The title compound, C(16)H(17)N(5)S, is in the thione form and crystallizes with two independent molecules in the asymmetric unit. In both molecules, the pentamethyleneimine five-membered ring adopts an envelope conformation, and in one of the molecules this ring shows positional disorder. The thione S and hydrazine N atoms are in the Z configuration with respect to the C-N bond.
Seeding is a versatile method for optimizing crystal growth. Coupling this technique with capillary counter diffusion crystallization enhances the size and diffraction quality of the crystals. In this article, crystals for organic solvent-tolerant recombinant elastase strain K were successfully produced through microseeding with capillary counter-diffusion crystallization. This technique improved the nucleation success rate with a low protein concentration (3.00 mg/mL). The crystal was grown in 1 M ammonium phosphate monobasic and 0.1 M sodium citrate tribasic dihydrate pH 5.6. The optimized crystal size was 1 × 0.1 × 0.05 mm³. Elastase strain K successfully diffracted up to 1.39 Å at SPring-8, Japan, using synchrotron radiation for preliminary data diffraction analysis. The space group was determined to be monoclinic space group P12(1)1 with unit cell parameters of a = 38.99 Ǻ, b = 90.173 Å and c = 40.60 Å.
Diacylglycerol at 1 or 6% was added into refined bleached and deodorized palm oil (RBDPO) and crystallized from the melt in a thermally controlled water bath at 22°C for 90 min. Slurries were withdrawn after 5, 15, 30, 60 and 90 min of crystallization for solid fat content (SFC) and crystal morphology studies. Crystallization was also performed in a similar manner using a Labmax reactor connected to a FBRM detector to obtain the information on crystal count and size distribution during crystallization. SFC of the slurries increased with increase in crystallization time up to a certain level followed by a plateau. SFC of RBDPO added with DAG was also higher with the increase in percentage of DAG added and no induction time was observed to initiate crystallization in RBDPO added with DAG. The addition of DAG caused rapid crystallization of RBDPO as observed by enhance nucleation and larger crystal size with increase in the percentages of DAG added.
Carbon nanotube reinforced aluminium matrix composites (Al-CNTs) have been widely used in aerospace and automotive industries where high quality and strength is required. The enhanced mechanical properties of Al-CNTs are closely related to processing technique due to challenges within production of these composite materials. In the current review, solid state processing techniques used for synthesizing Al-CNTs have been reviewed to provide an insight into the features and capabilities of each technique regarding the incorporation of CNT reinforcements. To conclude, the mechanical performance of Al-CNT composites is mainly decided by the capability of each technique in the dispersion of CNTs within the aluminum matrix.
Topological defect nucleation and boundary branching in crystal growth on a curved surface are two typical elastic instabilities driven by curvature induced stress, and have usually been discussed separately in the past. In this work they are simultaneously considered during crystal growth on a sphere. Phase diagrams with respect to sphere radius, size, edge energy and stiffness of the crystal for the equilibrium crystal morphologies are achieved by theoretical analysis and validated by Brownian dynamics simulations. The simulation results further demonstrate the detail of morphological evolution governed by these two different stress relaxation modes. Topological defect nucleation and boundary branching not only compete with each other but also coexist in a range of combinations of factors. Clarification of the interaction mechanism provides a better understanding of various curved crystal morphologies for their potential applications.
The effect of various multi-walled carbon nanotubes (MWNTs) on the tensile properties of thermoplastic natural rubber (TPNR) nanocomposite was investigated. The nanocomposite was prepared using melt blending method. MWNTs were added to improve the mechanical properties of MWNTs/TPNR composites in different compositions of 1, 3, 5, and 7 wt.%. The results showed that the mechanical properties of nanocomposites were affected significantly by the composition and the properties of MWNTs. SEM micrographs confirmed the homogenous dispersion of MWNTs in the TPNR matrix and promoted strong interfacial adhesion between MWNTs and the matrix which was improved mechanical properties significantly.
