Search results for: crystallinity.

Authors: Widi Astuti, Agus Prasetya, Endang Tri Wahyuni, I Made Bendiyasa

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Coal fly ash (CFA) generated by coal-based thermal power plants is mainly composed of some oxides having high crystallinity, like quartz and mullite. In this study, the effect of CFA crystallinity toward lead adsorption capacity was investigated. To get solid with various crystallinity, the solution of sodium hydroxide (NaOH) of 1-7 M was used to treat CFA at various temperature and reflux time. Furthermore, to evaluate the effect of NaOH-treated CFA with respect to adsorption capacity, the treated CFA were examine as adsorbent for removing lead in the solution. The result shows that using NaOH to treat CFA causes crystallinity of quartz and mullite decrease. At higher NaOH concentration (>3M), in addition the damage of quartz and mullite crystallinity is followed by crystal formation called hydroxysodalite. The lower crystalllinity, the higher adsorption capacity.

Keywords: Coal fly ash, crystallinity, lead, adsorption capacity

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Authors: Nidal H. Abu-Zahra, Mahmoud Algazzar

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In this research, n-dodecylthiol was added to P3HT/ PC70BM polymer solar cells to improve the crystallinity of P3HT and enhance the phase separation of P3HT/PC70BM. The improved crystallinity of P3HT:PC70BM doped with 0-5% by volume of n-dodecylthiol resulted in improving the power conversion efficiency of polymer solar cells by 33%. In addition, thermal annealing of the P3HT/PC70MB/n-dodecylthiolcompound showed further improvement in crystallinity with n-dodecylthiol concentration up to 2%. The highest power conversion efficiency of 3.21% was achieved with polymer crystallites size L of 11.2nm, after annealing at 150°C for 30 minutes under a vacuum atmosphere. The smaller crystallite size suggests a shorter path of the charge carriers between P3HT backbones, which could be beneficial to getting a higher short circuit current in the devices made with the additive. 

Keywords: n-dodecylthiol, Congugated PSC, P3HT/PCBM, Polymer Solar Cells.

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Authors: N. Tugrul, F. T. Senberber, A. S. Kipcak E. Moroydor Derun, S. Piskin

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In this research, it is aimed not only microwave synthesis of magnesium borates but also evaluation of magnesium wastes. Synthesis process can be described with the reaction of Mg wastes and boric acid using microwave energy. X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) were applied to synthesized minerals. According to XRD results, magnesium borate hydrate mixtures were obtained as mcallisterite (pdf# = 01-070-1902, Mg₂(B₆O₇(OH)₆)₂.9(H₂O)) at higher crystallinity properties was achieved at the mole ratio raw material 1:1. Also, other kinds of magnesium borate hydrates were obtained at lower crystallinity such as admontite (pdf # = 01-076-0540, MgO(B₂O₃)₃.7(H₂O)), inderite (pdf # = 01-072-2308, 2MgO.3B₂O₃.15(H₂O)) and magnesium borate hydrates (pdf # = 01-076-0539, MgO(B₂O₃)₃.6(H₂O)). FT-IR spectrums indicated that minor changes were seen at the band values of characteristic stretching in each experiment. At the end of experiments it is seen that using microwave energy may contribute positive effects to design of synthesis process such as reducing reaction time and products at higher crystallinity.

Keywords: Magnesium wastes, boric acid, magnesium borate, microwave energy.

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Authors: E. I. Akpan, S. O. Adeosun, G. I. Lawal, S. A. Balogun, X. D. Chen

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The characterisation of agro-wastes fibres for composite applications from Nigeria using X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM) has been done. Fibres extracted from groundnut shell, coconut husk, rice husk, palm fruit bunch and palm fruit stalk are processed using two novel cellulose fibre production methods developed by the authors. Cellulose apparent crystallinity calculated using the deconvolution of the diffractometer trace shows that the amorphous portion of cellulose was permeable to hydrolysis yielding high crystallinity after treatment. All diffratograms show typical cellulose structure with well-defined 110, 200 and 040 peaks. Palm fruit fibres had the highest 200 crystalline cellulose peaks compared to others and it is an indication of rich cellulose content. Surface examination of the resulting fibres using SEM indicates the presence of regular cellulose network structure with some agglomerated laminated layer of thin leaves of cellulose microfibrils. The surfaces were relatively smooth indicating the removal of hemicellulose, lignin and pectin.

