolymer repair material and OPC substrate concrete. The results showed that a shorter setting time corresponds to the higher NaOH molarity, within the range of 53 and 30 min at 8 and 14 M, respectively. The compressive strength of FA-based geopolymer paste was found to reach 92.5 MPa at 60 days. Also, from the slant shear test results, prism specimens with 125 mm length and 50 mm wide have a large bond strength of 11 MPa at 12 M. The scanning electron microscopy/energy-dispersive X-ray (SEM/EDX) analysis showed that the OPC substrate has a significant effect on slant shear bond strength, where the presence of free cations of Ca2+ on the OPC substrate surface contributed to the formation of calcium alumina-silicate hydrate gel (C-A-S-H) by building various cross-links of Ca-O-Si.19 11 -
PublicationCharacterisation at the bonding zone between fly ash based Geopolymer Repair Materials (GRM) and Ordinary Portland Cement Concrete (OPCC)( 2020)
;Warid Wazien Ahmad Zailani ;Mohd Fadzil Arshad ;Remy Rozainy Mohd Arif Zainol ;Marcin Nabialek ;Andrei Victor Sandu ;Jerzy J. WysłockiKatarzyna BłochIn recent years, research and development of geopolymers has gained significant interest in the fields of repairs and restoration. This paper investigates the application of a geopolymer as a repair material by implementation of high-calcium fly ash (FA) as a main precursor, activated by a sodium hydroxide and sodium silicate solution. Three methods of concrete substrate surface preparation were cast and patched: as-cast against ordinary Portland cement concrete (OPCC), with drilled holes, wire-brushed, and left as-cast against the OPCC grade 30. This study indicated that FA-based geopolymer repair materials (GRMs) possessed very high bonding strength at early stages and that the behavior was not affected significantly by high surface treatment roughness. In addition, the investigations using scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) spectroscopy have revealed that the geopolymer repair material became chemically bonded to the OPC concrete substrate, due to the formation of a C–A–S–H gel. Fundamentally, the geopolymer network is composed of tetrahedral anions (SiO4)4− and (AlO4)5− sharing the oxygen, which requires positive ions such as Na+, K+, Li+, Ca2+, Na+, Ba2+, NH4+, and H3O+. The availability of calcium hydroxide (Ca(OH)2) at the surface of the OPCC substrate, which was rich in calcium ions (Ca2+), reacted with the geopolymer; this compensated the electron vacancies of the framework cavities at the bonding zone between the GRM and the OPCC substrate.8 14 -
PublicationComparison of thermal performance between fly ash geopolymer and fly ash-ladle furnace slag geopolymer( 2022-06-01)
;Ng Hui Teng ;Pakawanit P. ;Bayuaji R. ;Ng Yong Sing ;Khairunnisa Zulkifly ;Ooi Wan En ;Hang Yong JieOng Shee WeenThis paper compared the thermal stability between fly ash (FA) and fly ash-ladle furnace slag (FA-LS) geopolymers. FA-LS geopolymer was prepared by mixing FA and LS (FA:LS weight ratio of 80:20) with an alkali activator. Geopolymers were aged at room temperature for 28 days before being exposed to high temperatures (200 °C – 1000 °C). Unexposed FA and FA-LS geopolymers had a compressive strength of 38.9 MPa and 40.5 MPa, respectively. The FA and FA-LS geopolymers retained 61.6% and 91.3% compressive strength, respectively, when exposed to temperatures up to 1000 °C. FA-LS geopolymers experienced smaller variation in the density (2.6 – 5.5%) and pores (17.4 – 23.0%) compared to FA geopolymers (density and porosity of 2.9 – 25.2% and 19.0 – 30.0%, respectively). The formation of crystalline peaks, densification of matrix, pores and their connectivity, cracks and dimensional changes influenced the compressive strength of exposed geopolymers. FA-LS geopolymers could be potentially applied as heat-resistance material.1 5 -
PublicationComparison of thermal performance between fly ash geopolymer and fly ash-ladle furnace slag geopolymer( 2022-06-01)
