Abstract: Fused Deposition Modelling (FDM) is one of the additive manufacturing techniques that has become highly attractive in the industrial and academic sectors. However, parts fabricated through FDM are highly susceptible to geometrical defects such as warpage, shrinkage, and delamination that can severely affect their function. Among the thermoplastic polymer feedstock for FDM, semi-crystalline polymers are highly prone to part distortion due to polymer crystallization. In this study, the influence of FDM processing conditions such as chamber temperature and print bed temperature on the induced thermal residual stress and resulting warpage are investigated using 3D transient thermal model for a semi-crystalline polymer. The thermo-mechanical properties and the viscoelasticity of the polymer, as well as the crystallization physics which considers the crystallinity of the polymer, are coupled with the evolving temperature gradient of the print model. From the results it was observed that increasing the chamber temperature from 25 °C to 75 °C leads to a decrease of 3.3% residual stress and increase of 0.4% warpage, while decreasing bed temperature from 100 °C to 60 °C resulted in 27% increase in residual stress and a significant rise of 137% in warpage. The simulated warpage data are validated by comparing it with the measured warpage values of the samples using 3D scanning.
Abstract: This study aimed to find out chemical and structural suitability of synthesized eppawala hydroxyapatite composite as bone cement, by comparing and contrasting it with human bone as well as commercially available bone cement, which is currently used in orthopedic surgeries. Therefore, a mixture of commercially available bone cement and its liquid monomer, commercially available methyl methacrylate (MMA) and a mixture of solid state synthesized eppawala hydroxyapatite powder with commercially available MMA were prepared as the direct substitution for bone cement. Then physical and chemical properties including composition, crystallinity, presence of functional groups, thermal stability, surface morphology, and microstructural features were examined compared to human bone. Results show that there is a close similarity between synthesized product and human bone and it has exhibited high thermal stability, good crystalline and porous properties than the commercial product. Finally, the study concluded that synthesized hydroxyapatite composite can be used directly as a substitution for commercial bone cement.
Abstract: 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 (To). 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.
Abstract: Hydroxyapatite is a bioceramic which can be used for applications in orthopedics and dentistry due to its structural similarity with the mineral phase of mammalian bones and teeth. In this study, it was synthesized, chemically changing natural Eppawala chloroapatite mineral as a value-added product. Sol-gel approach and solid state sintering were used to synthesize products using diluted nitric acid, ethanol and calcium hydroxide under different conditions. Synthesized Eppawala hydroxyapatite powder was characterized using X-ray Fluorescence (XRF), X-ray Powder Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) in order to find out its composition, crystallinity, presence of functional groups, bonding type, surface morphology, microstructural features, and thermal dependence and stability, respectively. The XRD results reflected the formation of a hexagonal crystal structure of hydroxyapatite. Elementary composition and microstructural features of products were discussed based on the XRF and SEM results of the synthesized hydroxyapatite powder. TGA and DSC results of synthesized products showed high thermal stability and good material stability in nature. Also, FTIR spectroscopy results confirmed the formation of hydroxyapatite from apatite via the presence of hydroxyl groups. Those results coincided with the FTIR results of mammalian bones including human bones. The study concludes that there is a possibility of producing hydroxyapatite using commercially available Eppawala chloroapatite in Sri Lanka.
Abstract: 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.
Abstract: 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.
Abstract: 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.
Abstract: 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.
Abstract: Cefixime, a BCS class II drug, is insoluble in water but freely soluble in acetone and in alcohol. The aqueous solubility of cefixime in water is poor and exhibits exceptionally slow and intrinsic dissolution rate. In the present study, cefixime and β-Cyclodextrin (β-CD) solid dispersions were prepared with a view to study the effect and influence of β-CD on the solubility and dissolution rate of this poorly aqueous soluble drug. Phase solubility profile revealed that the solubility of cefixime was increased in the presence of β-CD and was classified as AL-type. Effect of variable, such as drug:carrier ratio, was studied. Physical characterization of the solid dispersion was characterized by Fourier transform infrared spectroscopy (FT-IR) and Differential scanning calorimetry (DSC). These studies revealed that a distinct loss of drug crystallinity in the solid molecular dispersions is ostensibly accounting for enhancement of dissolution rate in distilled water. The drug release from the prepared solid dispersion exhibited a first order kinetics. Solid dispersions of cefixime showed a 6.77 times fold increase in dissolution rate over the pure drug.
Abstract: 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.
