This is our initial response towards preparation of nano-inductors garnet for high operating frequencies strontium iron garnet (Sr3Fe5O12) denoted as SrIG and yttrium iron garnet (Y3Fe5O12) denoted as YIG. The garnet nano crystals were prepared by novel sol-gel technique. The phase and crystal structure of the prepared samples were identified by using X-ray diffraction analysis. SEM images were done to reveal the surface morphology of the samples. Raman spectra was taken for yttrium iron garnet (Y3Fe5O12). The magnetic properties of the samples namely initial permeability (micro), relative loss factor (RLF) and quality factor (Q-Factor) were done by using LCR meter. From the XRD profile, both of the Y3Fe5O12 and Sr3Fe5O12 samples showed single phase garnet and crystallization had completely occurred at 900 degrees C for the SrIG and 950 degrees C for the YIG samples. The YIG sample showed extremely low RLF value (0.0082) and high density 4.623 g/cm3. Interesting however is the high Q factor (20-60) shown by the Sr3Fe5O12 sample from 20-100 MHz. This high performance magnetic property is attributed to the homogenous and cubical-like microstructure. The YIG particles were used as magnetic feeder for EM transmitter. It was observed that YIG magnetic feeder with the EM transmitter gave 39% higher magnetic field than without YIG magnetic feeder.
Hydroxyapatite (HAp) is an attractive bioceramics due to its similar composition to bone mineral and its ability to promote bone-implant interaction. However, its low strength has limited its application as load bearing implants. This paper presented a work focusing on the improvement of HAp mechanical property by synthesizing iron (Fe)-reinforced bovine HAp nanocomposite powders via mechanosynthesis method. The synthesis process was performed using high energy milling at varied milling time (3, 6, 9, and 12h). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM). Its mechanical properties were investigated by micro-Vicker's hardness and compression tests. Results showed that milling time directly influenced the characteristics of the nanocomposite powders. Amorphous BHAp was formed after 9 and 12h milling in the presence of HPO4(2-) ions. Continuous milling has improved the crystallinity of Fe without changing the HAp lattice structure. The nanocomposite powders were found in spherical shape, agglomerated and dense after longer milling time. The hardness and Young's modulus of the nanocomposites were also increased at 69% and 66%, respectively, as the milling time was prolonged from 3 to 12h. Therefore, the improvement of the mechanical properties of nanocomposite was attributed to high Fe crystallinity and homogenous, dense structure produced by mechanosynthesis.
Forsterite (Mg2SiO4) because of its exceptionally high fracture toughness which is close to that of cortical bones has been nominated as a possible successor to calcium phosphate bioceramics. Recent in vitro studies also suggest that forsterite possesses good bioactivity and promotes osteoblast proliferation as well as adhesion. However studies on preparation and sinterability of nanocrystalline forsterite remain scarce. In this work, we use a solid-state reaction with magnesium oxide (MgO) and talc (Mg3Si4(OH)2) as the starting precursors to synthesize forsterite. A systematic investigation was carried out to elucidate the effect of preparatory procedures including heat treatment, mixing methods and sintering temperature on development of microstructures as well as the mechanical properties of the sintered forsterite body.
Less sedimentation and convection in a microgravity environment has become a well-suited condition for growing high quality protein crystals. Thermostable T1 lipase derived from bacterium Geobacilluszalihae has been crystallized using the counter diffusion method under space and earth conditions. Preliminary study using YASARA molecular modeling structure program for both structures showed differences in number of hydrogen bond, ionic interaction, and conformation. The space-grown crystal structure contains more hydrogen bonds as compared with the earth-grown crystal structure. A molecular dynamics simulation study was used to provide insight on the fluctuations and conformational changes of both T1 lipase structures. The analysis of root mean square deviation (RMSD), radius of gyration, and root mean square fluctuation (RMSF) showed that space-grown structure is more stable than the earth-grown structure. Space-structure also showed more hydrogen bonds and ion interactions compared to the earth-grown structure. Further analysis also revealed that the space-grown structure has long-lived interactions, hence it is considered as the more stable structure. This study provides the conformational dynamics of T1 lipase crystal structure grown in space and earth condition.