Keywords: X-ray diffraction, SEM, cellulose, deconvolution, crystallinity.

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Authors: Amirali Ebrahimi, T. A. G. Langrish

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The effect of various humidities on process yields and degrees of crystallinity for spray-dried powders from spray drying of lactose with humid air in a straight-through system have been studied. It has been suggested by Williams–Landel–Ferry kinetics (WLF) that a higher particle temperature and lower glass-transition temperature would increase the crystallization rate of the particles during the spray-drying process. Freshly humidified air produced by a Buchi-B290 spray dryer as a humidifier attached to the main spray dryer decreased the particle glass-transition temperature (Tg), while allowing the particle temperature (Tp) to reach higher values by using an insulated drying chamber. Differential scanning calorimetry (DSC) and moisture sorption analysis were used to measure the degree of crystallinity for the spray-dried lactose powders. The results showed that higher Tp-Tg, as a result of applying humid air, improved the process yield from 21 ± 4 to 26 ± 2% and crystallinity of the particles by decreasing the latent heat of crystallization from 43 ± 1 to 30 ± 11 J/g and the sorption peak height from 7.3 ± 0.7% to 6 ± 0.7%.

Keywords: Lactose, crystallization, spray drying, humid air.

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Authors: K. Abbas, R. Ahmad, I. A. Khan, S. Saleem, U. Ikhlaq

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Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si₃N₄ confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N₂ plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Keywords: Crystallinity, glow discharge, nitriding, sputtering.

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

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The construction of Nitro -N-amino phenyl maleimide branches onto Cellulose acetate (CA) substrate by free radical graft copolymerization using benzoyl peroxide as initiator led to formation of highly thermal stable copolymers as shown from the results of gravimetric analysis (TGA). CA-g-2,4-dinitro amino phenyl maleimide exhibited higher thermal stability than the CA-g-4-nitro amino phenyl maleimide as shown from the initial decomposition temperature (T_o). This is due to the ability of nitro group to form hydrogen bonding with hydroxyl group of the glucopyranose ring which increases the crystallinity of polymeric matrix. The crystalline shapes representing the graft part are clearly distinct in the Emission scanning electron microscope (ESEM) morphology of the copolymer. A suggested reaction mechanism for the grafting process was also discussed.

Keywords: Cellulose acetate, crystallinity, graft copolymerization, thermal properties.

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Authors: Albana Hasimi, Edlira Tako, Partizan Malkaj, Elvin Çomo, Blerina Papajani, Mirela Ndrita, Ledjan Malaj

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Many endeavors have been exerted during the last years for developing new artificial polymeric membranes, which fulfill the demanded conditions for biomedical uses. One of the most tested polymers is Poly(vinyl alcohol) [PVA]. Our teams are based on the possibility of using PVA for personal protective equipment against COVID-19. In personal protective equipment, we explore the possibility of modifying the properties of the polymer by adding Montmorillonite [MMT]. Heat-treatment above the glass transition temperature is used to improve mechanical properties mainly by increasing the crystallinity of the polymer, which acts as a physical network. Temperature-Modulated Differential Scanning Calorimetry (TMDSC) measurements indicated that the presence of 0.5% MMT in PVA causes a higher Tg value and shaped peak of crystallinity. Decomposition is observed at two of the melting points of the crystals during heating 25-240 oC and overlap of the recrystallization ridges during cooling 240-25 oC. This is indicative of the presence of two types (quality or structure) of polymer crystals. On the other hand, some indication of improvement of the quality of the crystals by heat-treatment is given by the distinct non-reversing contribution to melting. Data on sorption and transport of water in PVA films: PVA pure and PVA/MMT matrix, modified by thermal treatment are presented. The membranes become more rigid as a result of the heat treatment and because of this the water uptake is significantly lower in membranes. That is indicated by analysis of the resulting water uptake kinetics. The presence of 0.5% w/w of MMT has no significant impact on the properties of PVA membranes. Water uptake kinetics deviate from Fick’s law due to slow relaxation of glassy polymer matrix for all types of membranes.