;Ng Hui Teng ;Pakawanit P. ;Bayuaji R. ;Ng Yong Sing ;Khairunnisa Zulkifly ;Ooi Wan En ;Hang Yong JieOng Shee WeenThis paper compared the thermal stability between fly ash (FA) and fly ash-ladle furnace slag (FA-LS) geopolymers. FA-LS geopolymer was prepared by mixing FA and LS (FA:LS weight ratio of 80:20) with an alkali activator. Geopolymers were aged at room temperature for 28 days before being exposed to high temperatures (200 °C – 1000 °C). Unexposed FA and FA-LS geopolymers had a compressive strength of 38.9 MPa and 40.5 MPa, respectively. The FA and FA-LS geopolymers retained 61.6% and 91.3% compressive strength, respectively, when exposed to temperatures up to 1000 °C. FA-LS geopolymers experienced smaller variation in the density (2.6 – 5.5%) and pores (17.4 – 23.0%) compared to FA geopolymers (density and porosity of 2.9 – 25.2% and 19.0 – 30.0%, respectively). The formation of crystalline peaks, densification of matrix, pores and their connectivity, cracks and dimensional changes influenced the compressive strength of exposed geopolymers. FA-LS geopolymers could be potentially applied as heat-resistance material.1 -
PublicationEffect of NaOH molar concentration on microstructure and compressive strength of Dolomite/Fly Ash-Based geopolymers( 2021)
;Emy Aizat Azimi ;M.A.A. Mohd Salleh ;Ikmal Hakem A. Aziz ;Jitrin Chaiprapa ;Petrica Vizureanu ;Sorachon Yoriya ;Marcin NabiałekJerzy J. WyslockiDolomite can be used as a source of aluminosilicate to produce geopolymers; however, this approach is limited by its low reactivity. This study analyzes the viability of producing geopolymers using dolomite/fly-ash with sodium silicate and NaOH solutions (at multiple concentrations) by determining the resultant geopolymers’ compressive strengths. The dolomite/fly-ash-based geopolymers at a NaOH concentration of ~22 M resulted in an optimum compressive strength of 46.38 MPa after being cured for 28 days, and the SEM and FTIR analyses confirmed the denser surface of the geopolymer matrix. The synchrotron micro-XRF analyses confirmed that the Ca concentration exceeded that of Si and Mg, leading to the formation of calcium silicate hydrate, which strengthens the resulting geopolymers. -
PublicationEffect of Naoh Molar Concentration on Microstructure and Compressive Strength of Dolomite/Fly Ash-Based Geopolymers( 2022-01-01)
;Emy Aizat Azimi ;Ikmal Hakem Abdul Aziz ;Chaiprapa J. ;Vizureanu P. ;Yoriya S. ;Nabialek M.Wyslocki J.J.Dolomite can be used as a source of aluminosilicate to produce geopolymers; however, this approach is limited by its low reactivity. This study analyzes the viability of producing geopolymers using dolomite/fly-ash with sodium silicate and NaOH solutions (at multiple concentrations) by determining the resultant geopolymers' compressive strengths. The dolomite/fly-ash-based geopolymers at a NaOH concentration of ∼22 M resulted in an optimum compressive strength of 46.38 MPa after being cured for 28 days, and the SEM and FTIR analyses confirmed the denser surface of the geopolymer matrix. The synchrotron micro-XRF analyses confirmed that the Ca concentration exceeded that of Si and Mg, leading to the formation of calcium silicate hydrate, which strengthens the resulting geopolymers.2 -
PublicationEffect of silica fume and alumina addition on the mechanical and microstructure of fly ash geopolymer concrete( 2022-01-01)
;Min Fong Sue ;Razi H.M. ;Low F.W. ;Ng Hui TenNg Yong SinThis paper discussed the effect of the addition of silica fume (2 wt.% and 4 wt.%) and alumina (2 wt.% and 4 wt.%) on the properties of fly ash geopolymer concrete. The fly ash geopolymer concrete achieved the highest 28-day compressive strength with 2 wt.% of silica fume (39 MPa) and 4 wt.% of alumina (41 MPa). The addition of 2 wt.% of silica fume increased the compressive strength by 105% with respect to the reference geopolymer (without additive). On the other hand, the compressive strength surged by 115% with 4 wt.% of alumina compared to the reference geopolymer. The addition of additives improved the compactness of the geopolymer matrix according to the morphology analysis.1 -
PublicationEFFECT OF SILICA FUME AND ALUMINA ADDITION ON THE MECHANICAL AND MICROSTRUCTURE OF FLY ASH GEOPOLYMER CONCRETE( 2022-01-01)