Background: Fluoride is needed for the normal development of bone and teeth; in high levels, it affects developing teeth and bone. Dental fluorosis (DF) is caused by ingestion of excess fluoride mainly through drinking water.
Aim: The present study aims to observe and understand the histological changes of fluorosed teeth under light microscope (LM).
Materials and Methods: Teeth which were indicated for extractions for orthodontic or periodontal problems were selected. Thirty extracted teeth were selected with varying degrees of DF based on modified Dean's fluorosis index. Ground sections of these teeth were prepared and the sections were studied under binocular LM. Photomicrographs were taken under high power objective using 15 megapixels Nikon camera.
Results and Conclusion: Qualitative histologic changes in different grades of fluorosed teeth were evaluated in enamel, dentin, cementum and between their junctions. Fluoride interacts with enamel in both mineral phases and organic macromolecules by strong ionic and hydrogen bonds resulting in incomplete crystal growth at prism peripheries. This presents as hypomineralization of enamel and dentin, increased interglobular dentin, increased secondary curvatures and changes in cementum such as diffuse cementodentinal junction and increased thickness of Tomes' granular layer. Changes in the structure of the teeth with Dean's index below 2 and teeth with Dean's index of 2 and above were compared using Chi-square test. P value was found to be highly significant being 0.00047. Many of the features of dental fluorosis seen in the present study under light microscope are comparable to those results studied under specialized microscopes.
The in situ polymorphic forms and thermal transitions of refined, bleached and deodorized palm oil (RBDPO), palm stearin (RBDPS) and palm kernel oil (RBDPKO) were investigated using coupled X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Results indicated that the DSC onset crystallisation temperature of RBDPO was at 22.6°C, with a single reflection at 4.2Å started to appear from 23.4 to 17.1°C, and were followed by two prominent exothermic peaks at 20.1°C and 8.5°C respectively. Further cooling to -40°C leads to the further formation of a β'polymorph. Upon heating, a of β'→βtransformation was observed between 32.1 to 40.8°C, before the sample was completely melted at 43.0°C. The crystallization onset temperature of RBDPS was 44.1°C, with the appearance of the α polymorph at the same temperature as the appearance of the first sharp DSC exothermic peak. This quickly changed from α→β´ in the range 25 to 21.7°C, along with the formation of a small β peak at -40°C. Upon heating, a small XRD peak for the β polymorph was observed between 32.2 to 36.0°C, becoming a mixture of (β´+ β) between 44.0 to 52.5°C. Only the β polymorph survived further heating to 59.8°C. For RBDPKO, the crystallization onset temperature was 11.6°C, with the formation of a single sharp exothermic peak at 6.5°C corresponding to the β' polymorphic form until the temperature reached -40°C. No transformation of the polymorphic form was observed during the melting process of RBDPKO, before being completely melted at 33.2°C. This work has demonstrated the detailed dynamics of polymorphic transformations of PKO and PS, two commercially important hardstocks used widely by industry and will contribute to a greater understanding of their crystallization and melting dynamics.
Cadmium oxide semiconductor nanoparticles were produced using a water based mixture, incorporating cadmium nitrates, polyvinyl pyrrolidone (PVP), and calcination temperature. An X-ray diffraction (XRD) evaluation was conducted to determine the degree of crystallization of the semiconductor nanoparticles. In addition, scanning electron microscopy (SEM) was conducted to identify the morphological features of the nanoparticles. The typical particle sizes and particle dispersal were analyzed via the use of transmission electron microscopy (TEM). The findings provided further support for the XRD outcomes. To determine the composition phase, Fourier transform infrared spectroscopy (FT-IR) was conducted, as it indicated the existence of not only metal oxide ionic band in the selection of samples, but also the efficient removal of organic compounds following calcinations. The optical characteristics were demonstrated, so as to analyze the energy band gap via the use of a UV⁻Vis spectrophotometer. A reduced particle size resulted in diminution of the intensity of photoluminescence, was demonstrated by PL spectra. Plus, the magnetic characteristics were examined using an electron spin resonance (ESR) spectroscopy, which affirmed the existence of unpaired electrons.
