The substrate effects on surface morphologies, crystal structures, and magnetic properties of the sputter-deposited FePt thin films on Corning 1737, normal glass, and Si wafer substrates, respectively, were investigated. High in-plane coercivities of 10 kOe were obtained for the air-annealed films on Corning 1737 and Si wafer, where both films similarly have granular-like morphologies. Besides, increasing grain size and surface roughness of all the FePt films with the post-anneal temperature were observed. Moreover, partially separated grains were seen in the film on Si wafer, where the formation of Fe silicides during post-anneal is suspected, in which has enhanced the magnetic ordering.
The title compound, 2C14H14N4O·H2O, comprises a neutral mol-ecule containing a central pyrazol-3-one ring flanked by an N-bound phenyl group and a C-bound 5-methyl-1H-pyrazol-3-yl group (at positions adjacent to the carbonyl substituent), its zwitterionic tautomer, whereby the N-bound proton of the central ring is now resident on the pendant ring, and a water mol-ecule of crystallization. Besides systematic variations in geometric parameters, the two independent organic mol-ecules have broadly similar conformations, as seen in the dihedral angle between the five-membered rings [9.72 (9)° for the neutral mol-ecule and 3.32 (9)° for the zwitterionic tautomer] and in the dihedral angles between the central and pendant five-membered rings [28.19 (8) and 20.96 (8)° (neutral mol-ecule); 11.33 (9) and 11.81 (9)°]. In the crystal, pyrazolyl-N-H⋯O(carbon-yl) and pyrazolium-N-H⋯N(pyrazol-yl) hydrogen bonds between the independent organic mol-ecules give rise to non-symmetric nine-membered {⋯HNNH⋯NC3O} and {⋯HNN⋯HNC3O} synthons, which differ in the positions of the N-bound H atoms. These aggregates are connected into a supra-molecular layer in the bc plane by water-O-H⋯N(pyrazolide), water-O-H⋯O(carbon-yl) and pyrazolyl-N-H⋯O(water) hydrogen bonding. The layers are linked into a three-dimensional architecture by methyl-C-H⋯π(phen-yl) inter-actions. The different inter-actions, in particular the weaker contacts, formed by the organic mol-ecules are clearly evident in the calculated Hirshfeld surfaces, and the calculated electrostatic potentials differentiate the tautomers.
The sintering behaviour of a commercial HA and synthesized HA was investigated over the temperature range of 700 degrees C to 1400 degrees C in terms of phase stability, bulk density, Young's modulus and Vickers hardness. In the present research, a wet chemical precipitation reaction was successfully employed to synthesize a submicron, highly crystalline, high purity and single phase stoichiometric HA powder that is highly sinteractive particularly at low temperature regimes below 1100 degrees C. It has been revealed that the sinterability of the synthesized HA was significantly greater than that of the commercial HA. The temperature for the onset of sintering and the temperature required to achieve densities above 98% of theoretical value were approximately 150 degrees C lower for the synthesized HA than the equivalent commercial HA. Nevertheless, decomposition of HA phase upon sintering was not observed in the present work for both powders.
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.
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.
A solution-phase route has been considered as the most promising route to synthesize noble nanostructures. A majority of their synthesis approaches of calcium carbonate (CaCO3) are based on either using fungi or the CO2 bubbling methods. Here, we approached the preparation of nano-precipitated calcium carbonate single crystal from salmacis sphaeroides in the presence of zwitterionic or cationic biosurfactants without external source of CO2. The calcium carbonate crystals were rhombohedron structure and regularly shaped with side dimension ranging from 33-41 nm. The high degree of morphological control of CaCO3 nanocrystals suggested that surfactants are capable of strongly interacting with the CaCO3 surface and control the nucleation and growth direction of calcium carbonate nanocrystals. Finally, the mechanism of formation of nanocrystals in light of proposed routes was also discussed.
