Hybrid composites of polypropylene (PP)/nanoclay (NC)/glass fiber (GF) were prepared byextrusion and injection molding. Molded specimens were analyzed by transmission electron microscopy (TEM), thermogravimetric analysis (TGA), tensile and flexural tests. TEM results revealed NC particle intercalation. TGA results showed that the incorporation of clay into the GF composite improves the thermal stability of the material. The initial thermal decomposition temperatures also shifted to higher values. Incorporation of GF into PP lowers the tensile strength of the binary composite, indicating poor fiber-matrix interfacial adhesion. However, introducing NC increased the strength of the ternary composites. Tensile modulus was enhanced with the incorporation of GF and further increased with an introduction of NC. Flexural strength and flexural modulus are both enhanced with an increase in GF and NC loading.
The magnetic adsorbents i.e. oil palm frond-magnetic particles (OPF-MP) and oil palm frond activated carbon-magnetic particles (OPFAC-MP) have been prepared by impregnation of iron oxide via co-precipitation method. The magnetic adsorbents and their parent materials were characterized using Fourier transform infrared (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), Brunauer Emmett Teller (BET), Barrett, Joyner & Halenda (BJH) and t-plot method, x-ray diffraction (XRD) and also using vibrating sample magnetometry (VSM) to study their properties and surface chemistry. The activated carbon magnetic adsorbent confers high surface area of 700 m2/g with amorphous structure and magnetic properties of 2.76 emu/g. The OPF-MP and OPFAC-MP were then applied in adsorption study for ions removal of Pb(II), Zn(II) and Cu(II). OPFAC-MP has shown high removal efficiency of 100 % with adsorption capacity up to 15 mg/g of Pb(II), Zn(II) and Cu(II) ions compared to OPF-MP. In addition, the magnetic adsorbents were also compared with their parent materials to observe the effect of magnetic particles. Accordingly, the impregnation of magnetic particles enhances the metal ions adsorption comparing to their parent materials.
This research was carried out to study the effects of kenaf loading and alkaline treatment on tensile properties, density,
thermal and morphological properties of kenaf filled natural rubber latex foam (NRLF). Samples were prepared using a
Dunlop method. From the results, increasing loading of kenaf reduced the tensile strength and elongation at break for
both samples, treated and untreated kenaf filled NRLF. Meanwhile, modulus at 100% elongation and density increased
with an increased in kenaf loading. Samples with treated kenaf showed higher tensile strength, modulus at 100%
elongation and density but low in elongation at break as compared with samples with untreated kenaf. Thermal study
by using thermogravimetric analysis (TGA) showed that thermal stability reduced with increased in kenaf loading for
both samples. Samples with treated kenaf have higher thermal stability compared with samples of untreated kenaf. The
filler-matrix interaction and the pores size variation of both samples was clearly seen in the micrograph images by using
scanning electron microscope (SEM).
The aim of the present research work is to enhance the thermal and dynamic mechanical properties of Kevlar/Cocos nucifera sheath (CS)/epoxy composites with graphene nano platelets (GNP). Laminates were fabricated through the hand lay-up method followed by hot pressing. GNP at different wt.% (0.25, 0.5, and 0.75) were incorporated with epoxy resin through ultra-sonication. Kevlar/CS composites with different weight ratios (100/0, 75/25, 50/50, 25/75, 0/100) were fabricated while maintaining a fiber/matrix weight ratio at 45/55. Thermal degradation and viscoelastic properties were evaluated using thermogravimetric analysys (TGA), differential scanning calorimetric (DSC) analysis, and a dynamic mechanical analyser (DMA). The obtained results revealed that Kevlar/CS (25/75) hybrid composites at 0.75 wt.% of GNP exhibited similar thermal stability compared to Kevlar/epoxy (100/0) composites at 0 wt.% of GNP. It has been corroborated with DSC observation that GNP act as a thermal barrier. However, DMA results showed that the Kevlar/CS (50/50) hybrid composites at 0.75 wt.% of GNP exhibited almost equal viscoelastic properties compared to Kevlar/epoxy (100/0) composites at 0 wt.% GNP due to effective crosslinking, which improves the stress transfer rate. Hence, this research proved that Kevlar can be efficiently (50%) replaced with CS at an optimal GNP loading for structural applications.