;Min Fong Sue ;Razi H.M. ;Low F.W. ;Ng Hui TenNg Yong SinThis paper discussed the effect of the addition of silica fume (2 wt.% and 4 wt.%) and alumina (2 wt.% and 4 wt.%) on the properties of fly ash geopolymer concrete. The fly ash geopolymer concrete achieved the highest 28-day compressive strength with 2 wt.% of silica fume (39 MPa) and 4 wt.% of alumina (41 MPa). The addition of 2 wt.% of silica fume increased the compressive strength by 105% with respect to the reference geopolymer (without additive). On the other hand, the compressive strength surged by 115% with 4 wt.% of alumina compared to the reference geopolymer. The addition of additives improved the compactness of the geopolymer matrix according to the morphology analysis.3 -
PublicationEffect of Sodium Aluminate on the Fresh and Hardened Properties of Fly Ash-Based One-Part Geopolymer( 2022-01-01)
;Wan-En O. ;Ong Shee WeenSandu A.V.The one-part geopolymer binder was synthesis from the mixing of aluminosilicate material with solid alkali activators. The properties of one-part geopolymers vary according to the type and amount of solid alkali activators used. This paper presents the effect of various sodium metasilicate-to-sodium aluminate (NaAlO2/Na2SiO3) ratios on fly ash-based one-part geopolymer. The NaAlO2/Na2SiO3 ratios were set at 1.0 to 3.0. Setting time of fresh one-part geopolymer was examined through Vicat needle apparatus. Mechanical and microstructural properties of developed specimens were analysed after 28 days of curing in ambient condition. The study concluded that an increase in NaAlO2 content delayed the setting time of one-part geopolymer paste. The highest compressive strength was achieved at the NaAlO2/Na2SiO3 ratio of 2.5, which was 33.65 MPa. The microstructural analysis revealed a homogeneous structure at the optimum ratio. While the sodium aluminium silicate hydrate (N-A-S-H) and anorthite phases were detected from the XRD analysis.5 -
PublicationEffect of Sodium Aluminate on the Fresh and Hardened Properties of Fly Ash-Based One-Part Geopolymer( 2022-01-01)
;Ooi Wan En ;Ong Shee WeenSandu A.V.The one-part geopolymer binder was synthesis from the mixing of aluminosilicate material with solid alkali activators. The properties of one-part geopolymers vary according to the type and amount of solid alkali activators used. This paper presents the effect of various sodium metasilicate-to-sodium aluminate (NaAlO2/Na2SiO3) ratios on fly ash-based one-part geopolymer. The NaAlO2/Na2SiO3 ratios were set at 1.0 to 3.0. Setting time of fresh one-part geopolymer was examined through Vicat needle apparatus. Mechanical and microstructural properties of developed specimens were analysed after 28 days of curing in ambient condition. The study concluded that an increase in NaAlO2 content delayed the setting time of one-part geopolymer paste. The highest compressive strength was achieved at the NaAlO2/Na2SiO3 ratio of 2.5, which was 33.65 MPa. The microstructural analysis revealed a homogeneous structure at the optimum ratio. While the sodium aluminium silicate hydrate (N-A-S-H) and anorthite phases were detected from the XRD analysis.2 -
PublicationEffect of sodium hydroxide molarity on physical, mechanical and thermal conductivity of metakaolin geopolymersIn the present work, the effect of different sodium hydroxide (NaOH) molarity (6M, 8M, 10M, 12M and 14M) on the physical, mechanical and thermal conductivity of metakaolin geopolymers (MkGPs) was investigated. Geopolymers were prepared by activating the metakaolin with a mixture of NaOH with sodium silicate (Na2SiO3). The products obtained were characterized after 28 days of curing. The density, porosity, compressive strength and thermal conductivity (TC) were determined. In general, the NaOH molarity has a significant effect on the compressive strength of the MkGPs. The highest compressive strength was 14.6 MPa achieved with 10M of NaOH solution. The thermal conductivity of MkGPs measured in this work was low in the range between 0.71-0.97 W/mK. NaOH molarity had a significant effect on compressive strength but a marginal effect on thermal conductivity of MkGPs. The thermal conductivity was mainly affected by the bulk density and thus the total porosity. The results showed that the geopolymer can be considered to be used as the thermal insulating material.