Nanocomposites of Zn/Al-layered double hydroxide(anthraquinone-2,6-disulfonate) were synthesized by spontaneous direct assembly of inorganic and organic phases from aqueous solution. Powder X-ray diffraction patterns showed that a pure, single nanocomposite phase of good crystallinity was obtained using 1.0 M antraquinone-2,6-disulfonate ion (AQ26) and aging at 80 degrees C using conventional heating for 7 days or 0.5 h under microwave radiation, and these samples are denoted as ZAAN26C or ZAAN26MH, respectively. Zn/Al-nitrate-layered double hydroxide synthesized by a conventional method (ZANLC) showed a basal spacing of 8.3 A while both the nanocomposites showed 18.8 A as a result of AQ26 intercalation. FTIR study showed that the resulting nanocomposites are free from nitrate, the co-anion present in the mother liquor, indicating that only AQ26 is preferred during intercalation for the formation of the nanocomposite. The Brunauer, Emmet and Teller (BET) and micropore surface areas for ZAAN26C decreased relative to the ZANLC from 16.2 to 4.7 and 1.6 to 1.3 m2/g, respectively. These results indicate that AQ26 can be rapidly interdcalated in layered double hydroxide using microwave-aging resulting in a nanocomposite.
Control synthesis of high quality large-area graphene on transition metals (TMs) by chemical vapor deposition (CVD) is the most fascinating approach for practical device applications. Interaction of carbon atoms and TMs is quite critical to obtain graphene with precise layer number, crystal size and structure. Here, we reveal a solid phase reaction process to achieve Cu assisted graphene growth in nanoscale by in-situ transmission electron microscope (TEM). Significant structural transformation of amorphous carbon nanofiber (CNF) coated with Cu is observed with an applied potential in a two probe system. The coated Cu particle recrystallize and agglomerate toward the cathode with applied potential due to joule heating and large thermal gradient. Consequently, the amorphous carbon start crystallizing and forming sp(2) hybridized carbon to form graphene sheet from the tip of Cu surface. We observed structural deformation and breaking of the graphene nanoribbon with a higher applied potential, attributing to saturated current flow and induced Joule heating. The observed graphene formation in nanoscale by the in-situ TEM process can be significant to understand carbon atoms and Cu interaction.
Jackfruit is now receiving extensive attention as a new source of starch. However, jackfruit seeds are discarded as waste, although they are rich in starch. The functional properties of the starches were investigated from new Chinese jackfruit species. All the starches have a high amylose (26.56-38.34%) with a potential to become functional foods rich in resistant starch. The jackfruit starches varied from trigonal and tetragonal, round to semi-oval/bell shapes and showed significant variations in particle sizes (5.53-14.46μm). These variations led to significant differences in their functional properties, and significant correlations were found in their pasting, thermal, crystal and texture parameters. Hierarchical cluster analysis sorted the samples into three groups of 1) Malaysia 8 (M8) and ZhenZhu (ZZ); 2) Malaysia 2, Malaysia 3 and Malaysia 4, (M2, M3, M4); and 3) Xiangyinsuo 11, Xiangyinsuo 4, Xiangyinsuo 3 and Xiangyinsuo 2 (X11, X4, X3, X2). The first group could be used as food thickening or gelling agents. The second group could be applied in glutinous foods. The third group make them suitable for fillings in confectionery or weaning foods.
The effects of scanning rates (1, 5, 10 and 20 degrees C/min) on the DSC cooling profiles of 11 vegetable oils have been determined in order to monitor peak transition temperatures, onset temperatures and crystallisation enthalpies. Triacylglycerol (TAG) profiles and iodine value analyses were used to complement the DSC data. The melted samples exhibited complicated crystallising exotherms. As the cooling rate increased, the crystallisation temperature decreased and the breadth of the crystallisation exotherm on cooling from the melt increased. In addition, the intensity of the exothermic peak increased somewhat when the cooling rate was increased. At slow cooling rates, TAG had more time to interact. It is conceivable that, at a low cooling rate (1 degree C/min), a prominent exotherm would be observed on crystallisation of vegetable oils and fats. The occurrence of one exotherm upon cooling indicated the co-crystallisation of the TAG upon slow cooling. On the basis of the corollary results obtained, vegetable oils may be differentiated by their onset temperature (Ton) values in the DSC cooling curves. Generally, there was a shift of Ton toward lower values with increasing cooling rates.
