Search results for: differential scanning calorimetry

Authors: Naveed Ahmad, Farooq Ahmad, Abdul Aal Al-Khazaal

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Rheology can be used as a tool to examine the crystallization kinetics of polymers and polymer composites, and it provides more accurate results than the commonly used conventional techniques like differential scanning calorimetry (DSC) when the crystallization kinetics are slow. Crystallization occurs when crystalline polymers are cooled below their thermodynamic melting point temperature. At the start of this process, there is a gradual change in the mechanical response of the material from the liquid to the solid state, which is due to the change at the microstructure level of the polymer and polymer composites. This is one of the main characteristics of the rheological methodology that sets it apart from the conventional DSC method. In the present work, we used both rheological and differential scanning calorimetric techniques to perform both isothermal and non-isothermal crystallization experiments on a range of syndiotactic polypropylenes/clay composites with varying doses of clay contents in order to investigate the crystallization behavior of the materials. The objective of this work is to explore the effect of clay contents on the crystallization behavior of the syndiotactic polypropylene/clay composites and to couple the rheological methods with more conventional techniques such as Differential Scanning Calorimetry (DSC). Time sweep tests at a constant heating rate of 40°C/minutes were used to investigate the crystallization kinetics using the Atomic Rheumetric Expansion System (ARES). Crystallization behavior was found to be strongly dependent on the clay contents of syndiotactic polypropylene/clay composites. Both melting point (Tₘ) and crystallization temperatures (T𝒸) were found to increase with an increase in clay contents. Excellent agreement is found between the results obtained by both the rheological and differential scanning calorimetric (DSC) methods.

Keywords: quiescent crystallization, polymer composites, rheology, differential scanning calorimetry, syndiotactic polypropylene/clay composites

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Authors: Seyfullah Madakbas, Hatice Birtane, Memet Vezir Kahraman

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In this study, we aimed to synthesize and characterize polyhedral oligomeric silsesquioxanes containing polyimide nanocomposite. Polyimide nanocomposites widely have been used in membranes in fuel cell, solar cell, gas filtration, sensors, aerospace components, printed circuit boards. Firstly, polyamic acid was synthesized and characterized by Fourier Transform Infrared. Then, polyhedral oligomeric silsesquioxanes containing polyimide nanocomposite was prepared with thermal imidization method. The obtained polyimide nanocomposite was characterized by Fourier Transform Infrared, Scanning Electron Microscope, Thermal Gravimetric Analysis and Differential Scanning Calorimetry. Thermal stability of polyimide nanocomposite was evaluated by thermal gravimetric analysis and differential scanning calorimetry. Surface morphology of composite samples was investigated by scanning electron microscope. The obtained results prove that successfully prepared polyhedral oligomeric silsesquioxanes are containing polyimide nanocomposite. The obtained nanocomposite can be used in many industries such as electronics, automotive, aerospace, etc.

Keywords: polyimide, nanocomposite, polyhedral oligomeric silsesquioxanes

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Authors: Sumara Khursheed, Jitendra Sharma

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The present work reports synthesis of nanocomposites (NCs) of phosphor (KCaVO4:Sm3+) embedded poly(methylmethacrylate) (PMMA) using solution casting method and their optical properties measurements for their possible application in making flexible luminescent films. X-ray diffraction analyses were employed to obtain the structural parameters as crystallinity, shape and size of the obtained NCs. The emission and excitation spectra were obtained using Photoluminescence spectroscopy to quantify the spectral properties of these fluorescent polymer/phosphor films. Optical energy gap has been estimated using UV-VIS spectroscopy while differential scanning calorimetry (DSC) was exploited to measure the thermal properties of the NC films in terms of their thermal stability, glass transition temperature and degree of crystallinity etc.

Keywords: nanocomposites, luminescence, XRD, differential scanning calorimetry, PMMA

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Authors: Adriana Souza M. Batista, Cláubia Pereira, Luiz O. Faria

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The irradiation of polymeric materials has received much attention because it can produce diverse changes in chemical structure and physical properties. Thus, studying the chemical and structural changes of polymers is important in practice to achieve optimal conditions for the modification of polymers. The effect of gamma irradiation on the crystalline structure of poly(vinylidene fluoride) (PVDF) has been investigated using differential scanning calorimetry (DSC) and X-ray diffraction techniques (XRD). Gamma irradiation was carried out in atmosphere air with doses between 100 kGy at 3,000 kGy with a Co-60 source. In the melting thermogram of the samples irradiated can be seen a bimodal melting endotherm is detected with two melting temperature. The lower melting temperature is attributed to melting of crystals originally present and the higher melting peak due to melting of crystals reorganized upon heat treatment. These results are consistent with those obtained by XRD technique showing increasing crystallinity with increasing irradiation dose, although the melting latent heat is decreasing.

