The development of advanced composite materials has taken center stage because of its advantages over traditional materials. Recently, carbon-based advanced additives have shown promising results in the development of advanced polymer composites. The inter- and intra-laminar fracture toughness in modes I and II, along with the thermal and electrical conductivities, were investigated. The HMWCNTs/epoxy composite was prepared using a multi-dispersion method, followed by uniform coating at the mid-layers of the CF/E prepregs interface using the spray coating technique. Analysis methods, such as double cantilever beam (DCB) and end notched flexure (ENF) tests, were carried out to study the mode I and II fracture toughness. The surface morphology of the composite was analyzed using field emission scanning electron microscopy (FESEM). The DCB test showed that the fracture toughness of the 0.2 wt.% and 0.4 wt.% HMWCNT composite laminates was improved by 39.15% and 115.05%, respectively, compared with the control sample. Furthermore, the ENF test showed that the mode II interlaminar fracture toughness for the composite laminate increased by 50.88% and 190%, respectively. The FESEM morphology results confirmed the HMWCNTs bridging at the fracture zones of the CF/E composite and the improved interlaminar fracture toughness. The thermogravimetric analysis (TGA) results demonstrated a strong intermolecular bonding between the epoxy and HMWCNTs, resulting in an improved thermal stability. Moreover, the differential scanning calorimetry (DSC) results confirmed that the addition of HMWCNT shifted the Tg to a higher temperature. An electrical conductivity study demonstrated that a higher CNT concentration in the composite laminate resulted in a higher conductivity improvement. This study confirmed that the demonstrated dispersion technique could create composite laminates with a strong interfacial bond interaction between the epoxy and HMWCNT, and thus improve their properties.
The effect of solid solution treatment on semisolid microstructure of Zn-22Al with developed dendrites was investigated. Zn-22Al is a zinc-based alloy with aluminium as its main alloying element. Producing Zn-22Al product by semisolid metal processing (SSM) offers significant advantages, such as reduction of macrosegregations, porosity and low forming efforts. Meanwhile, thermal and microstructure analyses of Zn-22Al alloy were studied using differential scanning calorimeter (DSC) and Olympus optical microscope. Solidus and liquidus of the alloy can be determined by DSC analysis. In addition, changes to the microstructures in response to solid solution treatments were also analyzed. The major effort of all the semi-solid technologies is the generation of small and spherical morphologies. Prior to the generation of spherical morphologies, the fine grains should be first produced. The as-cast samples were isothermally held at 315°C, ranging from 0.5 to 5 hours before they were partially re-melted at semisolid temperature of 438°C to produce solid globular grains structure in liquid matrix. The results indicated that a non-dendritic semisolid microstructure could not be obtained if the traditionally cast Zn-22Al alloy with developed dendrites was directly subjected to partial remelting. After solid solution treatment at 315°C, the black interdendritic eutectics were dissolved and gradually transformed into ß structure when the treatment time was increased. The microstructure of the solid solution treated sample changed into a small globular structure with the best shape factor of 0.9 and this corresponded to 40±16µm when the sample was treated for 3 hours, followed by directly partial remelting into its semi solid zone.
This paper studied the thermal behaviour of pineapple leaf fibre (PALF) reinforced high impact polystyrene (HIPS) composite. Thermogravimetric analysis (TGA) and differential scanning calorimetric (DSC) analysis were used to measure the thermal characteristic of HIPS/PALF composites. In particular, the TGA analysis was utilized to measure the degradation and decomposition of materials in neat polystyrene, pineapple fibre, and the composites. The measurements were carried out in the temperature of 25°C – 800°C, at a heating rate of 20°C min-1 and the nitrogen gas flow was 50 mL min-1. The temperature of the DSC analysis was programmed to be between 25°C – 300°C. The results from TGA analysis show that the addition of pineapple fibre has improved the thermal stability of the composites as compared to neat HIPS. In addition, the effects of compatibilising agent and surface modification of PALF with alkali treated were also determined and compared.