This paper reports the post-processing ageing phenomena of thermoplastic sago starch (TPS) and plasticised sago pith waste (SPW), which were processed using twin-screw extrusion and compression moulding techniques. Wide angle X-ray diffraction (XRD) analyses showed that after processing, starch molecules rearranged into VH-type (which was formed rapidly right post processing and concluded within 4 days) and B-type (which was formed slowly over a period of months) crystallites. Evidence from Fourier transform infrared spectroscopy (FTIR) analyses corroborated the 2-stage crystallisation process, which observed changes in peak styles and peak intensities (at 1043 and 1026 cm-1) and bandnarrowing. Thermogravimetric analysis (TGA) studies showed that the thermal stability of plasticised SPW declined continuously for 90 days before gradual increments ensued. For all formulations tested, post-processing ageing led to drastic changes in the tensile strength (increased) and elongation at break (decreased). Glycerol and fibres restrained the retrogradation of starch molecules in TPS and SPW.
Different fractions of fully hydrogenated soybean oil (FHSBO) in soybean oil (10-30% w/w) and the addition of 1% salt (sodium chloride) were used to investigate the effect of high-pressure treatments (HP) on the crystallization behaviors and physical properties of the binary mixtures. Sample microstructure, solid fat content (SFC), thermal and rheological properties were analyzed and compared against a control sample (crystallized under atmospheric condition). The crystallization temperature (Ts) of all model fats under isobaric conditions increased quadratically with pressure until reaching a pressure threshold. As a result of this change, the sample induction time of crystallization (tc) shifted from a range of 2.74-0.82 min to 0.72-0.43 min when sample crystallized above the pressure threshold under adiabatic conditions. At the high solid mass fraction, the addition of salt reduced the pressure threshold to induce crystallization during adiabatic compression. An increase in pressure significantly reduced mean cluster diameter in relation to the reduction of tc regardless of the solid mass fraction. In contrast, the sample macrostructural properties (SFC, storage modulus) were influenced more significantly by solid mass fractions rather than pressure levels. The creation of lipid gel was observed in the HP samples at 10% FHSBO. The changes in crystallization behaviors indicated that high-pressure treatments were more likely to influence crystallization mechanisms at low solid mass fraction.
In recent years, there has been considerable interest in the use of natural fibers as potential reinforcing fillers in polymer composites despite their hydrophilicity, which limits their widespread commercial application. The present study explored the fabrication of nanocomposites by melt mixing, using an internal mixer followed by a compression molding technique, and incorporating rice husk (RH) as a renewable natural filler, montmorillonite (MMT) nanoclay as water-resistant reinforcing nanoparticles, and polypropylene-grafted maleic anhydride (PP-g-MAH) as a compatibilizing agent. To correlate the effect of MMT delamination and MMT/RH dispersion in the composites, the mechanical and thermal properties of the composites were studied. XRD analysis revealed delamination of MMT platelets due to an increase in their interlayer spacing, and SEM micrographs indicated improved dispersion of the filler(s) from the use of compatibilizers. The mechanical properties were improved by the incorporation of MMT into the PP/RH system and the reinforcing effect was remarkable as a result of the use of compatibilizing agent. Prolonged water exposure of the prepared samples decreased their tensile and flexural properties. Interestingly, the maximum decrease was observed for PP/RH composites and the minimum was for MMT-reinforced and PP-g-MAH-compatibilized PP/RH composites. DSC results revealed an increase in crystallinity with the addition of filler(s), while the melting and crystallization temperatures remained unaltered. TGA revealed that MMT addition and its delamination in the composite systems improved the thermal stability of the developed nanocomposites. Overall, we conclude that MMT nanoclay is an effective water-resistant reinforcing nanoparticle that enhances the durability, mechanical properties, and thermal stability of composites.