Keywords: Crystallinity, montmorillonite, nanocomposite, poly(vinyl alcohol).

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Authors: Ahmed M. S. Hussein, Sahar Y. Al-Okbi

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In the present research, whole meal barley flour (WBF) was supplemented with gelatinized corn flour (GCF) in 0 and 30%. Whole meal wheat flour (WWF) was mixed with defatted rice bran (DRB) to produce 0, 20, 25, and 30% replacement levels. Rheological properties of dough were studied. Thermal properties and starch crystallinity of flours were evaluated. Flat bread, balady bread and pie were prepared from the different flour blends. The different bakeries were sensory evaluated. Color of raw materials and crust of bakery products were determined. Nutrients contents of raw flours and food products were assessed. Results showed that addition of GCF to WBF increased the viscosity and falling number of the produced dough. Water absorption, dough development time and dough stability increased with increasing the level of DRB in dough while, weakening and mixing tolerance index decreased. Extensibility and energy decreased, while, resistance to extension increased as DRB level increased. Gelatinized temperature of WWF, WBF, GCF, and DRB were 13.26, 35.09, 28.33, and 39.63, respectively. Starch crystallinity was affected when DRB was added to WWF. The highest protein content was present in balady bread made from 70% WWF and 30% DRB. The highest calcium, phosphorus, and potassium levels were present in products made from 100% WBF. Sensory attributes of the products were slightly affected by adding DRB and GCF. Conclusion: Addition of DRB or GCF to WWF or WBF, respectively affect the physical, chemical, rheological and sensory properties of balady bread, flat bread, and pie while improved their nutritive values.

Keywords: Bakeries, rheological properties, chemical and sensory attributes, flour thermal properties and starch crystallinity.

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Authors: Prima Luna, Afroditi Chatzifragkou, Dimitris Charalampopoulos

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Sorghum byproducts, namely bran, stalk, and panicle are examples of lignocellulosic biomass. These raw materials contain large amounts of polysaccharides, in particular hemicelluloses, celluloses, and lignins, which if efficiently extracted, can be utilised for the development of a range of added value products with potential applications in agriculture and food packaging sectors. The aim of this study was to characterise fractions extracted from sorghum bran and stalk with regards to their physicochemical properties that could determine their applicability as food-packaging materials. A sequential alkaline extraction was applied for the isolation of cellulosic, hemicellulosic and lignin fractions from sorghum stalk and bran. Lignin content, phenolic content and antioxidant capacity were also investigated in the case of the lignin fraction. Thermal analysis using differential scanning calorimetry (DSC) and X-Ray Diffraction (XRD) revealed that the glass transition temperature (T_g) of cellulose fraction of the stalk was ~78.33 ^oC at amorphous state (~65%) and water content of ~5%. In terms of hemicellulose, the T_g value of stalk was slightly lower compared to bran at amorphous state (~54%) and had less water content (~2%). It is evident that hemicelluloses generally showed a lower thermal stability compared to cellulose, probably due to their lack of crystallinity. Additionally, bran had higher arabinose-to-xylose ratio (0.82) than the stalk, a fact that indicated its low crystallinity. Furthermore, lignin fraction had T_g value of ~93 ^oC at amorphous state (~11%). Stalk-derived lignin fraction contained more phenolic compounds (mainly consisting of p-coumaric and ferulic acid) and had higher lignin content and antioxidant capacity compared to bran-derived lignin fraction.