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PublicationElectrical Performance of Curcuma longa Extract Dye using SnO2-Based Photoanode Dye-Sensitized Solar Cell( 2022-12-01)
;Siti Norhafizah Idris ;Magiswaran K.Abas Z.A.Due to their low output costs, straightforward manufacturing, and high effectiveness, dye-sensitized solar cell (DSSC) has a large following interest in the solar energy industry. Furthermore, due to its outstanding properties, tin oxide (SnO2) is an appealing semiconducting material suitable as a photoanode in DSSCs. In this research, the photoelectrodes of DSSC were fabricated using commercial SnO2 nanoparticles and sensitized with inorganic and organic dyes, N719 and Curcuma longa (turmeric) extract dye. On top of that, a platinum (Pt) counter electrode, iodide electrolyte and fluorine-doped tin oxide (FTO) coated glass substrate were used to fabricate the DSSC. The crystallographic structure and surface morphology of the SnO2 nanopowder were identified using X-ray diffraction (XRD) and scanning electron microscopy (SEM) characterizations respectively. In addition, UV-Visible and current density-voltage curves were used to analyze the optical properties of the photoanodes and the cell’s electrical performance. As a result, it was found that the DSSC fabricated with N719 dye exhibited higher efficiency in contrast with the turmeric extract dye with SnO2 photoanodes.1 -
PublicationFINITE ELEMENT ANALYSIS ON STRUCTURAL BEHAVIOUR OF GEOPOLYMER REINFORCED CONCRETE BEAM USING JOHNSON-COOK DAMAGE IN ABAQUS( 2022-01-01)
;Noorfifi Natasha Shahedan ;Li L.Y.Ikmal Hakem Abdul AzizThis paper details a finite element analysis of the behaviour of Si-Al geopolymer concrete beam reinforced steel bar under an impulsive load and hyper velocity speed up to 1 km/s created by an air blast explosion. The initial torsion stiffness and ultimate torsion strength of the beam increased with increasing compressive strength and decreasing stirrup ratio. The study involves building a finite element model to detail the stress distribution and compute the level of damage, displacement, and cracks development on the geopolymer concrete reinforcement beam. This was done in ABAQUS, where a computational model of the finite element was used to determine the elasticity, plasticity, concrete tension damages, concrete damage plasticity, and the viability of the Johnson-Cook Damage method on the Si-Al geopolymer concrete. The results from the numerical simulation show that an increase in the load magnitude at the midspan of the beam leads to a percentage increase in the ultimate damage of the reinforced geopolymer beams failing in shear plastic deformation. The correlation between the numerical and experimental blasting results confirmed that the damage pattern accurately predicts the response of the steel reinforcement Si-Al geopolymer concrete beams, concluded that decreasing the scaled distance from 0.298 kg/m3 to 0.149 kg/m3 increased the deformation percentage.1 -
PublicationFinite element analysis on structural behaviour of geopolymer reinforced concrete beam using Johnson-Cook Damage in ABAQUS( 2022)
;Rafiza Abdul Razak ;Noorfifi Natasha Shahedan ;Long Yuan LiIkmal Hakem A. AzizThis paper details a finite element analysis of the behaviour of Si-Al geopolymer concrete beam reinforced steel bar under an impulsive load and hyper velocity speed up to 1 km/s created by an air blast explosion. The initial torsion stiffness and ultimate torsion strength of the beam increased with increasing compressive strength and decreasing stirrup ratio. The study involves building a finite element model to detail the stress distribution and compute the level of damage, displacement, and cracks development on the geopolymer concrete reinforcement beam. This was done in ABAQUS, where a computational model of the finite element was used to determine the elasticity, plasticity, concrete tension damages, concrete damage plasticity, and the viability of the Johnson-Cook Damage method on the Si-Al geopolymer concrete. The results from the numerical simulation show that an increase in the load magnitude at the midspan of the beam leads to a percentage increase in the ultimate damage of the reinforced geopolymer beams failing in shear plastic deformation. The correlation between the numerical and experimental blasting results confirmed that the damage pattern accurately predicts the response of the steel reinforcement Si-Al geopolymer concrete beams, concluded that decreasing the scaled distance from 0.298 kg/m3 to 0.149 kg/m3 increased the deformation percentage.11 3 -