Aluminum substituted yttrium iron garnet nano particles with compositional variation of Y(3.0-x) A1(x)Fe5O12, where x = 0.0, 0.5, 1.0, 1.5, 2.0, 2.5 and 3.0 were prepared using sol gel technique. The X-ray diffraction results showed that the best garnet phase appeared when the sintering temperature was 800 degrees C. Nano-crystalline particles with high purity and sizes ranging from 20 to 100 nm were obtained. It was found that the aluminum substitution had resulted in a sharp fall of the d-spacing when x = 2, which we speculated is due to the preference of the aluminum atoms to the smaller tetrahedron and octahedron sites instead of the much larger dodecahedron site. High resolution transmission electron microscope (HRTEM) and electron diffraction (ED) patterns showed single crystal nanoparticles were obtained from this method. The magnetic measurement gave moderate values of initial permeability; the highest value of 5.3 was shown by sample Y3Fe5O12 at more than 100 MHz which was attributed to the morphology of the microstructure which appeared to be homogeneous. This had resulted in an easy movement of domain walls. The substitution of aluminum for yttrium is speculated to cause a cubic to rhombodedral structural change and had weakened the super-exchange interactions thus a fall of real permeability was observed. This might have created a strain in the sub-lattices and had subsequently caused a shift of resonance frequencies to more than 1.8 GHz when x > 0.5.
This paper presents the effects of calcination time and sintering temperature on the properties of CaCu(3)Ti(4)O(12). Electroceramic material of CaCu(3)Ti(4)O(12) was prepared using a modified mechanical alloying technique that covers several processes, which are preparation of raw material, mixing and ball milling for 5 hours, calcination, pellet forming and, sintering. The objective of this modified technique is to enable the calcination and sintering processes to be carried out at a shorter time and lower temperature. The x-ray diffraction (XRD) analysis result shows that a single-phase of CaCu(3)Ti(4)O(12) was completely formed by calcination at 750 degrees C for 12 hours. Meanwhile, the grain size of a sample sintered at 1050 degrees C for 24 hours is extremely large, in the range of 20-50 mum obtained from field emission scanning electron microscopy (FESEM) images. The dielectric constant value of 14,635 was obtained at 10 kHz by impedance (LCR) meter in the sintered sample at 1050 degrees C. However, the dielectric constant value of samples sintered at 900 and 950 degrees C is quite low, in the range of 52-119.
Purified thermostable recombinant L2 lipase from Bacillus sp. L2 was crystallized by the counter-diffusion method using 20% PEG 6000, 50 mM MES pH 6.5 and 50 mM NaCl as precipitant. X-ray diffraction data were collected to 2.7 A resolution using an in-house Bruker X8 PROTEUM single-crystal diffractometer system. The crystal belonged to the primitive orthorhombic space group P2(1)2(1)2(1), with unit-cell parameters a = 87.44, b = 94.90, c = 126.46 A. The asymmetric unit contained one single molecule of protein, with a Matthews coefficient (V(M)) of 2.85 A(3) Da(-1) and a solvent content of 57%.
Crystallization of the ionic liquid 3,3'-dimethyl-1,1'-(1,4-phenylenedimethylene)diimidazolium bis(tetrafluoroborate), C(16)H(20)N(4)(2+).2BF(4)(-), (I), from its solution in water has permitted the first single-crystal study of an imidazolium-based ionic liquid having a tetrafluoroborate ion as counter-ion. Despite the expectation that the anion would not participate in nonclassical hydrogen bonding, the ionic liquid features C-H...F hydrogen bonds. The dication lies about a center of inversion. The ionic liquid 3,3'-di-n-butyl-1,1'-(1,4-phenylenedimethylene)diimidazolium bis(trifluoromethanesulfonate), C(22)H(32)N(4)(2+).2CF(3)SO(3)(-), (II), features both C-H...F and C-H...O hydrogen bonds.
Refined bleached and deodorized palm oil (RBDPO) was crystallized from the melt in a thermally controlled water bath at 14 and 22°C for 90 min. Slurries were withdrawn after 5, 15, 30, 60 and 90 min of crystallization for crystal morphology studies. Crystallization was also performed in a similar manner using a Labmax reactor connected to a FBRM detector to obtain the information on crystal count and size distribution during crystallization. Based on the shape of the crystals viewed under the microscope, all crystals appeared as needle shaped spherulitic β´- form at both crystallization temperatures studied. Crystals were slightly larger with increase in crystallization time and at higher crystallization temperature (22°C). Crystals size range between 4.34 to 22.29µm. FBRM recorded high count of crystals with increased in crystallization time and at lower temperature (14°C).