Keywords: Alkaline extraction, bran, cellulose, hemicellulose, lignin, sorghum, stalk.

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Authors: S. Manjunatha, M. S. Dharmaprakash

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Well-defined 2D Eu⁺³ co-doped ZrO₂: Gd⁺³ nanoparticles were successfully synthesized by microwave assisted solution combustion technique for luminescent applications. The present investigation reports the rapid and effective method for the synthesis of the Eu⁺³ co-doped ZrO₂:Gd⁺³ nanoparticles and study of the luminescence behavior of Eu⁺³ ion in ZrO₂:Gd⁺³ nanostructures. The optical properties of the prepared nanostructures were investigated by using UV-visible spectroscopy and photoluminescence spectra. The phase formation and the morphology of the nanoplatelets were studied by XRD, FESEM and HRTEM. The average grain size was found to be 45-50 nm. The presence of Gd³⁺ ion increases the crystallinity of the material and hence acts as a good nucleating agent. The ZrO₂:Gd³⁺ co-doped with Eu⁺³ nanoplatelets gives an emission at 607 nm, a strong red emission under the excitation wavelength of 255 nm.

Keywords: Nanoparticles, XRD, TEM, photoluminescence.

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Authors: A. Ito, S. Okamoto

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We constructed an atomic structure model for a PAN-based carbon fiber containing amorphous structures using molecular dynamics methods. It was found that basic physical properties such as crystallinity, Young’s modulus, and thermal conductivity of our model were nearly identical to those of real carbon fibers. We then obtained the tensile strength of a carbon fiber, which has no macro defects. We finally determined that the limitation of the tensile strength was 19 GPa.

Keywords: Amorphous, carbon fiber, molecular dynamics, tensile strength.

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Authors: Samra Isadounene, Amar Boukerrou, Dalila Hammiche

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In this work, the composites were prepared with poly(lactic acid) (PLA) and olive husk flour (OHF) with different percentages (10, 20 and 30%) using extrusion method followed by injection molding. The morphological, mechanical properties and thermal behavior of composites were investigated. Tensile strength and elongation at break of composites showed a decreasing trend with increasing fiber content. On the other hand, Young modulus and storage modulus were increased. The addition of OHF resulted in a decrease in thermal stability of composites. The presence of OHF led to an increase in percentage of crystallinity (Xc) of PLA matrix.

Keywords: Biopolymers, composites, mechanical properties, poly(lactic acid).

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Authors: I. Grigoraviciute-Puroniene, K. Tsuru, E. Garskaite, Z. Stankeviciute, A. Beganskiene, K. Ishikawa, A. Kareiva

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Tricalcium phosphate (β-Ca₃(PO₄)₂, β-TCP) powders were synthesized using wet polymeric precipitation method for the first time to our best knowledge. The results of X-ray diffraction analysis showed the formation of almost single a Ca-deficient hydroxyapatite (CDHA) phase of a poor crystallinity already at room temperature. With continuously increasing the calcination temperature up to 800 °C, the crystalline β-TCP was obtained as the main phase. It was demonstrated that infrared spectroscopy is very effective method to characterize the formation of β-TCP. The SEM results showed that β-TCP solids were homogeneous having a small particle size distribution. The β-TCP powders consisted of spherical particles varying in size from 100 to 300 nm. Fabricated β-TCP specimens were placed to the bones of the rats and maintained for 1-2 months.

Keywords: β-TCP, bone regeneration, wet chemical processing, polymeric precipitation.

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Authors: N. Choosri, N. Swadchaipong, T. Utistham, U. W. Hartley

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Performance of a cobalt doped sol-gel derived silica (Co/SiO2) catalyst for Fischer–Tropsch synthesis (FTS) in slurryphase reactor was studied using paraffin wax as initial liquid media. The reactive mixed gas, hydrogen (H2) and carbon monoxide (CO) in a molar ratio of 2:1, was flowed at 50 ml/min. Braunauer-Emmett- Teller (BET) surface area and X-ray diffraction (XRD) techniques were employed to characterize both the specific surface area and crystallinity of the catalyst, respectively. The reduction behavior of Co/SiO2 catalyst was investigated using the Temperature Programmmed Reduction (TPR) method. Operating temperatures were varied from 493 to 533K to find the optimum conditions to maximize liquid fuels production, gasoline and diesel.