In this study, we fabricated a modified biomaterial based on chitosan and gelatin, which is an intrinsic hydrophilic membrane for oil-water separation to clean water contamination by oil. Modification of the membrane with a non-toxic natural crosslinker, genipin, significantly enhanced the stability of the biopolymer membrane in a water-based medium towards an eco-friendly environment. The effects of various compositions of genipin-crosslinked chitosan-gelatin membrane on the rheological properties, thermal stability, and morphological structure of the membrane were investigated using a dynamic rotational rheometer, thermogravimetry analysis, and chemical composition by attenuated total reflectance spectroscopy (ATR). Modified chitosan-gelatin membrane showed completely miscible blends, as determined by field-emission scanning electron microscopy, differential scanning calorimetry, and ATR. Morphological results showed membrane with establish microstructure to further experiment as filtration product. The membranes were successfully tested for their oil-water separation efficiencies. The membrane proved to be selective and effective in separating water from an oil-water mixture. The optimum results achieved a stable microporous structure of the membrane (microfiltration) and a separation efficiency of above 98%. The membrane showed a high permeation flux, generated as high as 698 and 420 L m-2 h-1 for cooking and crude oils, respectively. Owing to its outstanding recyclability and anti-fouling performance, the membrane can be washed away easily, ensuring the reusability of the prepared membrane.
The present study aims to develop a biodegradable polymer blend that is environmentally friendly and has comparable tensile and thermal properties with synthetic plastics. In this work, microcrystalline cellulose (MCC) extracted from bamboo-chips-reinforced poly (lactic acid) (PLA) and poly (butylene succinate) (PBS) blend composites were fabricated by melt-mixing at 180 °C and then hot pressing at 180 °C. PBS and MCC (0.5, 1, 1.5 wt%) were added to improve the brittle nature of PLA. Field emission scanning electron microscopy (FESEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), thermogravimetric analysis (TGA), differential thermogravimetry (DTG), differential scanning calorimetry (DSC)), and universal testing machine were used to analyze morphology, crystallinity, physiochemical, thermal, and tensile properties, respectively. The thermal stability of the PLA-PBS blends enhanced on addition of MCC up to 1wt % due to their uniform dispersion in the polymer matrix. Tensile properties declined on addition of PBS and increased with MCC above (0.5 wt%) however except elongation at break increased on addition of PBS then decreased insignificantly on addition of MCC. Thus, PBS and MCC addition in PLA matrix decreases the brittleness, making it a potential contender that could be considered to replace plastics that are used for food packaging.
Textile waste cellulose nanofibrillated fibre has been reported with excellent strength reinforcement ability in other biopolymers. In this research cellulose nanofibrilated fibre (CNF) was isolated from the textile waste cotton fabrics with combined supercritical carbon dioxide and high-pressure homogenisation. The isolated CNF was used to enhance the polylactic acid/chitin (PLA/chitin) properties. The properties enhancement effect of the CNF was studied by characterising the PLA/chitin/CNF biocomposite for improved mechanical, thermal, and morphological properties. The tensile properties, impact strength, dynamic mechanical analysis, thermogravimetry analysis, scanning electron microscopy, and the PLA/chitin/CNF biocomposite wettability were studied. The result showed that the tensile strength, elongation, tensile modulus, and impact strength improved significantly with chitin and CNF compared with the neat PLA. Furthermore, the scanning electron microscopy SEM (Scanning Electron Microscopy) morphological images showed uniform distribution and dispersion of the three polymers in each other, which corroborate the improvement in mechanical properties. The biocomposite's water absorption increased more than the neat PLA, and the contact angle was reduced. The results of the ternary blend compared with PLA/chitin binary blend showed significant enhancement with CNF. This showed that the three polymers' combination resulted in a better material property than the binary blend.
This paper presents a comparison on the effects of blending chitin and/or starch with poly(lactic acid) (PLA). Three sets of composites (PLA-chitin, PLA-starch and PLA-chitin-starch) with 92%, 94%, 96% and 98% PLA by weight were prepared. The percentage weight (wt.%) amount of the chitin and starch incorporated ranges from 2% to 8%. The mechanical, dynamic mechanical, thermal and microstructural properties were analyzed. The results from the tensile strength, yield strength, Young's modulus, and impact showed that the PLA-chitin-starch blend has the best mechanical properties compared to PLA-chitin and PLA-starch blends. The dynamic mechanical analysis result shows a better damping property for PLA-chitin than PLA-chitin-starch and PLA-starch. On the other hand, the thermal property analysis from thermogravimetry analysis (TGA) shows no significant improvement in a specific order, but the glass transition temperature of the composite increased compared to that of neat PLA. However, the degradation process was found to start with PLA-chitin for all composites, which suggests an improvement in PLA degradation. Significantly, the morphological analysis revealed a uniform mix with an obvious blend network in the three composites. Interestingly, the network was more significant in the PLA-chitin-starch blend, which may be responsible for its significantly enhanced mechanical properties compared with PLA-chitin and PLA-starch samples.