In this research work, graphene nanoplatelets (GNP) were selected as alternative reinforcing nanofillers to enhance the properties of polypropylene (PP) using different compatibilizers called polypropylene grafted maleic anhydride (PP-g-MA) and ethylene-octene elastomer grafted maleic anhydride (POE-g-MA). A twin screw extruder was used to compound PP, GNP, and either the PP-g-MA or POE-g-MA compatibilizer. The effect of GNP loading on mechanical and thermal properties of neat PP was investigated. Furthermore, the influence and performance of different compatibilizers on the final properties, such as mechanical and thermal, were discussed and reported. Tensile, flexural, impact, melting temperature, crystallization temperature, and thermal stability were evaluated by using a universal testing system, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). For mechanical properties, it was found that increasing GNP content from 1 wt.% to 5 wt.% increased tensile strength of the neat PP up to 4 MPa. The influence of compatibilizers on the mechanical properties had been discussed and reported. For instance, the addition of PP-g-MA compatibilizer improved tensile strength of neat PP with GNP loading. However, the addition of compatibilizer POE-g-MA slightly decreased the tensile strength of neat PP. A similar trend of behavior was observed for flexural strength. For thermal properties, it was found that both GNP loading and compatibilizers have no significant influence on both crystallization and melting temperature of neat PP. For thermal stability, however, it was found that increasing the GNP loading had a significant influence on improving the thermal behavior of neat PP. Furthermore, the addition of compatibilizers into the PP/GNP nanocomposite had slightly improved the thermal stability of neat PP.
Polylactic acid (PLA)/Epoxidized natural rubber (ENR-50) blends were prepared by melt extrusion followed by injection
molding to fabricate the test samples. The effect of ENR-50 loadings on the morphological, mechanical, chemical
resistance and water absorption properties of the blends were studied using standard methods. The toughness of the
blend improved with ENR loading up to 20 wt. % but flexural and tensile strength decreased. The balanced mechanical
properties were obtained at 20 wt. % ENR-50 loading. SEM showed good distribution and increased ENR particle size
as ENR content increased from 10 to 30 wt. %. The differential scanning calorimeter (DSC) showed a steady drop in
crystallization temperature (Tc
) as ENR content increases while the glass transition temperature (Tg
) remained unchanged.
Water absorption was observed to increase with ENR loadings. Increase in ENR content was also observed to reduce the
chemical resistance of the blends.
There has been an increasing interest in the use of natural materials as drug delivery vehicles due to their biodegradability, biocompatibility and ready availability. These properties make bacterial cellulose (BC), from nata de coco, a promising biopolymer for drug delivery applications. The aim of this study was to investigate the film-coating and drug release properties of this biopolymer. Physicochemical, morphological and thermal properties of BC films were studied. Model tablets were film coated with BC, using a spray coating technique, and in vitro drug release studies of these tablets were investigated. It was found that BC exhibited excellent ability to form soft, flexible and foldable films without the addition
of any plasticizer. They were comparable to Aquacoat ECD (with plasticizer) in tensile strength, percentage elongation and elasticity modulus. Differential scanning calorimetry (DSC) BC showed a high Tg value indicating thermally stability of films. These results suggest that BC can be used as novel aqueous film-coating agent with lower cost and better film forming properties than existing film-coating agents.
Feedstock preparation, as well as its characterization, is crucial in the production of highly sintered parts with minimal defect. The hard metal powder - particularly, cemented carbide (wc-co) used in this study was investigated both physically and thermally to determine its properties before the mixing and injection molding stage. Several analyses were conducted, such as scanning electron microscopy, energy dispersive X-ray diffraction, pycnometer density, critical powder volume percentage (cPvP), as well as thermal tests, such as thermogravimetric analysis and differential scanning calorimetry. On the basis of the CPVP value, the feedstock, consisting of wc-co powder, was mixed with 60% palm stearin and 40% polyethylene at an optimal powder loading, within 2 to 5% lower than the CPVP value. The CPVP spotted value was 65%. The feedstock optimal value at 61% showed good rheological properties (pseudoplastic behavior) with an n value lower than 1, considerably low activation energy and high moldability index. These preliminary properties of the feedstock serve as a benchmark in designing the schedule for the next whole steps (i.e. injection, debinding and sintering processes).
Photovoltaic module backsheets are characterized according to their thermal, optical, mechanical, and technical properties. This work introduces new fabricated backsheets for PV modules using polyvinylidene fluoride (PVDF) reinforced with short sugar palm fiber (SSPF) composites. The preparation of composites undergoes multiple phases of fabrication. Thermal, optical, and technical investigations of their properties were conducted. Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, in-situ scanning probe microscopy (SPM), dynamic mechanical analysis (DMA), thermal mechanical analysis (TMA), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and prolonged technical testing were accomplished to expansively understand the complex behavior of composites under various conditions. The optical properties of PV backsheets are critical components in determining the reflectance, absorbance, and transmittance of light. The PVDF-SSPF composites exhibited exceptional compatibility and thermal stability, further revealing a homogenous composite structure with enhanced interfacial bonding between the short fiber and polymer matrix.