Abstract: Enzymatic modification of rice flour can produce highly functional derivatives use in food industries. This study aimed to evaluate the physical properties and resistant starch content of rice flour residues hydrolyzed by α-amylase. Rice flour hydrolyzed by α-amylase (60 and 300 u/g) for 1, 24 and 48 hours were investigated. Increasing enzyme concentration and hydrolysis time resulted in decreased rice flour residue’s lightness (L*) but increased redness (a*) and yellowness (b*) of rice flour residues. The resistant starch content and peak viscosity increased when hydrolysis time increased. Pasting temperature, trough viscosity, breakdown, final viscosity, setback and peak time of the hydrolyzed flours were not significantly different (p>0.05). The morphology of native flour was smooth without observable pores and polygonal with sharp angles and edges. However, after hydrolysis, granules with a slightly rough and porous surface were observed and a rough and porous surface was increased with increasing hydrolyzed time. The X-ray diffraction patterns of native flour showed A-type configuration, which hydrolyzed flour showed almost 0% crystallinity indicated that both amorphous and crystalline structures of starch were simultaneously hydrolyzed by α-amylase.
Abstract: 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 (Tg) of cellulose fraction of the stalk was ~78.33 oC at amorphous state (~65%) and water content of ~5%. In terms of hemicellulose, the Tg 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 Tg 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.
Abstract: 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.
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.
Abstract: 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.
Abstract: 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).
Abstract: Microbial fuel cells (MFCs) represent a promising
technology for simultaneous bioelectricity generation and wastewater
treatment. Catalysts are significant portions of the cost of microbial
fuel cell cathodes. Many materials have been tested as aqueous
cathodes, but air-cathodes are needed to avoid energy demands for
water aeration. The sluggish oxygen reduction reaction (ORR) rate at
air cathode necessitates efficient electrocatalyst such as carbon
supported platinum catalyst (Pt/C) which is very costly. Manganese
oxide (MnO2) was a representative metal oxide which has been
studied as a promising alternative electrocatalyst for ORR and has
been tested in air-cathode MFCs. However the single MnO2 has poor
electric conductivity and low stability. In the present work, the MnO2
catalyst has been modified by doping Pt nanoparticle. The goal of the
work was to improve the performance of the MFC with minimum Pt
loading. MnO2 and Pt nanoparticles were prepared by hydrothermal
and sol gel methods, respectively. Wet impregnation method was
used to synthesize Pt/MnO2 catalyst. The catalysts were further used
as cathode catalysts in air-cathode cubic MFCs, in which anaerobic
sludge was inoculated as biocatalysts and palm oil mill effluent
(POME) was used as the substrate in the anode chamber. The asprepared
Pt/MnO2 was characterized comprehensively through field
emission scanning electron microscope (FESEM), X-Ray diffraction
(XRD), X-ray photoelectron spectroscopy (XPS), and cyclic
voltammetry (CV) where its surface morphology, crystallinity,
oxidation state and electrochemical activity were examined,
respectively. XPS revealed Mn (IV) oxidation state and Pt (0)
nanoparticle metal, indicating the presence of MnO2 and Pt.
Morphology of Pt/MnO2 observed from FESEM shows that the
doping of Pt did not cause change in needle-like shape of MnO2
which provides large contacting surface area. The electrochemical
active area of the Pt/MnO2 catalysts has been increased from 276 to
617 m2/g with the increase in Pt loading from 0.2 to 0.8 wt%. The
CV results in O2 saturated neutral Na2SO4 solution showed that
MnO2 and Pt/MnO2 catalysts could catalyze ORR with different
catalytic activities. MFC with Pt/MnO2 (0.4 wt% Pt) as air cathode
catalyst generates a maximum power density of 165 mW/m3, which
is higher than that of MFC with MnO2 catalyst (95 mW/m3). The
open circuit voltage (OCV) of the MFC operated with MnO2 cathode
gradually decreased during 14 days of operation, whereas the MFC
with Pt/MnO2 cathode remained almost constant throughout the
operation suggesting the higher stability of the Pt/MnO2 catalyst.
Therefore, Pt/MnO2 with 0.4 wt% Pt successfully demonstrated as an
efficient and low cost electrocatalyst for ORR in air cathode MFC with higher electrochemical activity, stability and hence enhanced
performance.
Abstract: 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.
Abstract: This paper illustrates the effect of nano Magnesium
Hydroxide (MH) loading on the thermal properties of Low Density
Polyethylene (LDPE)/Poly (ethylene-co vinyl acetate) (EVA) nano
composite. Thermal studies were conducted, as it understanding is
vital for preliminary development of new polymeric systems.
Thermal analysis of nanocomposite was conducted using thermo
gravimetric analysis (TGA), and differential scanning calorimetry
(DSC). Major finding of TGA indicated two main stages of
degradation process found at (350 ± 25oC) and (480 ± 25oC)
respectively. Nano metal filler expressed better fire resistance as it
stand over high degree of temperature. Furthermore, DSC analysis
provided a stable glass temperature around 51 (±1oC) and captured
double melting point at 84 (±2oC) and 108 (±2oC). This binary
melting point reflects the modification of nano filler to the polymer
matrix forming melting crystals of folded and extended chain. The
percent crystallinity of the samples grew vividly with increasing filler
content. Overall, increasing the filler loading improved the
degradation temperature and weight loss evidently and a better
process and phase stability was captured in DSC.
Abstract: 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%.