The ability of inkjet-based 3D printing (3DP) to fabricate biocompatible ceramics has made it one of the most favorable techniques to generate bone tissue engineering (BTE) scaffolds. Calcium sulfates exhibit various beneficial characteristics, and they can be used as a promising biomaterial in BTE. However, low mechanical performance caused by the brittle character of ceramic materials is the main weakness of 3DP calcium sulfate scaffolds. Moreover, the presence of certain organic matters in the starting powder and binder solution causes products to have high toxicity levels. A post-processing treatment is usually employed to improve the physical, chemical, and biological behaviors of the printed scaffolds. In this study, the effects of heat treatment on the structural, mechanical, and physical characteristics of 3DP calcium sulfate prototypes were investigated. Different microscopy and spectroscopy methods were employed to characterize the printed prototypes. The in vitro cytotoxicity of the specimens was also evaluated before and after heat treatment. Results showed that the as-printed scaffolds and specimens heat treated at 300°C exhibited severe toxicity in vitro but had almost adequate strength. By contrast, the specimens heat treated in the 500°C-1000°C temperature range, although non-toxic, had insufficient mechanical strength, which was mainly attributed to the exit of the organic binder before 500°C and the absence of sufficient densification below 1000°C. The sintering process was accelerated at temperatures higher than 1000°C, resulting in higher compressive strength and less cytotoxicity. An anhydrous form of calcium sulfate was the only crystalline phase existing in the samples heated at 500°C-1150°C. The formation of calcium oxide caused by partial decomposition of calcium sulfate was observed in the specimens heat treated at temperatures higher than 1200°C. Although considerable improvements in cell viability of heat-treated scaffolds were observed in this study, the mechanical properties were not significantly improved, requiring further investigations. However, the findings of this study give a better insight into the complex nature of the problem in the fabrication of synthetic bone grafts and scaffolds via post-fabrication treatment of 3DP calcium sulfate prototypes.
This study examined the influence of pyrolysis temperature on biochar characteristics and evaluated its suitability for carbon capture and energy production. Biochar was produced from corn stover using slow pyrolysis at 300, 400 and 500°C and 2 hrs holding time. The experimental biochars were characterized by elemental analysis, BET, FTIR, TGA/DTA, NMR (C-13). Higher heating value (HHV) of feedstock and biochars was measured using bomb calorimeter. Results show that carbon content of corn stover biochar increased from 45.5% to 64.5%, with increasing pyrolysis temperatures. A decrease in H:C and O:C ratios as well as volatile matter, coupled with increase in the concentration of aromatic carbon in the biochar as determined by FTIR and NMR (C-13) demonstrates a higher biochar carbon stability at 500°C. It was estimated that corn stover pyrolysed at 500°C could provide of 10.12 MJ/kg thermal energy. Pyrolysis is therefore a potential technology with its carbon-negative, energy positive and soil amendment benefits thus creating win- win scenario.
A substantive approach converting waste date pits to mercerized mesoporous date pit activated carbon (DPAC) and utilizing it in the removal of Cd(II), Cu(II), Pb(II), and Zn(II) was reported. In general, rapid heavy metals adsorption kinetics for Co range: 25-100 mg/L was observed, accomplishing 77-97% adsorption within 15 min, finally, attaining equilibrium in 360 min. Linear and non-linear isotherm studies revealed Langmuir model applicability for Cd(II) and Pb(II) adsorption, while Freundlich model was fitted to Zn(II) and Cu(II) adsorption. Maximum monolayer adsorption capacities (qm) for Cd(II), Pb(II), Cu(II), and Zn(II) obtained by non-linear isotherm model at 298 K were 212.1, 133.5, 194.4, and 111 mg/g, respectively. Kinetics modeling parameters showed the applicability of pseudo-second-order model. The activation energy (Ea) magnitude revealed physical nature of adsorption. Maximum elution of Cu(II) (81.6%), Zn(II) (70.1%), Pb(II) (96%), and Cd(II) (78.2%) were observed with 0.1 M HCl. Thermogravimetric analysis of DPAC showed a total weight loss (in two-stages) of 28.3%. Infra-red spectral analysis showed the presence of carboxyl and hydroxyl groups over DPAC surface. The peaks at 820, 825, 845 and 885 cm-1 attributed to Zn-O, Pb-O, Cd-O, and Cu-O appeared on heavy metals saturated DPAC, confirmed their binding on DPAC during the adsorption.