Cu2ZnSnS4 (CZTS) ink was synthesized from metal chloride precursors, sulfur, and oleylamine (OLA), as a ligand by a simple and low-cost hot-injection method. Thin films of CZTS were then prepared by spin coating, followed by thermal annealing. The effects of the fabrication parameters, such as ink concentration, spinning rate, and thermal treatment temperatures on the morphology and structural, optical, and electrical properties of the films were investigated. As expected, very thin films, for which the level of transmittance and band-gap values increase, can be obtained either by reducing the concentration of the inks or by increasing the rate of spinning. Moreover, the thermal treatment affects the phase formation and crystallinity of the film, as well as the electrical conductivity, which decreases at a higher temperature.
This study explores the effect of physical aging and/or crystallization on the supersaturation potential and crystallization kinetics of amorphous active pharmaceutical ingredients (APIs). Spray-dried, fully amorphous indapamide, metolazone, glibenclamide, hydrocortisone, hydrochlorothiazide, ketoconazole, and sulfathiazole were used as model APIs. The parameters used to assess the supersaturation potential and crystallization kinetics were the maximum supersaturation concentration (Cmax,app), the area under the curve (AUC), and the crystallization rate constant (k). These were compared for freshly spray-dried and aged/crystallized samples. Aged samples were stored at 75% relative humidity for 168 days (6 months) or until they were completely crystallized, whichever came first. The solid-state changes were monitored with differential scanning calorimetry, Raman spectroscopy, and powder X-ray diffraction. Supersaturation potential and crystallization kinetics were investigated using a tenfold supersaturation ratio compared to the thermodynamic solubility using the µDISS Profiler. The physically aged indapamide and metolazone and the minimally crystallized glibenclamide and hydrocortisone did not show significant differences in their Cmax,app and AUC when compared to the freshly spray-dried samples. Ketoconazole, with a crystalline content of 23%, reduced its Cmax,app and AUC by 50%, with Cmax,app being the same as the crystalline solubility. The AUC of aged metolazone, one of the two compounds that remained completely amorphous after storage, significantly improved as the crystallization kinetics significantly decreased. Glibenclamide improved the most in its supersaturation potential from amorphization. The study also revealed that, besides solid-state crystallization during storage, crystallization during dissolution and its corresponding pathway may significantly compromise the supersaturation potential of fully amorphous APIs.
The influence of diacylglycerol (DAG) combined with polyglycerol polyricinoleate (PGPR) on the stability of water-in-oil (W/O) emulsions containing hydrogenated palm oil (HPO) was studied. Polarized light microscope revealed that DAG promoted HPO to crystallize at the water-oil interface, providing the combination of Pickering and network stabilization effects. It was proposed that the molecular compatibility of fatty acids in DAG with HPO accounted for the promotional effect. The interfacial crystallization of DAG together with the surface activity of PGPR led to the formation of emulsions with uniform small droplets and high freeze-thaw stability. Further exploration of physical properties indicated that the combination of DAG and PGPR dramatically improved the emulsion's viscoelasticity and obtained a larger deformation yield. Water droplets in DAG-based emulsions acted as active fillers to improve the network rigidity. Therefore, DAG is a promising material to be used as emulsifier to enhance the physical stability of W/O emulsions.