Keywords: Fischer Tropsch synthesis, slurry phase, Co/SiO2, operating temperature.

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Authors: Ridzuan Ramli, Norhafzan Junadi, Mohammad D.H. Beg, Rosli M. Yunus

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In this study, microcrystalline cellulose (MCC) was extracted from oil palm empty fruit bunch (EFB) cellulose which was earlier isolated from oil palm EFB fibre. In order to isolate the cellulose, the chlorination method was carried out. Then, the MCC was prepared by simultaneous ultrasonic and alkali treatment from the isolated α-cellulose. Based on mass balance calculation, the yields for MCC obtained from EFB was 44%. For fiber characterization, it is observed that the chemical composition of the hemicellulose and lignin for all samples decreased while composition for cellulose increased. The structural property of the MCC was studied by X-ray diffraction (XRD) method and the result shows that the MCC produced is a cellulose-I polymorph, with 73% crystallinity.

Keywords: Oil palm empty fruit bunch, microcrystalline cellulose, ultrasonic, alkali treatment, X-ray diffraction.

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Authors: Nuray Uçar, Mervin Ölmez, Özge Alptoğa, Nilgün K. Yavuz, Ayşen Önen

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In recent years, research on continuous graphene oxide fibers has been intensified. Therefore, many factors of production stages are being studied. In this study, the effect of exfoliation time and presence of activated carbon particle (ACP) on graphene oxide fiber’s properties has been analyzed. It has been seen that cross-sectional appearance of sample with ACP is harsh and porous because of ACP. The addition of ACP did not change the electrical conductivity. However, ACP results in an enormous decrease of mechanical properties. Longer exfoliation time results to higher crystallinity degree, C/O ratio and less d space between layers. The breaking strength and electrical conductivity of sample with less exfoliation time is some higher than sample with high exfoliation time.

Keywords: Activated carbon, coagulation by wet spinning, exfoliation, graphene oxide fiber.

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Authors: Shahin Kazemi, Mohammad Reza Mohaddes Mojtahedi, Ruhollah Semnani Rahbar, Wataru Takarada, Takeshi Kikutani

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Nylon 6-clay hybrid/neat nylon 6, sheath/core bicomponent nanocomposite fibers containing 4 wt% of clay in sheath section were melt spun at different take-up speeds. Their orientation and crystalline structure were compared to those of neat nylon 6 fibers. Birefringence measurements showed that the orientation development in sheath and core parts of bicomponent fibers was different. Crystallinity results showed that clay did not act as a nucleating agent for bicomponent fibers. The neat nylon 6 fiber had a smooth surface while striped pattern was appeared on the surface of bicomponent fiber containing clay due to thermal shrinkage of the core part.

Keywords: Bicomponent fiber, High speed melt spinning, Nylon 6-clay hybrid, Nylon 6.

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Authors: Marzieh Moosavi-Nasab, Ali R. Yousefi

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Bacterial cellulose, a biopolysaccharide, is produced by the bacterium, Gluconacetobacter xylinus. Static batch fermentation for bacterial cellulose production was studied in sucrose and date syrup solutions (Bx. 10%) at 28 °C using G. xylinus (PTCC, 1734). Results showed that the maximum yields of bacterial cellulose (BC) were 4.35 and 1.69 g/l00 ml for date syrup and sucrose medium after 336 hours fermentation period, respectively. Comparison of FTIR spectrum of cellulose with BC indicated appropriate coincidence which proved that the component produced by G. xylinus was cellulose. Determination of the area under X-ray diffractometry patterns demonstrated that the crystallinity amount of cellulose (83.61%) was more than that for the BC (60.73%). The scanning electron microscopy imaging of BC and cellulose were carried out in two magnifications of 1 and 6K. Results showed that the diameter ratio of BC to cellulose was approximately 1/30 which indicated more delicacy of BC fibers relative to cellulose.