Keywords: differential scanning calorimetry, gamma irradiation, PVDF, X-ray diffraction technique

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Authors: Pauline Ribert, Gaelle Roudaut, Sebastien Dupont, Laurent Beney

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Yeasts, anhydrobiotic organisms, can survive extreme water disturbances, thanks to the prolonged and reversible suspension of their cellular activity as well as the establishment of a defense arsenal. This property is exploited by many industrialists. One of the protection systems implemented by yeast is the vitrification of its cytoplasm by trehalose. The thermal resistance of dry yeasts is a crucial parameter for their use. However, studies on the thermal resistance of dry yeasts are often based on yeasts produced in laboratory conditions with non-optimal drying processes. We, therefore, propose a study on the thermal resistance of industrial dry yeasts in relation to their thermophysical properties. Heat stress was applied at three temperatures (50, 75, and 100°C) for 10, 30, or 60-minute treatments. The survival of yeasts to these treatments was estimated, and their thermophysical properties were studied by differential scanning calorimetry. The industrial dry yeasts resisted 60 minutes at 50°C and 75°C and 10 minutes at a temperature close to 100°C. At 100°C, yeast was above their glass transition temperature. Industrial dry yeasts are therefore capable of withstanding high thermal stress if maintained in a specific thermophysical state.

Keywords: dry yeast, glass transition, thermal resistance, vitrification

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Authors: Anton Trník, Lenka Scheinherrová, Robert Černý

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Silica fume is a by-product of the ferro-silicon and silicon metal industries. It is mainly in the form of amorphous silica. Silica fume belongs to pozzolanic active materials which can be used in concrete to improve its final properties. In this paper, the influence of silica fume on hydration of cement pastes is studied using differential scanning calorimetry (DSC) and thermogravimetry (TG) at various curing times (2, 7, 28, and 90 days) in the temperature range from 25 to 1000 °C in an argon atmosphere. Samples are prepared from Portland cement CEM I 42.5 R which is partially replaced with the silica fume of 4, 8, and 12 wt.%. The water/binder ratio is chosen as 0.5. It is identified and described the liberation of physically bound water, calcium–silicate–hydrates dehydration, portlandite and calcite decomposition in studied samples. Also, it is found out that an exothermic peak at 950 °C is observed without a significant mass change for samples with 12 wt.% of silica fume after two days of hydration. This peak is probably caused by the pozzolanic reaction between silica fume and Portland cement. Its size corresponds to the degree of crystallization between Ca and Si. The portlandite content is lower for the samples with a higher amount of silica fume.

Keywords: differential scanning calorimetry, hydration, silica fume, thermogravimetry

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Authors: Sharmila Pradhan, Ralf Lach, George Michler, Jean Mark Saiter, Rameshwar Adhikari

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Ethylene/1-octene copolymer was modified incorporating three types of nanofillers differed in their dimensionality in order to investigate the effect of filler dimensionality on mechanical properties, for instance, tensile strength, microhardness etc. The samples were prepared by melt mixing followed by compression moldings. The microstructure of the novel material was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) method and Transmission electron microscopy (TEM). Other important properties such as melting, crystallizing and thermal stability were also investigated via differential scanning calorimetry (DSC) and Thermogravimetry analysis (TGA). The FTIR and XRD results showed that the composites were formed by physical mixing. The TEM result supported the homogeneous dispersion of nanofillers in the matrix. The mechanical characterization performed by tensile testing showed that the composites with 1D nanofiller effectively reinforced the polymer. TGA results revealed that the thermal stability of pure EOC is marginally improved by the addition of nanofillers. Likewise, melting and crystallizing properties of the composites are not much different from that of pure.