In this research work, carbon nanofibers (CNFs) were synthesized on honeycomb monolith substrates using injection chemical vapor deposition (ICVD) technique. The effect of various wash-coated materials and catalyst promoter on the growth rate of CNFs on monolith substrates were examined. The characteristics of the synthesized CNFs-coated monolith composites were examined using Raman spectroscopy, Brunauer-Emmett-Teller (BET), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FE-SEM), and Transmission electron microscopy (TEM) techniques. According to the textural characterization study, the specific surface area and pore volume of CNFs-coated monolith composites were significantly improved as compared to bare monolith which might be attributed to the growth of highly pure and aligned CNFs over monolith substrate. Besides that, the synthesized CNFs-coated monolith possessed extremely well thermal stability up to the temperature of 550 °C which was corresponded to the strong attachment of highly graphitized CNFs over monolith substrates.
There has been significant progress in the last few decades in addressing the biomedical applications of polymer hydrogels. Particularly, stimuli responsive hydrogels have been inspected as elegant drug delivery systems capable to deliver at the appropriate site of action within the specific time. The present work describes the synthesis of pH responsive semi-interpenetrating network (semi-IPN) hydrogels of N-succinyl-chitosan (NSC) via Schiff base mechanism using glutaraldehyde as a crosslinking agent and Poly (acrylamide-co-acrylic acid)(Poly (AAm-co-AA)) was embedded within the N-succinyl chitosan network. The physico-chemical interactions were characterized by Fourier transform infrared (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and field emission scanning electron microscope (FESEM). The synthesized hydrogels constitute porous structure. The swelling ability was analyzed in physiological mediums of pH 7.4 and pH 1.2 at 37°C. Swelling properties of formulations with various amounts of NSC/ Poly (AAm-co-AA) and crosslinking agent at pH 7.4 and pH 1.2 were investigated. Hydrogels showed higher swelling ratios at pH 7.4 while lower at pH 1.2. Swelling kinetics and diffusion parameters were also determined. Drug loading, encapsulation efficiency, and in vitro release of 5-fluorouracil (5-FU) from the synthesized hydrogels were observed. In vitro release profile revealed the significant influence of pH, amount of NSC, Poly (AAm-co-AA), and crosslinking agent on the release of 5-FU. Accordingly, rapid and large release of drug was observed at pH 7.4 than at pH 1.2. The maximum encapsulation efficiency and release of 5-FU from SP2 were found to be 72.45% and 85.99%, respectively. Kinetics of drug release suggested controlled release mechanism of 5-FU is according to trend of non-Fickian. From the above results, it can be concluded that the synthesized hydrogels have capability to adapt their potential exploitation as targeted oral drug delivery carriers.
Polymer electrolyte membranes based on the natural polymer κ-carrageenan were modified and characterized for application in electrochemical devices. In general, pure κ-carrageenan membranes show a low ionic conductivity. New membranes were developed by chemically modifying κ-carrageenan via phosphorylation to produce O-methylene phosphonic κ-carrageenan (OMPC), which showed enhanced membrane conductivity. The membranes were prepared by a solution casting method. The chemical structure of OMPC samples were characterized using Fourier transform infrared spectroscopy (FTIR), 1H nuclear magnetic resonance (1H NMR) spectroscopy and 31P nuclear magnetic resonance (31P NMR) spectroscopy. The conductivity properties of the membranes were investigated by electrochemical impedance spectroscopy (EIS). The characterization demonstrated that the membranes had been successfully produced. The ionic conductivity of κ-carrageenan and OMPC were 2.79 × 10-6 S cm-1 and 1.54 × 10-5 S cm-1, respectively. The hydrated membranes showed a two orders of magnitude higher ionic conductivity than the dried membranes.
A facile thermal-treatment route was successfully used to synthesize ZnO nanosheets. Morphological, structural, and optical properties of obtained nanoparticles at different calcination temperatures were studied using various techniques. The FTIR, XRD, EDX, SEM and TEM images confirmed the formation of ZnO nanosheets through calcination in the temperature between 500 to 650 °C. The SEM images showed a morphological structure of ZnO nanosheets, which inclined to crumble at higher calcination temperatures. The XRD and FTIR spectra revealed that the samples were amorphous at 30 °C but transformed into a crystalline structure during calcination process. The average particle size and degree of crystallinity increased with increasing calcination temperature. The estimated average particle sizes from TEM images were about 23 and 38 nm for the lowest and highest calcination temperature i.e. 500 and 650 °C, respectively. The optical properties were determined by UV-Vis reflection spectrophotometer and showed a decrease in the band gap with increasing calcination temperature.