PublicationFlexural Properties of Thin Fly Ash Geopolymers at Elevated Temperature( 2022-01-01)
;Ng Yong Sing ;Ng Hui TengChan L.W.L.This paper reports on the flexural properties of thin fly ash geopolymers exposed to elevated temperature. The thin fly ash geopolymers (dimension = 160 mm × 40 mm × 10 mm) were synthesised using12M NaOH solution mixed with designed solidsto- liquids ratio of 1:2.5 and Na2SiO3/NaOH ratio of 1:4 and underwent heat treatment at different elevated temperature (300°C, 600°C, 900°C and 1150°C) after 28 days of curing. Flexural strength test was accessed to compare the flexural properties while X-Ray Diffraction (XRD) analysis was performed to determine the phase transformation of thin geopolymers at elevated temperature. Results showed that application of heat treatment boosted the flexural properties of thin fly ash geopolymers as the flexural strength increased from 6.5 MPa (room temperature) to 16.2 MPa (1150°C). XRD results showed that the presence of crystalline phases of albite and nepheline contributed to the increment in flexural strength.4 1 -
PublicationFlexural Properties of Thin Fly Ash Geopolymers at Elevated Temperature( 2022-01-01)
;Ng Yong Sing ;Ng Hui TengChan L.W.L.This paper reports on the flexural properties of thin fly ash geopolymers exposed to elevated temperature. The thin fly ash geopolymers (dimension = 160 mm × 40 mm × 10 mm) were synthesised using12M NaOH solution mixed with designed solidsto- liquids ratio of 1:2.5 and Na2SiO3/NaOH ratio of 1:4 and underwent heat treatment at different elevated temperature (300°C, 600°C, 900°C and 1150°C) after 28 days of curing. Flexural strength test was accessed to compare the flexural properties while X-Ray Diffraction (XRD) analysis was performed to determine the phase transformation of thin geopolymers at elevated temperature. Results showed that application of heat treatment boosted the flexural properties of thin fly ash geopolymers as the flexural strength increased from 6.5 MPa (room temperature) to 16.2 MPa (1150°C). XRD results showed that the presence of crystalline phases of albite and nepheline contributed to the increment in flexural strength.1 -
PublicationImprovements of Flexural Properties and Thermal Performance in Thin Geopolymer Based on Fly Ash and Ladle Furnace Slag Using Borax Decahydrates( 2022-06-01)
;Ng Yong-Sing ;Pakawanit P. ;Vizureanu P. ;Khalid M.S. ;Ng Hui-Teng ;Hanh Yong-Jie ;Nabiałek M. ;Pietrusiewicz P. ;Garus S. ;Sochacki W.Śliwa A.This paper elucidates the influence of borax decahydrate addition on the flexural and thermal properties of 10 mm thin fly ash/ladle furnace slag (FAS) geopolymers. The borax decahydrate (2, 4, 6, and 8 wt.%) was incorporated to produce FAB geopolymers. Heat treatment was applied with temperature ranges of 300◦C, 600◦C, 900◦C, 1000◦C and 1100◦C. Unexposed FAB geopolymers experienced a drop in strength due to a looser matrix with higher porosity. However, borax decahydrate inclusion significantly enhanced the flexural performance of thin geopolymers after heating. FAB2 and FAB8 geopolymers reported higher flexural strength of 26.5 MPa and 47.8 MPa, respectively, at 1000◦C as compared to FAS geopolymers (24.1 MPa at 1100◦C). The molten B2O3 provided an adhesive medium to assemble the aluminosilicates, improving the interparticle connectivity which led to a drastic strength increment. Moreover, the borax addition reduced the glass transition temperature, forming more refractory crystalline phases at lower temperatures. This induced a significant strength increment in FAB geopolymers with a factor of 3.6 for FAB8 at 900◦C, and 4.0 factor for FAB2 at 1000◦C, respectively. Comparatively, FAS geopolymers only achieved 3.1 factor in strength increment at 1100◦C. This proved that borax decahydrate could be utilized in the high strength development of thin geopolymers.1 -
PublicationImprovements of Flexural Properties and Thermal Performance in Thin Geopolymer Based on Fly Ash and Ladle Furnace Slag Using Borax Decahydrates( 2022-06-01)