Keywords: copolymer, differential scanning calorimetry, nanofiller, tensile strength

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Authors: K. Tomolya, D. Janovszky, A. Sycheva, M. Sveda, A. Roosz

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CuZrAl amorphous alloys have attracted high interest due to unique physical and mechanical properties, which can be enhanced by adding of Ni and Ti elements. It is known that this properties can be enhanced by crystallization of amorphous alloys creating nanocrystallines in the matrix. The present work intends to produce nanosized crystalline parti-cle reinforced amorphous matrix composite powders by crystallization of amorphous powders. As the first step the amorphous powders were synthe-tized by ball-milling of crystalline powders. (Cu49Zr45Al6) 80Ni10Ti10 and (Cu49Zr44Al7) 80Ni10Ti10 (at%) alloys were ball-milled for 12 hours in order to reach the fully amorphous structure. The impact en-ergy of the balls during milling causes the change of the structure in the powders. Scanning electron microscopical (SEM) images shows that the phases mixed first and then changed into a fully amorphous matrix. Furthermore, nanosized particles in the amorphous matrix were crystallized by heat treatment of the amorphous powders that was confirmed by TEM measurement. It was of importance to define the tem-perature when the amorphous phase starts to crystal-lize. Amorphous alloys have a special heating curve and characteristic temperatures, which can be meas-ured by differential scanning calorimetry (DSC). A typical DSC curve of an amorphous alloy exhibits an endothermic event characteristic of the equilibrium glass transition (Tg) and a distinct undercooled liquid region, followed by one or two exothermic events corresponding to crystallization processes (Tp). After measuring the DSC traces of the amorphous powders, the annealing temperatures should be determined between Tx and Tp. In our experiments several temperatures from the annealing temperature range were selected and de-pendency of crystallized nanoparticles fraction on their hardness was investigated.

Keywords: amorphous structure, composite, mechanical milling, powder, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electronmocroscopy (TEM)

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Authors: A. M. T. Jacinto, M.O. Osi

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Tamarind has various medicinal properties among which is its antibacterial property. Its bark contains saponins, alkaloids, sesquiterpenes and tannins. It is rich in phlobapenes which is responsible for antibacterial property. The objective of the study was to determine which bark will produce the highest antibacterial property, develop it into a topical cream and evaluate its quality and characteristics. Powdered barks of Tamarind were extracted by soxhlet method using 70% acetone. Stem bark produced a higher yield than trunk bark (5.85 g vs. 4.73 g). It was found that the trunk bark was more sensitive than stem bark to microorganisms namely Staphylococcus aureus, Corynebacterium minutissimum, and Streptococcus spp. Sensitivity of trunk bark can be attributed to a more developed phytoconstituents. Dermal sensitization test on both sexes of rabbits using the following concentrations: 100%, 40% and 20% of extract showed that Tamarind has no irritating property and therefore safe for formulation into an antibacterial cream. Excipients used for formulation such as methyl paraben, propyl paraben, stearyl alcohol and white petrolatum were compatible with the Tamarind acetone extract through Differential Scanning Calorimetry except sodium lauryl sulfate that exhibited crystallization when subjected at 200˚C. The method of manufacture used in cream is fusion, therefore strict compliance of processing temperature should be observed to prevent polymorphism. Quality control tests of formulated cream based on USP 30 and Philippine Pharmacopeia were satisfactory.

Keywords: antibacterial, differential scanning calorimetry, tannins, dermal sensitization

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Authors: M. Khlifa, A. Youssef, A. F. Zaed, A. Kraft, V. Arrighi

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A series of PS-nanoparticles were prepared by grafting PS from both aggregated silica and colloidally silica using atom-transfer radical polymerisation (ATRP). The mechanical behaviour of the nanocomposites have been examined by differential scanning calorimetry (DSC)and dynamic mechanical thermal analysis (DMTA).

Keywords: ATRP, nanocomposites, polystyrene, reinforcement

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Authors: Ekere E. Kokonne, Isimi C. Yetunde, Okoh E. Judith, Okafor E. Ijeoma, Ajeh J. Isaac, Olobayo O. Kunle, Emeje O. Martins

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NIPRIMAL® is a mono herbal formulation of Nauclea latifolia used in the treatment of malaria. The stability of extracts made from plant material is essential to ensure the quality, safety and efficacy of the finished product. This study assessed the stability of the formulation under three different storage conditions; normal room temperature, infrared and under refrigeration. Differential Scanning Calorimetry (DSC) and Thin Layer Chromatography (TLC) were used to monitor the formulations. The DSC analysis was done from 0oC to 350oC under the three storage conditions. Results obtained indicate that NIPRIMAL® was stable at all the storage conditions investigated. Thin layer chromatography (TLC) after 6 months showed there was no significant difference between retention factor (RF) values for the various storage conditions. The reference sample had four spots with RF values of 0.47, 0.68, 0.76, 0.82 respectively and these spots were retained in the test formulations with corresponding RF values were after 6 months at room temperature and refrigerated temperature been 0.56, 0.73, 0.80, 0.92 and 0.47, 0.68, 0.76, 0.82 respectively. On the other hand, the RF values (0.55, 0.74, 0.77, 0.93) obtained under infrared after 1 month varied slightly from the reference. The sample exposed to infrared had a lower heat capacity compared to that stored under room temperature or refrigeration. A combination of TLC and DSC measurements has been applied for assessing the stability of NIPRIMAL®. Both methods were found to be rapid, sensitive and reliable in determining its stability. It is concluded that NIPRIMAL® can be stored under any of the tested conditions without degradation. This study is a major contribution towards developing appropriate stability monitoring parameters for herbal products.