The effects of microwave on drug release properties of pectin films carrying sulfanilamide (SN-P), sulfathiazole (ST-P) and sulfamerazine (SM-P) of high to low aqueous solubilities were investigated. These films were prepared by solvent evaporation technique and treated by microwave at 80 W for 5-40 min. Their profiles of drug dissolution, drug content, matrix interaction and matrix crystallinity were determined by drug dissolution testing, drug content assay, differential scanning calorimetry, X-ray diffractometry and scanning electron microscopy techniques. Microwave induced an increase in matrix amorphousness but lower drug release propensity with a greater retardation extent in SN-P films, following a rise in strength of matrix interaction. A gain in amorphous structure does not necessarily increase the drug release of film. Microwave can possibly retard drug release of pectin film carrying water-soluble drug through modulating its state of matrix interaction.
Dark chocolates filled with palm mid-fraction (PMF) were stored at different temperatures to evaluate the physical and chemical changes. Storage at low temperature (18 degrees C) reduces the PMF migration to negligible extent. Higher storage temperatures (30 and 35 degrees C) increased the PMF migration from the filling centre into the chocolate coating. As a consequence of fat migration, fatty acid composition, triglyceride composition, hardness, solid fat content, melting point and polymorphic structure changed, leading to bloom formation, which started by fat migration and was influenced by recrystallization tendency within the chocolate coating.
White rice husk ash (RHA), an agriculture waste containing crystalline tridymite and alpha-cristobalite, was used as a silica source for zeolite Beta synthesis. The crystallization of zeolite Beta from RHA at 150 degrees C in the presence of tetraethylammonium hydroxide was monitored by XRD, FTIR and (29)Si MAS NMR techniques. It was found that zeolite Beta started to form after 12h and the complete crystallization of zeolite Beta phase was achieved after 2d. XRD, (29)Si MAS NMR and solid yield studies indicate that the transformation mechanism of silica present in RHA to zeolite Beta involves dissolution of the ash, formation of an amorphous aluminosilicate after 6h of crystallization, followed by dissolution in the mother liquor and final transformation to pure zeolite Beta crystals.
Anomers and epimers α- and β-gluco and -galactosides are expected to behave differently. However, recent results on a series of Guerbet glycosides have indicated similar liquid crystal clearing temperatures for pure β-glucosides and the corresponding α-galactosides. This observation has led to speculation on similarities in the self-assembly interactions between the two systems, attributed to the trans-configuration of the 4-OH group and the hydrophobic aglycon. Previous simulations on related bilayers systems support this hypothesis, by relating this clearing transition temperature to intralayer (sugar-sugar) hydrogen bonding. In order to confirm the hypothesis, the comparison was expanded to include the cis-configurated pair, that is, α-gluco/β-galactoside. A set of α-configurated Guerbet glucosides as well as octyl α-galactoside were prepared and their thermotropic phase behavior studied. The data obtained enabled a complete comparison of the isomers of interest. While the results in general are in line with a pairing of the stereo-isomers according to the indicated cis/trans-configuration, differences within the pairs can be explained based on the direction of hydrogen bonds from a simple modeling study.