The experiment aims to investigate the effect of high energy milling to the crystallite size of α-alumina. The starting material used is α-alumina powder with starting crystal size of 86nm. This powder was milled at different time ranges from 0 to 60 minutes and milling speed ranges from 400 rpm to 1100 rpm using a wet milling technique in corundum abrasive materials. The wet milling technique involved the use of water with the alumina to water ratio of 1:6.1. Samples prepared were then examined using the X-Ray Diffraction (XRD) to calculate the crystallite size and scanning electron microscope (SEM) was also used to determine changes in the morphology. Results from these analysis showed that the crystallite size will get smaller when milling speed and time of more than 600rpm and 30 minutes respectively were used. Optimum conditions to achieve the smallest crystal size of 79.7nm are 1000 rpm and 60 minutes.
The main purpose of this study was to analyzed and examined the cocoa butter samples from Sabah. This work presence the crystal phases present in cocoa butter sample thus proved the existence of polymorphs obtained from differential scanning calorimeter (DSC) analysis and confirmed by X-ray diffraction (XRD). The cocoa butter samples were extracted using a conventional method by Soxhlet Extraction method. Crystals were formed under controlled static and tempered conditions. Cocoa butter polymorphism demonstrates that it is the actual crystallization temperature, not the cooling rate that determines the polymorph that crystallizes.
Biodiesel is an attractive renewable energy source, which is suitable as a substitute to the non-renewablepetroleum diesel. However, it is plagued by its relatively bad cold flow behaviour. In this review, the factorsaffecting the cold flow of biodiesel, vis-à-vis the contradicting requirement of good cold flow and good ignitionproperties, are discussed. Fuel filter plugging, and crystallization of biodiesel are considered, together with thecold flow properties such as Pour Point (PP), Cloud Point (CP), Cold Filter Plugging Point (CFPP) and LowTemperature Filterability Test (LTFT). In addition, various methods used to improve the cold flow of biodieselare also presented, with a special emphasis laid on the effects of these methods in reducing the Cloud Point.Strategies to improve cold flow, and yet maintaining the good ignition quality of biodiesel, are also proposed.As far as the cold flow of biodiesel is concerned, desirable attributes of its esters are short, unsaturated andbranched carbon chains. However, these desirable attributes present opposing properties in terms of ignitionquality and oxidation stability. This is because esters with short, unsaturated and branched carbon chainspossess very good cold flow but poor ignition quality and oxidation stability. The target is therefore to producebiodiesel with good cold flow, sufficient ignition quality, and good oxidation stability. This target proves tobe quite difficult and is a major problem in biodiesel research. New frontiers in this research might be thedesign of the new cold flow improvers that is similar to those used in the petroleum diesel but is tailored forbiodiesel. Genetic modifications of the existing feedstock are also desirable but the food uses of this particularfeedstock should always be taken into consideration.
Fat content and macroscopic properties of fat network formulation result in final products in chocolate industry. The knowledge of physical properties is required in regard to stability of final food products resulting to quality. The study was carried out to investigate the thermal behavior, solid fat content and hardness of Rambutan fat (RF), cocoa butter and mixtures between two fats. The results found that the mixtures can be compatibility; the cocoa butter indicated the higher of solid fat content at room temperature more than RF and other mixtures. The RF had the highest melting point in both non-stabilized and stabilized form among cocoa butter and their mixtures. The hardness behavior showed lower in the mixture 1 and RF. For the phase behavior of crystallization exhibited the similar for all samples whereas the time of crystallization and temperatures were different. Therefore, the RF might be possible source of cocoa butter substitute with suitable proportion in the manufacturing chocolate and confectionery products.
In this work, the preparation of ZnO, N-doped ZnO (NZO), Al-doped ZnO (AZO) and Al, N-doped ZnO (ANZO) thin films by the sol-gel spin-coating method is reported. The structural properties and surface morphologies of films were characterized by X-ray diffraction (XRD) and field emission scanning electron microscope (FE-SEM). The optical properties of the films were interpreted from their transmission spectra using UV-VIS spectrophotometer. The XRD and SEM results disclosed that the crystallization quality and grain size of as-prepared films were highly influenced by N and Al doping. UV-VIS spectrophotometer results indicated that Al and N additives could significantly enhance the optical transparency and induce the blue-shift in optical bandgap of ZnO films.