Curcumin (CUR), a curcuminoid originating from turmeric root, possesses diverse pharmacological applications, including potent anticancer properties. However, the use of this efficacious agent in cancer therapy has been limited due to low water solubility and poor bioavailability. To overcome these problems, a drug delivery system was established as an excipient allowing improved dispersion in aqueous media coupled with enhanced in vitro anticancer effects. Different analyses such as UV-vis spectroscopy, differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), solubility and dissolution assays were determined to monitor the successful encapsulation of CUR within the inner cavity of a β-cyclodextrin (β-CD) complex. The results indicated that water solubility was improved by 205.75-fold compared to pure CUR. Based on cytotoxicity data obtained from MTT assays, the inclusion complex exhibited a greater decrease in cancer cell viability compared to pure CUR. Moreover, cancer cell migration rates were decreased by 75.5% and 38.92%, invasion rates were decreased by 37.7% and 35.7%, while apoptosis rates were increased by 26.3% and 14.2%, and both caused caspase 3 activation toward colorectal cancer cells (SW480 and HCT116 cells). This efficacious formulation that enables improved aqueous dispersion is potentially useful and can be extended for various chemotherapeutic applications. Preliminary toxicity evaluation also indicated that its composition can be safely used in humans for cancer therapy.
For effective topical and transdermal drug delivery, it is necessary for most actives to penetrate and permeate through the stratum corneum (SC). Extensive investigation of the thermal behaviour of mammalian SC has been performed to understand the barrier function of the skin. However, little attention has been paid to the related experimental variables in thermal analysis of the SC using differential scanning calorimetry that may influence the results obtained from such studies. In this review, we provide a comprehensive overview of the thermal transitions of the SC of both porcine and human skin. More importantly, the selection and impact of the experimental and instrumental parameters used in thermal analysis of the SC are critically evaluated. New opportunities for the use of thermal analysis of mammalian SC in advancing skin research, particularly for elucidation of the actions of excipients employed in topical and transdermal formulations on the skin are also highlighted.
A synthesis of acrylonitrile (AN)/butyl acrylate (BA)/fumaronitrile (FN) and AN/EHA (ethyl hexyl acrylate)/FN terpolymers was carried out by redox polymerization using sodium bisulfite (SBS) and potassium persulphate (KPS) as initiator at 40 °C. The effect of comonomers, BA and EHA and termonomer, FN on the glass transition temperature (Tg) and stabilization temperature was studied using Differential Scanning Calorimetry (DSC). The degradation behavior and char yield were obtained by Thermogravimetric Analysis. The conversions of AN, comonomers (BA and EHA) and FN were 55%-71%, 85%-91% and 76%-79%, respectively. It was found that with the same comonomer feed (10%), the Tg of AN/EHA copolymer was lower at 63 °C compared to AN/BA copolymer (70 °C). AN/EHA/FN terpolymer also exhibited a lower Tg at 63 °C when compared to that of the AN/BA/FN terpolymer (67 °C). By incorporating BA and EHA into a PAN system, the char yield was reduced to ~38.0% compared to that of AN (~47.7%). It was found that FN reduced the initial cyclization temperature of AN/BA/FN and AN/EHA/FN terpolymers to 228 and 221 °C, respectively, in comparison to that of AN/BA and AN/EHA copolymers (~260 °C). In addition, FN reduced the heat liberation per unit time during the stabilization process that consequently reduced the emission of volatile group during this process. As a result, the char yields of AN/BA/FN and AN/EHA/FN terpolymers are higher at ~45.1% and ~43.9%, respectively, as compared to those of AN/BA copolymer (37.1%) and AN/EHA copolymer (38.0%).
Pasteurized shell eggs are eggs that have been thermally treated to eliminate harmful bacteria, however the treatment may also denature some of the egg white proteins. In this study the degree of denaturation and functional properties (emulsifying, foaming, and gelling properties) of egg white obtained from pasteurized eggs (EWP) were compared with those of unpasteurized eggs (EWUP). Data from differential scanning calorimeter showed that the EWP (ovotransferin, lysozyme, and ovalbumin) denatured at lower temperatures and required lower denaturation enthalpies than EWUP, indicating a partial loss of protein structure during the pasteurization process in the pasteurized eggs. The emulsion and foam stability formed from EWP were significantly (P < 0.05) lower than those of EWUP, however the EWP formed stronger gels than EWUP. To assess suitability of EWP as a cake ingredient, angel food cake was prepared using both egg whites. As compared to EWUP-cake, EWP-cake was significantly (P < 0.05) lower in volume, cohesiveness and springiness values, but significantly (P < 0.05) higher in hardness, gumminess and chewiness. Overall, the sensory panelists gave significantly (P < 0.05) higher scores for angel food cake prepared with EWUP. The differences in functional properties of egg white proteins and the quality of cake were due mainly to the higher levels of denaturation attained by EWP as a result of the pasteurization process.