Keywords: differential scanning calorimetry, formulation, NIPRIMAL®, stability, thin layer hromatography

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Authors: M. Fatmi, T. Chihi, M. A. Ghebouli, B. Ghebouli

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This work presents the experimental results of the differential scanning calorimetry (DSC), hardness measurements (Hv) and XRD analysis, for order to investigate the kinetics of precipitation phenomena in Al-7%wt. Mg alloy. In the XRD and DSC curves indicates the formation of the intermediate precipitation of β-(Al3Mg2) phase respectively. The activation energies associated with the processes have been determined according to the three models proposed by Kissinger, Ozawa, and Boswell. Consequently, the nucleation mechanism of the precipitates can be explained. These phases are confirmed by XRD analysis.

Keywords: discontinuous precipitation, hardening, Al–Mg alloys, mechanical and mechatronics engineering

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Authors: Patricia Mikchaela D. L. Feliciano, Ciela Kadeshka A. Fuentes, Bea Trixia B. Gales, Ethel Princess A. Gepulango, Martin R. Hernandez, Elina Andrea S. Lantion, Jhoe Cynder P. Legaspi, Peter F. Quilala, Gina C. Castro

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Propolis is a resin-like material used by bees to fill large gap holes in the beehive. It has been found to possess anti-inflammatory property, which stimulates hair growth in rats by inducing hair keratinocytes proliferation, causing water retention and preventing damage caused by heat, ultraviolet rays, and other microorganisms without abnormalities in hair follicles. The present study aimed to formulate 10% and 30% Propolis Hair Cream for use in enhancing hair properties. Raw propolis sample was tested for heavy metals using Atomic Absorption Spectroscopy; zinc and chromium were found to be present. Likewise, propolis was extracted in a percolator using 70% ethanol and concentrated under vacuum using a rotary evaporator. The propolis extract was analyzed for total flavonoid content. Compatibility of the propolis extract with excipients was evaluated using Differential Scanning Calorimetry (DSC). No significant changes in organoleptic properties, pH and viscosity of the formulated creams were noted after four weeks of storage at 2-8°C, 30°C, and 40°C. The formulated creams were found to be non-irritating based on the Modified Draize Rabbit Test. In vivo efficacy was evaluated based on thickness and tensile strength of hair grown on previously shaved rat skin. Results show that the formulated 30% propolis-based cream had greater hair enhancing properties than the 10% propolis cream, which had a comparable effect with minoxidil.

Keywords: atomic absorption spectroscopy, differential scanning calorimetry (DSC), modified draize rabbit test, propolis

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Authors: A. Azizi, M. Toubane, L. Chetibi

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Differential scanning calorimetry (DSC) is a widely used technique for the study of phase transformations, particularly in the study of precipitation. The kinetic of the precipitation and dissolution is always related to the concept of activation energy Ea. The determination of the activation energy gives important information about the kinetic of the precipitation reaction. In this work, we were interested in the study of the isothermal and non-isothermal treatments on the decomposition of the supersaturated solid solution in the alloy AZ91 (Mg-9 Al-Zn 1-0.2 Mn. mass fraction %), using Differential Calorimetric method. Through this method, the samples were heat treated up to 425° C, using different rates. To calculate the apparent activation energies associated with the formation of precipitated phases, we used different isoconversional methods. This study was supported by other analysis: X-ray diffraction and microhardness measurements.