Polylactic acid (PLA), a potential alternative material for single use plastics, generally portrays a slow crystallization rate during melt-processing. The use of a nanomaterial such as cellulose nanofibers (CNF) may affect the crystallization rate by acting as a nucleating agent. CNF at a certain wt.% has been evidenced as a good reinforcement material for PLA; nevertheless, there is a lack of information on the correlation between the amount of CNF in PLA that promotes its functionality as reinforcement material, and its effect on PLA nucleation for improving the crystallization rate. This work investigated the nucleation effect of PLA incorporated with CNF at different fiber loading (1-6 wt.%) through an isothermal and non-isothermal crystallization kinetics study using differential scanning calorimetry (DSC) analysis. Mechanical properties of the PLA/CNF nanocomposites were also investigated. PLA/CNF3 exhibited the highest crystallization onset temperature and enthalpy among all the PLA/CNF nanocomposites. PLA/CNF3 also had the highest crystallinity of 44.2% with an almost 95% increment compared to neat PLA. The highest crystallization rate of 0.716 min-1 was achieved when PLA/CNF3 was isothermally melt crystallized at 100 °C. The crystallization rate was 65-fold higher as compared to the neat PLA (0.011 min-1). At CNF content higher than 3 wt.%, the crystallization rate decreased, suggesting the occurrence of agglomeration at higher CNF loading as evidenced by the FESEM micrographs. In contrast to the tensile properties, the highest tensile strength and Young's modulus were recorded by PLA/CNF4 at 76.1 MPa and 3.3 GPa, respectively. These values were, however, not much different compared to PLA/CNF3 (74.1 MPa and 3.3 GPa), suggesting that CNF at 3 wt.% can be used to improve both the crystallization rate and the mechanical properties. Results obtained from this study revealed the dual function of CNF in PLA nanocomposite, namely as nucleating agent and reinforcement material. Being an organic and biodegradable material, CNF has an increased advantage for use in PLA as compared to non-biodegradable material and is foreseen to enhance the potential use of PLA in single use plastics applications.
The main physical properties of ferroelectric crystals are described, and the macroscopic and microscopic viewpoints are discussed along with some applications, such as in capacitors and nonlinear optics. The emphasis is on physical understanding, while the mathematical level is kept to a minimum or supplemented by graphical representations to make the article more accessible.
Poly(lactic acid) (PLA)-based nanocomposites filled with graphene nanoplatelets (xGnP) that contains epoxidized palm oil (EPO) as plasticizer were prepared by melt blending method. PLA was first plasticized by EPO to improve its flexibility and thereby overcome its problem of brittleness. Then, xGnP was incoporated into plasticized PLA to enhance its mechanical properties. Plasticized and nanofilled PLA nanocomposites (PLA/EPO/xGnP) showed improvement in the elongation at break by 3322% and 61% compared to pristine PLA and PLA/EPO, respectively. The use of EPO and xGnP increases the mobility of the polymeric chains, thereby improving the flexibility and plastic deformation of PLA. The nanocomposites also resulted in an increase of up to 26.5% in the tensile strength compared with PLA/EPO blend. XRD pattern showed the presence of peak around 26.5° in PLA/EPO/xGnP nanocomposites which corresponds to characteristic peak of graphene nanoplatelets. Plasticized PLA reinforced with xGnP showed that increasing the xGnP content triggers a substantial increase in thermal stability. Crystallinity of the nanocomposites as well as cold crystallization and melting temperature did not show any significant changes upon addition of xGnP. However, there was a significant decrease of glass transition temperature up to 0.3wt% of xGnP incorporation. The TEM micrograph of PLA/EPO/xGnP shows that the xGnP was uniformly dispersed in the PLA matrix and no obvious aggregation was observed.