Dough mixing and thermal properties including the pasting profiles of various commercial wheat flour (WF)-banana pseudostem flour (BP)-hydrocolloid blends were determined using a farinograph, differential scanning calorimetry (DSC) and a rapid-visco analyser (RVA). The prepared blends were WF, WF substituted with 10% BP (10BP) and 10BP with added 0.8% w/w (flour weight basis) xanthan gum (XG) or sodium carboxymethylcellulose (CMC) (10BPX and 10BPC, respectively). The dough of 10BP and the doughs containing XG or CMC reduced stability and breakdown time compared with the WF dough. All dough containing BP demonstrated greater water absorption and mixing tolerance index values than the WF dough. The substitution of 10% BP into WF and the addition of hydrocolloids did not significantly affect the conclusion temperature (Tc) of the mixture, but did increased the onset temperature (To), peak temperature (Tp) and decreased the gelatinisation enthalpy change (ΔHg) of the blends. Samples of 10BP, 10BPX and 10BPC significantly decreased (p
A study was conducted to detect and quantify lard stearin (LS) content in canola oil (CaO) using differential scanning calorimetry (DSC). Authentic samples of CaO were obtained from a reliable supplier and the adulterant LS were obtained through a fractional crystallization procedure as reported previously. Pure CaO samples spiked with LS in levels ranging from 5 to 15% (w/w) were analyzed using DSC to obtain their cooling and heating profiles. The results showed that samples contaminated with LS at 5% (w/w) level can be detected using characteristic contaminant peaks appearing in the higher temperature regions (0 to 70°C) of the cooling and heating curves. Pearson correlation analysis of LS content against individual DSC parameters of the adulterant peak namely peak temperature, peak area, peak onset temperature indicated that there were strong correlations between these with the LS content of the CaO admixtures. When these three parameters were engaged as variables in the execution of the stepwise regression procedure, predictive models for determination of LS content in CaO were obtained. The predictive models obtained with single DSC parameter had relatively lower coefficient of determination (R(2) value) and higher standard error than the models obtained using two DSC parameters in combination. This study concluded that the predictive models obtained with peak area and peak onset temperature of the adulteration peak would be more accurate for prediction of LS content in CaO based on the highest coefficient of determination (R(2) value) and smallest standard error.
The main goal of the present work was to assess the mechanism of crystallisation, more precisely the dominant component responsible for primary crystal formations and fat agglomerations. Therefore, DSC results exhibited significant effect on temperature transition; peak sharpness and enthalpy at palm stearin (PS) levels more than 40wt.%. HPLC data demonstrated slight reduction in the content of POO/OPO at PS levels less than 40wt.%, while the excessive addition of PS more than 40wt.% increased significantly PPO/POP content. The pNMR results showed significant drop in SFC for blends containing PS less than 40wt.%, resulting in low SFC less than 15% at body temperature (37°C). Moreover, the values of viscosity (η) and shear stress (τ) at PS levels over 40wt.% expressed excellent internal friction of the admixtures. All the data reported indicate that PPO/POP was the major component of primary nucleus developed. In part, the levels of PS should be less than 40wt.%, if these blends are designed to be used for margarine production.
The aim of this study was to evaluate the mechanical properties and glass transition temperature (Tg) of a denture base material prepared from high molecular weight poly methyl methacrylate (PMMA) and alumina (Al2O3). The glass transition temperature was studied by using differential scanning calorimetry (DSC). The effect of powder-to-liquid ratio was investigated. The result showed that the tensile properties and the Tg were slightly effected by the powder-to-liquid ratio. The ratio of 2.2:1 by weight of powder to liquid was found to be the best ratio for mixing the material to give the best result in this formulation.