Keywords: calorimetric, activation energy, AZ91 alloys, microstructural evolution

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Authors: Karina I. Hidas, Csaba Németh, Anna Visy, Judit Csonka, László Friedrich, Ildikó Cs. Nyulas-Zeke

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Egg yolk is a popular ingredient in the food industry due to its gelling, emulsifying, colouring, and coagulating properties. Because of the heat sensitivity of proteins, egg yolk can only be heat treated at low temperatures, so its shelf life, even with the addition of a preservative, is only a few weeks. Freezing can increase the shelf life of liquid egg yolk up to 1 year, but it undergoes gelling below -6 ° C, which is an irreversible phenomenon. The degree of gelation depends on the time and temperature of freezing and is influenced by the process of thawing. Therefore, in our experiment, we examined egg yolks thawed in different ways. In this study, unpasteurized, industrially broken, separated, and homogenized liquid egg yolk was used. Freshly produced samples were frozen in plastic containers at -18°C in a laboratory freezer. Frozen storage was performed for 90 days. Samples were analysed at day zero (unfrozen) and after frozen storage for 1, 7, 14, 30, 60 and 90 days. Samples were thawed in two ways (at 5°C for 24 hours and 30°C for 3 hours) before testing. Calorimetric properties were examined by differential scanning calorimetry, where heat flow curves were recorded. Denaturation enthalpy values were calculated by fitting a linear baseline, and denaturation temperature values were evaluated. Besides, dry matter content of samples was measured by the oven method with drying at 105°C to constant weight. For statistical analysis two-way ANOVA (α = 0.05) was employed, where thawing mode and freezing time were the fixed factors. Denaturation enthalpy values decreased from 1.1 to 0.47 at the end of the storage experiment, which represents a reduction of about 60%. The effect of freezing time was significant on these values, already the enthalpy of samples stored frozen for 1 day was significantly reduced. However, the mode of thawing did not significantly affect the denaturation enthalpy of the samples, and no interaction was seen between the two factors. The denaturation temperature and dry matter content did not change significantly either during the freezing period or during the defrosting mode. Results of our study show that slow freezing and frozen storage at -18°C greatly reduces the amount of protein that can be denatured in egg yolk, indicating that the proteins have been subjected to aggregation, denaturation or other protein conversions regardless of how they were thawed.

Keywords: denaturation enthalpy, differential scanning calorimetry, liquid egg yolk, slow freezing

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Authors: Lee Chiau Yeng, Norhayani Othman

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Regenerated cellulose fiber is fabricated in the NaOH/urea aqueous solution. In this work, cellulose is dissolved in 7 .wt% NaOH/12 .wt% urea in the temperature of -12 °C to prepare regenerated cellulose. Thermal and structure properties of cellulose and regenerated cellulose was compared and investigated by Field Emission Scanning Electron Microscopy (FeSEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Thermogravimetric analysis (TGA), and Differential Scanning Calorimetry. Results of FeSEM revealed that the regenerated cellulose fibers showed a more circular shape with irregular size due to fiber agglomeration. FTIR showed the difference in between the structure of cellulose and the regenerated cellulose fibers. In this case, regenerated cellulose fibers have a cellulose II crystalline structure with lower degree of crystallinity. Regenerated cellulose exhibited better thermal stability than the cellulose.

Keywords: regenerated cellulose, cellulose, NaOH, urea

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Authors: Beena Sethi

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This work involves the degradation of plastic waste in the presence of three different nanocatalysts. A thin film of LLDPE was formed with all three nanocatalysts separately in the solvent. Thermo Gravimetric Analysis (TGA) and Differential Scanning Calorimetric (DSC) analysis of polymers suggest that the presence of these catalysts lowers the degradation temperature and the change mechanism of degradation. Gas chromatographic analysis was carried out for two films. In gas chromatography (GC) analysis, it was found that degradation of pure polymer produces only 32% C3/C4 hydrocarbons and 67.6% C5/C9 hydrocarbons. In the presence of these catalysts, more than 80% of polymer by weight was converted into either liquid or gaseous hydrocarbons. Change in the mechanism of degradation of polymer was observed therefore more C3/C4 hydrocarbons along with valuable feedstock are produced. Adjustment of dose of nanocatalyst, use of nano-admixtures and recycling of catalyst can make this catalytic feedstock recycling method a good tool to get sustainable environment. The obtained products can be utilized as fuel or can be transformed into other useful products. In accordance with the principles of sustainable development, chemical recycling i.e. tertiary recycling of polymers along with the reuse (zero order recycling) of plastics can be the most appropriate and promising method in this direction. The tertiary recycling is attracting much attention from the viewpoint of the energy resource.