;Ng Yong-Sing ;Pakawanit P. ;Vizureanu P. ;Khalid M.S. ;Ng Hui-Teng ;Yong-Jie H. ;Nabiałek M. ;Pietrusiewicz P. ;Garus S. ;Sochacki W.Śliwa A.This paper elucidates the influence of borax decahydrate addition on the flexural and thermal properties of 10 mm thin fly ash/ladle furnace slag (FAS) geopolymers. The borax decahydrate (2, 4, 6, and 8 wt.%) was incorporated to produce FAB geopolymers. Heat treatment was applied with temperature ranges of 300◦C, 600◦C, 900◦C, 1000◦C and 1100◦C. Unexposed FAB geopolymers experienced a drop in strength due to a looser matrix with higher porosity. However, borax decahydrate inclusion significantly enhanced the flexural performance of thin geopolymers after heating. FAB2 and FAB8 geopolymers reported higher flexural strength of 26.5 MPa and 47.8 MPa, respectively, at 1000◦C as compared to FAS geopolymers (24.1 MPa at 1100◦C). The molten B2O3 provided an adhesive medium to assemble the aluminosilicates, improving the interparticle connectivity which led to a drastic strength increment. Moreover, the borax addition reduced the glass transition temperature, forming more refractory crystalline phases at lower temperatures. This induced a significant strength increment in FAB geopolymers with a factor of 3.6 for FAB8 at 900◦C, and 4.0 factor for FAB2 at 1000◦C, respectively. Comparatively, FAS geopolymers only achieved 3.1 factor in strength increment at 1100◦C. This proved that borax decahydrate could be utilized in the high strength development of thin geopolymers.1 -
PublicationInfluence of ZnO Nanoparticles on Mechanical Properties and Photocatalytic Activity of Self-cleaning ZnO-Based Geopolymer Paste( 2020-06-01)
;Siti Norsaffirah Zailan ;Bouaissi, AissaAbstract: The influence of zinc oxide (ZnO) nanoparticles on the mechanical properties and photocatalytic degradation of methylene blue (MB) of ZnO-based geopolymer material was investigated under the illumination of ultraviolet (UV) radiations. In this work, ZnO-based geopolymer paste was manufactured using class F fly ash (FA) and ZnO nanoparticles powders with different mass percentages (0, 2.5, 5.0, 7.5 and 10 wt%). The FA-ZnO dry mix was activated by alkaline activator solution made from sodium silicate and sodium hydroxide with a ratio of 2.5. The mechanical properties were investigated by performing a compressive strength test at 28 days. The photocatalytic activity of ZnO nanoparticles was evaluated by measuring the photodegradation level of methylene blue under sunlight rays. The results showed a substantial influence of ZnO on the compressive strength, which decreased with the increase of ZnO amounts ranging from 2.5 to 7.5 wt% then a slightly increased at 10 wt% of ZnO. The addition of ZnO nanoparticles to a geopolymeric material showed a satisfactory efficiency of photocatalytic degradation of methylene blue after 150 min of exposure to sunlight. Phase analysis revealed that the addition of ZnO nanoparticles in the geopolymeric system develops a new ZnO crystalline phases. Graphic Abstract: [Figure not available: see fulltext.].4 5 -
PublicationInsight on the structural aspect of ENR-50/TiO2 hybrid in KOH/C3H8O medium revealed by NMR spectroscopy( 2020-01-01)
;Dahham O.S. ;Abu Bakar M. ;Alakrach A.M.Al-rashdi A.A.The ring-opening reactions (ROR) of epoxide groups in epoxidized natural rubber/titania (ENR-50/TiO2) hybrid in potassium hydroxide/isopropanol medium were examined using NMR spectroscopy and supported by the FTIR technique. The thermal behaviour of the hybrid was also studied using TG/DTG and DSC analyses. The 1H NMR results suggested that 16.82% of ROR occurred in the hybrid, while the 13C NMR results exhibited five new peaks at δ 19.5, 71.0, 73.7, 91.7 and 94.4 ppm in the hybrid. 2D NMR, such as HMQC, HMBC and COSY techniques, further scrutinized these assignments. The FTIR spectrum exhibited Ti-O-C characteristics via the peak at 1028 cm−1. The TG/DTG results showed four steps of thermal degradation at 44–148, 219–309, 331–489 and 629–810 °C due to the existence of Ti moieties along with a polymer chain mixture (intact and ring-opened epoxide groups) of ENR-50, which in turn led to an increase in the Tg value of the hybrid to 27 °C compared to that of purified ENR-50 at −17.72 °C.1