In this study, dynamic vulcanization process was used to improve the thermal properties of calcium carbonate filled composites. The composites were prepared using a Z-blade mixer at 180oC and rotor speed 50rpm. Thermogravimetric analysis (TGA) and Differential scanning calorimetry (DSC) techniques were used to analyze the thermal properties of the composites. The vulcanized and unvulcanized PP/EPDM composites were filled by CaCO3 at 0, 10, 20, 30, and 40 %wt. Meanwhile, thermogravimetric analysis indicates that the total weight loss of PP/EPDM/CaCO3 composites decreased with increasing filler loading. Dynamic vulcanized composites have higher thermal stability, while the crystallinity of PP/EPDM/CaCO3 composites were increased as compared to unvulcanized composites. Therefore, the thermal properties were improved by the presence of
dynamic vulcanization process.
Cellulose acetate (CA) is an interesting material due to its wide spectrum of utilities across different domains ranging from absorbent to membrane filters. In this study, polystyrene (PS) nanofibres, and cellulose acetate/polystyrene (CA/PS) blend nanofibres with various ratios of CA: PS from 20: 80 to 80: 20 were fabricated by using electrospinning technique. The SEM images show that the nanofibres exhibited non-uniform and random orientation with the average fibre diameter in the range of 100 to 800 nm. It was found that the incorporation of PS had a great effect on the morphology of nanofibre. At high proportion of PS, no or less beaded CA/PS nanofibres were formed. Thermal properties of the composite nanofibres were investigated by using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) techniques. The TGA results showed thermal stability of CA/PS nanofibres were higher than pristine CA.
Ag/PMMA nanocomposites were successfully synthesized by in-situ technique. Transmission electron microscopy (TEM) images show that the particles are spherical in shape and their sizes are dependent on temperature. The smallest particle achieved high stability as indicated from Zeta sizer analysis. The red shift of surface plasmon resonance (SPR) indicated the increases of particle sizes. X-ray diffraction (XRD) patterns exhibit a two-phase (crystalline and amorphous) structure of Ag/PMMA nanocomposites. The complexation of Ag/PMMA nanocomposites was confirmed using Raman spectroscopy. Fourier transform infrared spectroscopy spectra confirmed that the bonding was dominantly influenced by the PMMA and DMF solution. Finally, thermogravimetric analysis (TGA) results indicate that the total weight loss increases as the temperature increases.
Silver nanoparticles and silver-graphene oxide nanocomposites were fabricated using a rapid and green microwave irradiation synthesis method. Silver nanoparticles with narrow size distribution were formed under microwave irradiation for both samples. The silver nanoparticles were distributed randomly on the surface of graphene oxide. The Fourier transform infrared and thermogravimetry analysis results showed that the graphene oxide for the AgNP-graphene oxide (AgGO) sample was partially reduced during the in situ synthesis of silver nanoparticles. Both silver nanoparticles and AgGO nanocomposites exhibited stronger antibacterial properties against Gram-negative bacteria (Salmonella typhi and Escherichia coli) than against Gram-positive bacteria (Staphyloccocus aureus and Staphyloccocus epidermidis). The AgGO nanocomposites consisting of approximately 40 wt.% silver can achieve antibacterial performance comparable to that of neat silver nanoparticles.
Herein, hybrid k-carrageenan bio-nanocomposite films were fabricated by using two types of nanofillers, organically modified montmorillonite (OMMT), and cellulose nanocrystals (CNCs). Hybrid bio-nanocomposite films were made by casting techniques employing 4 wt% of CNCs, OMMT, and hybridized CNCs/OMMT in a 1:1 ratio. The rheological and morphological properties and thermal stability of all composites were investigated using rotational rheometry, thermogravimetry analysis, differential scanning calorimetry, field emission scanning electron microscopy, and transmission electron microscopy (TEM). The results showed that the hybrid CNC/OMMT bio-nanocomposite exhibited significantly improved properties as compared to those for the bio-nanocomposites with single fillers due to the nanosize and homogenous nanofiller dispersion in the matrix. Rheological analysis of the hybrid bio-nanocomposite showed higher dynamic shear storage modulus and complex viscosity values when compared to those for the bio-nanocomposite with individual fillers. The TEM analysis of the hybridized CNC/OMMT bio-nanocomposite revealed that more particles were packed together in the CNC network, which restricted the matrix mobility. The heat resistance and thermal stability bio-nanocomposite k-carrageenan film enhanced rapidly with the addition of hybridized CNCs/OMMT to 275 °C. The hybridized CNCs/OMMT exhibited synergistic effects due to the good affinity through interfacial interactions, resulting in the improvement of the material properties.