Keywords: Gluconacetobacter xylinus, Fourier Transform Infrared spectroscopy, Scanning Electron Microscopy, X-ray diffractometry

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Authors: Marzieh Moosavi-Nasab, Ali R. Yousefi, Hamed Askari, Maryam Bakhtiyari

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In this study, static batch fermentation was used for bacterial cellulose production in date syrup solution (Bx. 10%) at 28°C using Gluconacetobacter. xylinus (PTCC 1734). The physicochemical properties of standard Sigma CMC and the produced carboxymethyl bacterial cellulose (CMBC) were studied using FT-IR spectroscopy, X-ray diffractometry (XRD) and Scanning Electron Microscopy (SEM). According to the FT-IR spectra the bands at 1664 and 1431 cm-1 indicate that carboxylic acid groups and carboxylate groups exist on the surface. The SEM imaging of CMBC and CMC carried out in magnification of 1K. Comparing the SEM imaging obviously showed that the ribbon shape in CMC remained but the length of ribbons became shorter while that shape changed to flake shape for CMBC. Determination of the area under XRD patterns demonstrated that the crystallinity amount of CMC was more than that for CMBC (51.08% and 81.84% for CMBC and CMC, respectively).

Keywords: Carboxymethyl bacterial cellulose, Fourier Transform Infrared spectroscopy, Scanning Electron Microscopy, X-ray diffractometry.

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Authors: Anjan Sil, Rajni Sharma, Subrata Ray

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The effect of carbon nanofibers (CNFs) on the electrical properties of Poly(vinylidene fluoride-hexafluoropropylene) (P(VdF-HFP)) based gel polymer electrolytes has been investigated in the present work. The length and diameter ranges of CNFs used in the present work are 5-50 μm and 200-600 nm respectively. The nanocomposite gel polymer electrolytes have been synthesized by solution casting technique with varying CNFs content in terms of weight percentage. Electrochemical impedance analysis demonstrates that the reinforcement of carbon nanofibers significantly enhances the ionic conductivity of the polymer electrolyte. The decrease of crystallinity of P(VdF-HFP) due the addition of CNFs has been confirmed by X-ray diffraction (XRD). The interaction of CNFs with various constituents of nanocomposite gel polymer electrolytes has been assessed by Fourier Transform Infrared (FTIR) spectroscopy. Moreover CNFs added gel polymer electrolytes offer superior thermal stability as compared to that of CNFs free electrolytes as confirmed by Thermogravimetric analysis (TGA).

Keywords: Polymer electrolytes, CNFs, Ionic conductivity, TGA.

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Authors: Ramin Yousefi, Muhamad. Rasat. Muhamad

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We investigated a modified thermal evaporation method in the growth process of ZnO nanowires. ZnO nanowires were fabricated on p-type silicon substrates without using a metal catalyst. A simple horizontal double-tube system along with chemical vapor diffusion of the precursor was used to grow the ZnO nanowires. The substrates were placed in different temperature zones, and ZnO nanowires with different diameters were obtained for the different substrate temperatures. In addition to the nanowires, ZnO microdiscs with different diameters were obtained on another substrate, which was placed at a lower temperature than the other substrates. The optical properties and crystalline quality of the ZnO nanowires and microdiscs were characterized by room temperature photoluminescence (PL) and Raman spectrometers. The PL and Raman studies demonstrated that the ZnO nanowires and microdiscs grown using such set-up had good crystallinity with excellent optical properties. Rectifying behavior of ZnO/Si heterostructures was characterized by a simple DC circuit.

Keywords: ZnO nano and microstructures, Photoluminescence, Raman, Rectifying behavior.