The study aims to characterize the structural relaxation times of quench-cooled co-amorphous systems using Kohlrausch-Williams-Watts (KWW) and to correlate the relaxation data with the onset of crystallization. Comparison was also made between the relaxation times obtained by KWW and the width of glass transition temperature (ΔTg) methods (simple and quick). Differential scanning calorimetry, Fourier-transformed infrared spectroscopy, and polarized light microscopy were used to characterize the systems. Results showed that co-amorphous systems yielded a single Tg and ΔCp, suggesting the binary mixtures exist as a single amorphous phase. A narrow step change at Tg indicates the systems were fragile glasses. In co-amorphous nap-indo and para-indo, experimental Tgs were in good agreement with the predicted Tg. However, the Tg of co-amorphous nap-cim and indo-cim were 20°C higher than the predicted Tg, possibly due to stronger molecular interactions. Structural relaxation times below the experimental Tg were successfully characterized using the KWW and ΔTg methods. The comparison plot showed that KWW data are directly proportional to the ½ power of ΔTg data, after adjusting for a small offset. A moderate positive correlation was observed between the onset of crystallization and the KWW data. Structural relaxation times may be useful predictor of physical stability of co-amorphous systems.
Gel polymer electrolytes using imidazolium based ionic liquids have attracted much attention in dye-sensitized solar cell applications. Hydroxypropyl cellulose (HPC), sodium iodide (NaI), 1-methyl-3-propylimidazolium iodide (MPII) as ionic liquid (IL), ethylene carbonate (EC) and propylene carbonate (PC) are used for preparation of non-volatile gel polymer electrolyte (GPE) system (HPC:EC:PC:NaI:MPII) for dye-sensitized solar cell (DSSC) applications. The highest ionic conductivity of 7.37 × 10(-3) S cm(-1) is achieved after introducing 100% of MPII with respect to the weight of HPC. Temperature-dependent ionic conductivity of gel polymer electrolytes is studied in this work. XRD patterns of gel polymer electrolytes are studied to confirm complexation between HPC polymer, NaI and MPII. Thermal behavior of the GPEs is studied using simultaneous thermal analyzer (STA) and differential scanning calorimetry (DSC). DSSCs are fabricated using gel polymer electrolytes and J-V centeracteristics of fabricated dye sensitized solar cells were analyzed. The gel polymer electrolyte with 100 wt.% of MPII ionic liquid shows the best performance and energy conversion efficiency of 5.79%, with short-circuit current density, open-circuit voltage and fill factor of 13.73 mA cm(-2), 610 mV and 69.1%, respectively.
The D-optimal mixture experimental design was employed to optimize the melting point of natural lipstick based on pitaya (Hylocereus polyrhizus) seed oil. The influence of the main lipstick components-pitaya seed oil (10%-25% w/w), virgin coconut oil (25%-45% w/w), beeswax (5%-25% w/w), candelilla wax (1%-5% w/w) and carnauba wax (1%-5% w/w)-were investigated with respect to the melting point properties of the lipstick formulation. The D-optimal mixture experimental design was applied to optimize the properties of lipstick by focusing on the melting point with respect to the above influencing components. The D-optimal mixture design analysis showed that the variation in the response (melting point) could be depicted as a quadratic function of the main components of the lipstick. The best combination of each significant factor determined by the D-optimal mixture design was established to be pitaya seed oil (25% w/w), virgin coconut oil (37% w/w), beeswax (17% w/w), candelilla wax (2% w/w) and carnauba wax (2% w/w). With respect to these factors, the 46.0 °C melting point property was observed experimentally, similar to the theoretical prediction of 46.5 °C. Carnauba wax is the most influential factor on this response (melting point) with its function being with respect to heat endurance. The quadratic polynomial model sufficiently fit the experimental data.
Plasticized poly(lactic acid) PLA with epoxidized vegetable oils (EVO) were prepared using a melt blending method to improve the ductility of PLA. The plasticization of the PLA with EVO lowers the Tg as well as cold-crystallization temperature. The tensile properties demonstrated that the addition of EVO to PLA led to an increase of elongation at break, but a decrease of tensile modulus. Plasticized PLA showed improvement in the elongation at break by 2058% and 4060% with the addition of 5 wt % epoxidized palm oil (EPO) and mixture of epoxidized palm oil and soybean oil (EPSO), respectively. An increase in the tensile strength was also observed in the plasticized PLA with 1 wt % EPO and EPSO. The use of EVO increases the mobility of the polymeric chains, thereby improving the flexibility and plastic deformation of PLA. The SEM micrograph of the plasticized PLA showed good compatible morphologies without voids resulting from good interfacial adhesion between PLA and EVO. Based on the results of this study, EVO may be used as an environmentally friendly plasticizer that can improve the overall properties of PLA.