Keywords: degradation, differential scanning calorimetry, feedstock recycling, gas chromatography, thermogravimetric analysis

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Authors: Rishi Sharma, S. N. Maiti

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The non-isothermal crystallization kinetics of PP/SEBS-g-MA blends up to 0-50% concentration of copolymer was studied by differential scanning calorimetry at four different cooling rates. Crystallization parameters were analyzed by Avrami and Jeziorny models. Primary and secondary crystallization processes were described by Avrami equation. Avrami model showed that all types of shapes grow from small dimensions during primary crystallization. However, three-dimensional crystal growth was observed during the secondary crystallization process. The crystallization peak and onset temperature decrease, however

Keywords: crystallization kinetics, non-isothermal, polypropylene, SEBS-g-MA

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Authors: Manel Hannachi, Mustapha Nechiche, Said Azem

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This study focuses on biodegradable materials made from Poly-lactic acid (PLA) and vegetal reinforcements. Three materials are developed from PLA, as a matrix, and : (i) olive kernels (OK); (ii) alfa (α) short fibers and (iii) OK+ α mixture, as reinforcements. After processing of PLA pellets and olive kernels in powder and alfa stems in short fibers, three mixtures, namely PLA-OK, PLA-α, and PLA-OK-α are prepared and homogenized in Turbula®. These mixtures are then compacted at 180°C under 10 MPa during 15 mn. Scanning Electron Microscopy (SEM) examinations show that PLA matrix adheres at surface of all reinforcements and the dispersion of these ones in matrix is good. X-ray diffraction (XRD) analyses highlight an increase of PLA inter-reticular distances, especially for the PLA-OK case. These results are explained by the dissociation of some molecules derived from reinforcements followed by diffusion of the released atoms in the structure of PLA. This is consistent with Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC) analysis results.

Keywords: alfa short fibers, biodegradable composite, olive kernels, poly-lactic acid

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Authors: Memet Vezir Kahraman, Ferhat Sen

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This study aimed to develop polyelectrolyte structured antimicrobial food packaging materials that do not contain any antimicrobial agents. Cationic hydroxyethyl cellulose was synthesized and characterized by Fourier Transform Infrared, carbon and proton Nuclear Magnetic Resonance spectroscopy. Its nitrogen content was determined by the Kjeldahl method. Polyelectrolyte structured antimicrobial food packaging materials were prepared using hydroxyethyl cellulose, cationic hydroxyethyl cellulose, and sodium alginate. Antimicrobial activity of materials was defined by inhibition zone method (disc diffusion method). Thermal stability of samples was evaluated by thermal gravimetric analysis and differential scanning calorimetry. Surface morphology of samples was investigated by scanning electron microscope. The obtained results prove that produced food packaging materials have good thermal and antimicrobial properties, and they can be used as food packaging material in many industries.

Keywords: antimicrobial food packaging, cationic hydroxyethyl cellulose, polyelectrolyte, sodium alginate

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Authors: Azza A. Al-Ghamdi, Abir S. Abdel-Naby

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Cellulose acetate (CA) is a natural biodegradable polymer. It forms transparent films by the casting technique. CA suffers from high degree of water permeability as well as the low thermal stability at high temperatures. To adjust the CA polymeric films to the manufacture of food packaging, its thermal and mechanical properties should be improved. The modification of CA by grafting it with N-Amino phenyl maleimide (N-APhM) led to the construction of hydrophobic branches throughout the polymeric matrix which reduced its wettability as compared to the parent CA. The branches built onto the polymeric chains had been characterized by UV/Vis, ¹³C-NMR and ESEM. The improvement of the thermal properties was investigated and compared to the parent CA using thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), differential thermal analysis (DTA), contact angle and mechanical testing measurements. The results revealed that the water-uptake was reduced by increasing the graft percentage. The thermal and mechanical properties were also improved.

Keywords: cellulose acetate, food packaging, graft copolymerization, thermal properties

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Authors: Fatemeh Alsadat Miri, Morteza Ehsani, Hossein Ali Khonakdar, Behjat Kavyani

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This paper studies the effect of nano glass flakes on morphology, dynamic-mechanical properties, and crystallization behavior of poly (ethylene terephthalate) (PET). The concentration of nano glass flakes was varied from 0.5, 1, 2, and 3% wt of the total formulation. Scanning electron microscopy (SEM) micrographs showed the poor distribution of nano-glass flake particles in PET, as well as low adhesion of particles to the polymer matrix. According to differential scanning calorimetry (DSC), the crystallization rate and crystallization temperature of PET were increased by the addition of nano glass flakes. The crystallization rate of PET was increased from 31.41% to 34.25% by the incorporation of 1%wt of nano glass flakes. Based on the results of the dynamic-mechanical analysis, the storage modulus of PET gets increased by adding nano glass flakes, especially below glass transition temperature (Tg). The glass transition of PET did not change remarkably with the addition of nano glass flakes. Moreover, the use of nano glass flakes reduced the impact strength of PET.