Changes in molecular structure configuration during strain induced crystallisation of an amorphous Poly(Lactic Acid) (PLA 4032D) polymer was monitored in-situ by simultaneously recording the wide angle x-ray scattering (WAXS) and small angle x-ray scattering (SAXS) patterns together with polymer deformation images and force data. The amorphous chain orientation from the beginning of deformation until the onset of crystallisation was studied from the WAXS patterns. The true mechanical behaviour described by the true stress-true strain curve related to an amorphous chain orientation exhibited a linear behaviour. Approaching critical amorphous orientation, the true stress-true strain curve deviated from linear into non-linear behaviour. After the onset of crystallization, when the deformed polymer became a semicrystalline state, the true mechanical behaviour exhibited true strain hardening which greatly affected by the formation of the morphology. The gradual true strain hardening was associated with the formation of micro-fibrillar structure containing thin crystallite morphology whilst sharp increased in true strain hardening was associated with the formation of stacked lamellar morphology in the form of macro-lattice structure. The study was accomplished by the application of high brilliance synchrotron radiation at beamline ID2 of ESRF, Grenoble in France and the usage of the high contrast resolution of WAXS and SAXS charge-couple device (CCD) camera as well as 40 milliseconds temporal resolution of data acquisition system.
Indialite or α-cordierite was synthesized by glass crystallization method using mainly talc and kaolin and with small amount of MgO, Al2O3, SiO2 to compensate the chemical formulation of non-stoihiometric compositions of cordierite. (3MgO.1.5Al2O3.5SiO2). B2O3, P2O5 and CaO was also added to decrease the melting and sintering temperature of cordierite. The glasses were pelletized and sintered from 850 o C up to 1050 o C. Phase compositions of both heat treated glass was quantified by X-ray powder diffraction data by the Rietveld method using TOPAS Ver 3 software. Result shows that about 60wt% of α cordierite has successfully crystallized at 850 o C. Beside secondary phases (forsterite) which come from initial raw materials, phases from grinding media were also presents in the sample. The contamination was considered high since it has reacted with existence phases to form a new phase at higher temperature. Without any contamination from grinding it was expected to obtain more than 90wt% α cordierite using the same composition.
In order to modify the self-assembly of sucrose esters (SEs) in sunflower oil, we added sunflower lecithin (SFL) as co-surfactant. It is hypothesized that SFL modifies the self-assembly of SEs by interrupting the extensive hydrogen bonding between SEs monomers. The addition of SFL into SEs induced gelation of the mixed surfactant system oleogels at all studied ratios. The 7:3 SEs:SFL combination showed enhanced rheological properties compared to the other studied ratios, which suggests better molecular ordering induced by SFL. The modifications might have been caused by interference in the hydrogen bonding, connecting the polar heads of SEs molecules in the presence of SFL. This effect was confirmed by thermal behavior and small angle X-ray diffraction (SAXD) analysis. From the crystallization and melting analyses, it was shown that the peak temperature, shape and enthalpy decreased as the SFL ratio increases. Meanwhile, the bi-component oleogels exhibited new peaks in the SAXD profile, which imply a self-assembly modification. The microscopic study through polarized and electrons revealed a change in the structure. Therefore, it can be concluded that a synergistic effect between SEs and SFL, more particularly at 7:3 ratio, towards sunflower oil structuring could be obtained. These findings shed light for greater applications of SEs as structuring and carrier agent in foods and pharmaceutical.
Cellulose was extracted from rice husk (RH) using an integrated delignification process using alkaline treatment and acid hydrolysis (concentrated HNO3) for lignocellulosic biomass dissolution. Cellulose yield and quality were assessed through analysis of lignocellulosic content, thermogravimetric, functional group, X-ray diffraction, and surface morphology. HNO3 treatment showed an increment (2.01-fold) in the cellulose content and some enhancement in the crystallinity of cellulose (up to 40.8%). A slight increase was observed in thermal properties from 334.6 °C to 339.3 °C. Economic analysis showed chlorine extraction produce higher cellulose recovery (58%) as compared to HNO3 (26.7%) with the total cost of operation using HNO3 was double compared to chlorine extraction. The economic feasibility of HNO3 can be improved using various progress in the pre-treatment process, chemical recycling and cellulose recovery process since adopting it is crucial for environmental sustainability.