Thin films of barium strontium titanate (Ba0.6Sr0.4TiO3) perovskite system are promising candidates for microelectronic devices that can be integrated with semiconductor technology. Ba0.6Sr0.4TiO3 thin films have been prepared onto BST/TiO2/RuO2/SiO2/Si substrate using the spin coating and sol-gel process. Then the samples were subsequently annealed at 600oC, 650oC and 700oC for 60 minutes in air. The microstructure and dielectric properties show that the crystallization improved as the annealing temperature was increased. All of the films have nanometer grain size. The average grain size of the films increased as the temperature was increased. The dielectric constant and ac conductivity of the films also increased as the average grain size increased. These results showed that the microstructure and dielectric properties depend on the annealing temperature.
The stearin fraction of palm-based diacylglycerol (PDAGS) was produced from dry fractionation of palm-based diacylglycerol (PDAG). Bakery shortening blends were produced by mixing PDAGS with either palm mid fraction, PMF (PDAGS/PMF), palm olein, POL(PDAGS/POL) or sunflower oil, SFO (PDAGS/SFO) at PDAGS molar fraction of XPDAGS=0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%. The physicochemical results obtained indicated that C16:0 and C18:1 were the dominant fatty acids for PDAGS/PMF and PDAGS/POL, while C18:1 and C18:2 were dominant in the PDAGS/SFO mixtures. SMP and SFC of the PDAGS were reduced with the addition of PMF, POL and SFO. Binary mixtures of PDAGS/PMF had better structural compatibility and full miscibility with each other. PDAGS/PMF and PDAGS/SFO crystallised in β'+β polymorphs in the presence of 0.4-0.5% PDAGS while PDAGS/POL resulted in β polymorphs crystal. The results gave indication that PDAGS: PMF at 50%:50% and 60%:40% (w/w) were the most suitable fat blend to be used as bakery shortening.
Piroxicam is a nonsteroidal anti-inflammatory drug with low aqueous solubility which exhibits polymorphism. The present study was carried out to develop polymorphs of piroxicam with enhanced solubility and dissolution rate by the crystal modification technique using different solvent mixtures prepared with PEG 4000 and PVP K30. Physicochemical characteristics of the modified crystal forms of piroxicam were investigated by X-ray powder diffractometry, FT-IR spectrophotometry and differential scanning calorimetry. Dissolution and solubility profiles of each modified crystal form were studied and compared with pure piroxicam. Solvent evaporation method (method I) produced both needle and cubic shaped crystals. Slow crystallization from ethanol with addition of PEG 4000 or PVP K30 at room temperature (method II) produced cubic crystal forms. Needle forms produced by method I improved dissolution but not solubility. Cubic crystals produced by method I had a dissolution profile similar to that of untreated piroxicam but showed better solubility than untreated piroxicam. Cubic shaped crystals produced by method II showed improved dissolution, without a significant change in solubility. Based on the XRPD results, modified piroxicam crystals obtained by method I from acetone/benzene were cube shaped, which correlates well with the FTIR spectrum; modified needle forms obtained from ethanol/methanol and ethanol/acetone showed a slight shift of FTIR peak that may be attributed to differences in the internal structure or conformation.
The Burstein-Moss shift and band gap narrowing of sputtered indium-doped zinc oxide (IZO) thin films are investigated as a function of carrier concentrations. The optical band gap shifts below the carrier concentration of 5.61 × 1019 cm-3 are well-described by the Burstein-Moss model. For carrier concentrations higher than 8.71 × 1019 cm-3 the shift decreases, indicating that band gap narrowing mechanisms are increasingly significant and are competing with the Burstein-Moss effect. The incorporation of In causes the resistivity to decrease three orders of magnitude. As the mean-free path of carriers is less than the crystallite size, the resistivity is probably affected by ionized impurities as well as defect scattering mechanisms, but not grain boundary scattering. The c lattice constant as well as film stress is observed to increase in stages with increasing carrier concentration. The asymmetric XPS Zn 2p3/2 peak in the film with the highest carrier concentration of 7.02 × 1020 cm-3 suggests the presence of stacking defects in the ZnO lattice. The Raman peak at 274 cm-1 is attributed to lattice defects introduced by In dopants.