Keywords: PET, nano glass flakes, morphology, crystallization

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Authors: Tahira Pirzada, Zahra Ashrafi, Saad Khan

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We present a facile and sustainable solid templating approach to fabricate highly porous, flexible and superhydrophobic aerogels of composite nanofibers of cellulose diacetate and silica which are produced through sol gel electrospinning. Scanning electron microscopy, contact angle measurement, and attenuated total reflection-Fourier transform infrared spectrometry are used to understand the structural features of the resultant aerogels while thermogravimetric analysis and differential scanning calorimetry demonstrate their thermal stability. These aerogels exhibit a self-supportive three-dimensional network abundant in large secondary pores surrounded by primary pores resulting in a highly porous structure. Thermal crosslinking of the aerogels has further stabilized their structure and flexibility without compromising on the porosity. Ease of processing, thermal stability, high porosity and oleophilic nature of these aerogels make them promising candidate for a wide variety of applications including acoustic and thermal insulation and oil and water separation.

Keywords: hybrid aerogels, sol-gel electrospinning, oil-water separation, nanofibers

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Authors: Ngwenya M., Gumede T. P., Perez Camargo R. A., Motloung B.

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This study presents the development of eco-friendly bio-nanocomposites using poly(lactic acid) (PLA), poly(caprolactone) (PCL), and their blends with nanocellulose extracted from Saccharum Officinarum. The extracted nanocellulose was optimized through chemical treatment and hydrolysis processes, yielding a sustainable and renewable resource for enhancing polymer properties. Bio-nanocomposites of PLA/nanocellulose, PCL/nanocellulose, and PLA/PCL/nanocellulose with varying nanocellulose contents (1, 3, and 5 wt%) were prepared via melt-blending and characterized using Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), dynamic mechanical analysis (DMA) and tensile testing. The results show significant improvements in the thermal and mechanical properties of the polymeric matrices upon the addition of nanocellulose, demonstrating the potential of these bio-nanocomposites for advanced applications. These developments are promising for obtaining bio-nanocomposites from local bio-sources, leading to more sustainable and eco-friendly alternatives to traditional materials.

Keywords: bionanocomposites, polycaprolactone, poly(lactic acid), nanocellulose, saccharum officinarum

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Authors: Heloise Sasso Teixeira, Talita Szlapak Franco, Thais Helena Sydenstricker Flores-Sahagun, Milton Vazquez Lepe, Graciela Bolzon Muñiz

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Due to the need to reduce the consumption of materials produced from non-renewable sources, the search for new raw materials of natural origin is growing. In this regard, lignocellulosic fibers have great potential. Ceiba sp fibers are found in the fruit of the tree of the same name and have characteristics that differ from other natural fibers. Ceiba fibers are very light, have a high cellulose content, and are hydrophobic due to the presence of waxes on their surface. In this study, Ceiba fiber was used as raw material to obtain cellulose nanofibers (CNF), with the potential to be used in polymeric matrices. Due to the characteristics of this fiber, no chemical pretreatment was necessary before the mechanical defibrilation process in a colloidal mill, obtaining sustainable nanocellulose. The CNFs were characterized by Fourier infrared (FTIR), differential scanning calorimetry (DSC), analysis of the rmogravimetic (TGA), scanning electron microscopy (SEM), transmission electron microscopy, and X-ray photoelectron spectroscopy (XPS).

Keywords: cellulose nanofibers, nanocellulose, fibers, Brazilian fIbers, lignocellulosic, characterization

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Authors: D. Benmoussa, H. Hannache, O. Cherkaoui

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In textiles, the major interest in microencapsulation is currently in the application of durable fragrances, skin softeners, phase-change materials, antimicrobial agents and drug delivery systems onto textile materials. In our research “Polyethylene Glycol” was applied as phase change material and it was encapsulated in polymethacrylic acid (PMA) by radical polymerization in suspension of methacrylic acid in presence of N,N'-methylenebisacrylamide (MBAM) as crosslinking agent. Thereafter the obtained microcapsule was modified by amidation with ethylenediamine as a spacer molecule. At the end of this spacer trichlorotriazine reactive group was fixed. Microcapsules were grafted onto cotton textile substrate. The surface morphologies of the microencapsulated phase change materials (micro PCMs) were studied by scanning electron microscopy (SEM). Thermal properties, thermal reliabilities and thermal stabilities of the as-prepared micro PCMs were investigated by differential scanning calorimetry (DSC) and thermogravmetric analysis (TGA). The results obtained show the obtaining microcapsules with a mean diameter of 10 µm and the resistance of the microcapsules is demonstrated by thermal analysis.