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Authors: Roberta Ranielle M. de Freitas, Vagner R. Botaro

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The relationship between biodegradation and mechanical behavior is fundamental for studies of the application of cellulose acetate films as a possible material for biodegradable packaging. In this work, the biodegradation of cellulose acetate (CA) with DS 2.5 was analyzed in simulated soil. CA films were prepared by casting and buried in the simulated soil. Samples were taken monthly and analyzed, the total time of biodegradation was 6 months. To characterize the biodegradable CA, the DMA technique was employed. The main result showed that the time of exposure to the simulated soil affects the mechanical properties of the films and the values of crystallinity. By DMA analysis, it was possible to conclude that as the CA is biodegraded, its mechanical properties were altered, for example, storage modulus has increased with biodegradation and the modulus of loss has decreased. Analyzes of DSC, XRD, and FTIR were also carried out to characterize the biodegradation of CA, which corroborated with the results of DMA. The observation of the carbonyl band by FTIR and crystalline indices obtained by XRD were important to evaluate the degradation of CA during the exposure time.

Keywords: Biodegradation, cellulose acetate, DMA, simulated soil.

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Authors: Emi Govorčin Bajsić, Vesna Ocelić Bulatović, Miroslav Slouf, Ana Šitum

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Composites based on a biodegradable polycaprolactone (PCL) containing 0.5, 1.0 and 2.0 wt % of titanium dioxide (TiO₂) micro and nanoparticles were prepared by melt mixing and the effect of filler type and contents on the thermal properties, dynamic-mechanical behaviour and morphology were investigated. Measurements of storage modulus and loss modulus by dynamic mechanical analysis (DMA) showed better results for microfilled PCL/TiO₂ composites than nanofilled composites, with the same filler content. DSC analysis showed that the T_g and T_c of micro and nanocomposites were slightly lower than those of neat PCL. The crystallinity of the PCL increased with the addition of TiO₂ micro and nanoparticles; however, the c_c for the PCL was unchanged with micro TiO₂ content. The thermal stability of PCL/TiO₂ composites were characterized using thermogravimetric analysis (TGA). The initial weight loss (5 wt %) occurs at slightly higher temperature with micro and nano TiO₂ addition and with increasing TiO₂ content.

Keywords: Morphology, polycaprolactone, thermal properties, titanium dioxide.

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Authors: Jirakarn Nantapipat, Apanee Luengnaruemitchai, Sujitra Wongkasemjit

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Biofuels, like biobutanol, have been recognized for being renewable and sustainable fuels which can be produced from lignocellulosic biomass. To convert lignocellulosic biomass to biofuel, pretreatment process is an important step to remove hemicelluloses and lignin to improve enzymatic hydrolysis. Dilute acid pretreatment has been successful developed for pretreatment of corncobs and the optimum conditions of dilute sulfuric and phosphoric acid pretreatment were obtained at 120 °C for 5 min with 15:1 liquid to solid ratio and 140 °C for 10 min with 10:1 liquid to solid ratio, respectively. The result shows that both of acid pretreatments gave the content of total sugar approximately 34–35 g/l. In case of inhibitor content (furfural), phosphoric acid pretreatment gives higher than sulfuric acid pretreatment. Characterizations of corncobs after pretreatment indicate that both of acid pretreatments can improve enzymatic accessibility and the better results present in corncobs pretreated with sulfuric acid in term of surface area, crystallinity, and composition analysis.

Keywords: Corncobs, Pretreatment, Sulfuric acid, Phosphoric acid.