The current study focused on the microscopic studies of a native Bacillus thuringiensis strain isolated from Malaysia, Bt-S84-13a, that produced an unusual crystal type. Primary detection of parasporal inclusions using a phase contrast microscope presented one to two small crystal proteins in the sporulating cells of Bt-S84-13a. Compound light microscopic examination of autolysed Bt-S84-13a cells stained with 0.133% Coomassie Brilliant Blue showed two types of crystal morphology: small crystals independent of spores and spore-associated crystals. Surface structure analysis with a scanning electron microscope revealed spherical-like, coarse and wrinkled-looking crystal in Bt-S84-13a. A close-up observation of the crystal morphology using a transmission electron microscope also demonstrated two parasporal inclusions in Bt-S84-13a. One inclusion was deposited against the forespore and was in a shape of incomplete rectangular. Another smaller inclusion was developed within the exosporium and was rectangular in shape. However, the latter inclusion was found lack in another bacterial cell which was still in the early stages of sporulation. This unique crystal morphology may imply some biological potential in Bt-S84-13a.
The sintering behaviour of synthesized HA powder that was calcined at various temperatures ranging from 700 degrees C to 1000 degrees C was investigated in terms of phase stability, bulk density, Young's modulus and Vickers hardness. The calcination treatment resulted in higher crystallinity of the starting HA powder. Decomposition of HA phase to form secondary phases was not observed in all the calcined powders. The results also indicated that powder calcination (up to 900 degrees C) prior to sintering has negligible effect on the sinterability of the HA compacts. However, powder calcined at 1000 degrees C was found to be detrimental to the properties of sintered hydroxyapatite bioceramics.
Crystals isolated from Hylocereus polyrhizus were analyzed using four different approaches--X-ray Crystallography, High Performance Liquid Chromatography (HPLC), Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) and Nuclear Magnetic Resonance (NMR) and identified as myo-inositol. The X-ray crystallography analysis showed that the unit-cell parameters were: a = 6.6226 (3) Å, b = 12.0462 (5) Å, c = 18.8942 (8) Å, α = 90.00, β = 93.98, δ = 90.00. The purity of the crystals were checked using HPLC, whereupon a clean single peak was obtained at 4.8 min with a peak area of 41232 μV*s. The LC-MS/MS technique, which is highly sensitive and selective, was used to provide a comparison of the isolated crystals with a myo-inositol standard where the results gave an identical match for both precursor and product ions. NMR was employed to confirm the molecular structure and conformation of the crystals, and the results were in agreement with the earlier results in this study. The discovery of myo-inositol crystals in substantial amount in H. polyrhizus has thus far not been reported and this is an important finding which will increase the marketability and importance of H. polyrhizus as a crop with a wide array of health properties.
This study aims to evaluate the effect of sucrose replacer mixtures (erythritol, mannitol, or tagatose in combination with inulin or polydextrose) on the crystal morphology, particle size distribution, rheology, melting properties, and fat polymorphism of dark compound chocolate. The result showed that the replacer mixture's hygroscopicity, particle size, and sugar crystal shape might significantly impact dark compound chocolate's rheological and textural properties but had no substantial impact on the melting properties and fat crystallization. Mannitol-containing samples exhibited the highest rheological value, likely related to their high moisture content, small particle size, and elongated crystal shape. Due to the similar specific surface area and comparable D90 value, the sample containing erythritol-polydextrose mixture resulted in a similar (P ≥ 0.05) Casson yield value (46.184 ± 2.45 Pa) compared to the sample containing sucrose (38.348 ± 1.68 Pa). It could be a potential sucrose replacer in the dark compound chocolate.
The title compound, C16H10, crystallizes with four unique mol-ecules, designated 1-4, in the asymmetric unit of the monoclinic unit cell. None of the mol-ecules is planar, with the benzene rings of mol-ecules 1-4 inclined to one another at angles of 42.41 (4), 24.07 (6), 42.59 (4) and 46.88 (4)°, respectively. In the crystal, weak C-H⋯π(ring) interactions, augmented by even weaker C C-H⋯π(alkyne) contacts, generate a three-dimensional network structure with inter-linked columns of mol-ecules formed along the c-axis direction.