Keywords: energy storage, microencapsulation, phase-change materials, thermogravmetric analysis (TGA)

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Authors: Seyfullah Madakbaş, Ferhat Şen, Memet Vezir Kahraman

Abstract:

The aim of this study was to improve thermal stability, mechanical and surface properties of thermoplastic polyurethane (TPU) with the addition of BaTiO3. The TPU/ BaTiO3 composites having various ratios of TPU and BaTiO3 were prepared. The chemical structure of the prepared composites was investigated by FT-IR. FT-IR spectra of TPU/ barium titanate composites show that they successfully were prepared. Thermal stability of the samples was evaluated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The prepared composites showed high thermal stability, and the char yield increased as barium titanate content increased. The glass transition temperatures of the composites rise with the addition of barium titanate. Mechanical properties of the samples were characterized with stress-strain test. The mechanical properties of the TPU were increased with the contribution of the contribution of the barium titanate it increased. Hydrophobicity of the samples was determined by the contact angle measurements. The contact angles have the tendency to increase the hydrophobic behavior on the surface, when barium titanate was added into TPU. Moreover, the surface morphology of the samples was investigated by a scanning electron microscopy (SEM). SEM-EDS mapping images showed that barium titanate particles were dispersed homogeneously. Finally, the obtained results prove that the prepared composites have good thermal, mechanical and surface properties and that they can be used in many applications such as the electronic devices, materials engineering and other emergent.

Keywords: barium titanate, composites, thermoplastic polyurethane, scanning electron microscopy

Procedia PDF Downloads 297

Authors: Kwangin Kim, Taewon Yoo, Haksoo Han

Abstract:

Polyimide is a superior polymer in the electronics industry, and we conducted a study to synthesize poly(amide-imide) at low temperatures. Poly(amide-imide) was synthesized at low-temperature curing to offer a thermal stable membrane with low residual stress and good processability. As a result, the low crack polymer with good processability could be used to various applications such as semiconductors, integrated circuits, coating materials, membranes, and display. The synthesis of poly(amide-imide) at low temperatures was confirmed by Fourier transform infrared spectroscopy (FT-IR). Thermal stabilities of the polymer was confirmed by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC).

Keywords: poly(amide-imide), residual stress, thermal stability

Procedia PDF Downloads 390

Authors: H. A. Brandão Cordeiro, M. G. Bocardo, N. C. Penteado, V. T. de Moraes, S. M. Giampietri Lebrão, G. W. Lebrão

Abstract:

The present study desired to obtain a nanocomposite of epoxy resin reinforced with graphene oxide (OG), for aerospace application, produced by aqueous emulsion. It was obtained proof bodies with 0.00 wt%, 0.10 wt%, 0.25 wt% and 0.50 wt% in weight of nanoparticles, to check the influence of it in the final quality of the obtained product. The validation of the results was done by the application thermal characterization by differential scanning calorimetry (DSC). It was seen that the nanocomposite reinforced with 0.10 wt% of OG showed the best results, the average glass transition temperature, at 2 °C, compared to the pure resin.

Keywords: aqueous emulsion, graphene, nanocomposites, thermal characterization

Procedia PDF Downloads 136

Authors: H. Özkan Gülsoy, Antonyraj Arockiasamy

Abstract:

The application of powder injection molding technology for the fabrication of metallic and non-metallic components is of growing interest as the process considerably saves time and cost. Utilizing this fabrication method, full dense components are being prepared in various sizes. In this work, our effort is focused to study the densification behavior of the parts made using different size 316L stainless steel powders. The metal powders were admixed with an adequate amount of polymeric compounds and molded as standard tensile bars. Solvent and thermal debinding was carried out followed by sintering in ultra pure hydrogen atmosphere based on the differential scanning calorimetry (DSC) cycle. Mechanical property evaluation and microstructural characterization of the sintered specimens was performed using universal Instron tensile testing machine, Vicker’s microhardness tester, optical (OM) and scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction were used. The results are compared and analyzed to predict the strength and weakness of the test conditions.

Keywords: powder injection molding, sintering, particle size, stainless steels

Procedia PDF Downloads 330