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Authors: Suthat Turapan, Cattareya Yotkamchornkun, Kamchai Nuithitikul

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The production of biodiesel from crude palm oil with a homogeneous base catalyst is unlikely owing to considerable formation of soap. Free fatty acids (FFA) in crude palm oil need to be reduced, e.g. by esterification. This study investigated the activity of sulfated zirconia calcined at various temperatures for esterification of FFA in crude palm oil to biodiesel. It was found that under a proper reaction condition, sulfated zirconia well catalyzes esterification. FFA content can be reduced to an acceptable value for typical biodiesel production with a homogeneous base catalyst. Crystallinity and sulfate attachment of sulfated zirconia depend on calcination temperature during the catalyst preparation. Too low temperature of calcination gives amorphous sulfated zirconia which has low activity for esterification of FFA. In contrast, very high temperature of calcination removes sulfate group, consequently, conversion of FFA is reduced. The appropriate temperature range of calcination is 550-650 oC.

Keywords: Biodiesel, Esterification, Free fatty acids, Sulfatedzirconia.

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Authors: Rahmah, M., Farhan, M., Akidah, N.M.Y

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Polybag and mulch film in agricultural field are used plastics which caused environmental problems after transplantation and planting processes due to the discarded wastes. Thus a degradable polybag was designed in this study to replace non degradable polybag with natural biodegradable resin that is widely available, namely sago starch (SS) and polyvinyl alcohol (PVA). Hybrid blend consists of SS, PVA and linear low density polyethylene (LLDPE) was compounded at different ratios. The thermal and mechanical properties of the blends were investigated. Hybrid films underwent landfill degradation tests for up to 2 months. The films showed gelation and melting transition existed for all three systems with significant melting peaks by LLDPE and PVA. All hybrid blends loses its LLDPE semi crystalline characteristics as PVA and SS systems had disrupted crystallinity and enhanced the amorphosity of the hybrid system. Generally, blending SS with PVA improves the mechanical properties of the SS based materials. Tensile strength of each film was also decreased with the increase of SS contents while its modulus had increased with SS content.

Keywords: Appearance peak, LLDPE, PVA, sago starch.

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Authors: Kessara Seneesrisakul, Erdogan Gulari, Sumaeth Chavadej

Abstract:

The complex structure of lignocellulose leads to great difficulties in converting it to fermentable sugars for the ethanol production. The major hydrolysis impediments are the crystallinity of cellulose and the lignin content. To improve the efficiency of enzymatic hydrolysis, microbial pretreatment of corncob was investigated using two bacterial strains of Bacillus subtilis A 002 and Cellulomonas sp. TISTR 784 (expected to break open the crystalline part of cellulose) and lignin-degrading fungus, Phanerochaete sordida SK7 (expected to remove lignin from lignocellulose). The microbial pretreatment was carried out with each strain under its optimum conditions. The pretreated corncob samples were further hydrolyzed to produce reducing glucose with low amounts of commercial cellulase (25 U·g-1 corncob) from Aspergillus niger. The corncob samples were determined for composition change by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscope (SEM). According to the results, the microbial pretreatment with fungus, P. sordida SK7 was the most effective for enhancing enzymatic hydrolysis, approximately, 40% improvement.

Keywords: Corncob, Enzymatic hydrolysis, Microorganisms, Pretreatment.

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

Abstract:

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: Nawapat Detduangchan, Thawien Wittaya

Abstract:

Photo-crosslinked rice starch-based biodegradable films were prepared by casting film-solution on leveled trays and ultra violet (UV) irradiation was applied for 10 minute. The effect of the content (3%, 6% and 9 wt. %)of photosensitiser (sodium benzoate) on mechanical properties, water vapor permeability (WVP) and structural properties of rice starch films were investigated. The tensile strength increased while elongation at break and water resistance properties of rice starch films decreased with addition and increasing content of photosensitiser. The % crystallinity of rice starch films were decreased when the content of photosensitiser increased and UV were applied. The results showed that the carboxylate group band of sodium benzoate was found in the FTIR spectrum of rice starch films and found that incorporation of 6% of photosensitiser into the films showed a higher absorption band of resulted films. This result pointed out the highest interaction between starch molecules was occurred.

Keywords: Biodegradable film, Rice starch, UV treatment, Photosensitiser, Photo-crosslink

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