Modeling of recrystallization behaviour of AA6xxx aluminum alloy during extrusion process

An innovative approach was introduced for the development of a AA6063 recrystallization model.This method incorporated a regression-based technique for the determination of material constants and introduced novel equations for assessing the grain size evolution.Calibration and validation of this methodology involved a combination of experimentally acquired microstructural data from the extrusion of three different AA6063 profiles and results from the simulation using the Qform Extrusion UK finite element code.The outcomes proved the agreement between experimental findings and numerical prediction of the microstructural evolution.The trend of the grain size variation based on different process parameters was accurately simulated,both after dynamic and static recrystallization,with an error of less than 25% in almost the whole sampling computations.

Optimal Conditions for the Purification of Sesamin by Recrystallization

[Objective] Sesamin has been widely used in healthy food and medicines in recent years due to its prominent biological functions. This study was aimed to determine the optimal parameters for sesamin recrystallization, to obtain high-quality and high-purity sesamin. [Method] The effects of solid-liquid ratio, heating tempera- ture and cooling temperature on sesamin recrystallization were investigated by sin- gle-factor experiments and orthogonal array testing （ORT）. The purity of resulting sesamJn was investigated by HPLC, [Result] The optimal conditions for the purifica- tion of sesamin were solid-liquid ratio of 1：10, heating temperature of 45 ℃ and cooling temperature of 25 ℃. Under these conditions, the purity of sesamin reached 95.26%. [Conclusion] Recrystallization is an effective technique to purify sesamin from sesame meal. Moreover, HPLC is also an ideal method for analyzing the purity of sesamin.

Dissolution kinetics and mechanism of gibbsitic bauxite and pure gibbsite in sodium hydroxide solution under atmospheric pressure

The crystal structure, morphology, dissolution kinetics and mechanism of gibbsitic bauxite and pure gibbsite in Na OH solution under atmospheric pressure were systematically investigated by XRD and SEM. The results show that the size of single crystal of gibbsite in gibbsitic bauxite is smaller than that in pure gibbsite, but the interplanar distance is larger than that of pure gibbsite, which result in more defects in the crystal and less energy needed to dissolve in alkaline solution for the gibbsitic bauxite. The dissolution kinetic equations of gibbsitic bauxite and pure gibbsite were established, and the corresponding activation energies were calculated to be 99.144 and 115.149 k J/mol, respectively.

A Modified Phase-Field Model for Polymer Crystal Growth

The irrationality of existing phase field model is analyzed and a modified phase-field model is proposed for polymer crystal growth, in which the parameters are obtained from real materials and very simple to use, and most importantly, no paradoxical parameters appeared in the model. Moreover, it can simulate different microstructure patterns owing to the use of a new different free energy function for the simulation of morphologies of polymer. The new free energy function considers both the cases of T〈Tm and T≥Tm, which is more reasonable than that in published literatures that all ignored the T≥Tm case. In order to show the validity of the modified model, the finite difference method is used to solve the model and different crystallization morphologies during the solidification process of isotactic polystyrene are obtained under different conditions. Numerical results show that the growth rate of the initial secondary arms is obviously increased as the anisotropy strength increases. But the anisotropy strength seems to have no apparent effect on the global growth rate. The whole growth process of the dendrite depends mainly upon the latent heat and the latent heat has a direct effect on the tip radius and tip velocity of side branches.

Growth and crystallization behaviors of anodic oxide films on sputter-deposited titanium at very low potentials

Growth and crystallization of titanium anodized films were studied by performing the anodization of the sputter-deposited titanium samples under cyclic voltammetry （CV） mode at very low potentials. The surface features, crystalline behaviors and chemical compositions of the formed anodic oxide layers were detected by AFM, SE and XPS. It was found that the structure of the titanium anodized films is crystalline, even though the maximum oxidation potential （（Pmax） is very low （as low as 1000 mY）. Both enlarging the applied voltage and reducing the potential scanning rate are beneficial for the growth and crystallization of titanium oxide films. It was thought that the internal compressive stress, other than the local joule heating accepted for many researchers, is the main force of stimulating the crystallization of anodic titanium oxide films at very low potentials.

Advances in Supercritical Fluid Crystallization

The supercritical fluid crystallization technique is a novel technology for preparing ultrafine particles. This paper introduced the concept and features of the technique with an emphasis on three kinds of supercritical fluid crystallization techniques, i.e. rapid expansion of supercritical solutions, supercritical fluid anti-solvent and particles from gas saturated solutions Some questions and the prospect of this technique were also discussed.

Transformation behavior of ferrous sulfate during hematite precipitation for iron removal

The transformation behavior of ferrous sulfate was examined during hematite precipitation for iron removal in hydrometallurgical zinc.Specifically,the effects of the method used for oxygen supply(pre-crystallization or pre-oxidation of ferrous sulfate)and temperature(170–190℃)on the redissolution and oxidation–hydrolysis of ferrous sulfate were studied.The precipitation characteristics and phase characterization of the hematite product were investigated.The results showed that the solubility of ferrous sulfate was considerably lower at elevated temperatures.The dissolution behavior of ferrous sulfate crystals was influenced by both the concentrations of free acid and zinc sulfate and the oxydrolysis of ferrous ions.Rapid oxydrolysis of ferrous ions may serve as the dissolution driving force.Hematite precipitation proceeded via the following sequential steps:crystallization,redissolution,oxidation,and precipitation of ferrous sulfate.The dissolution of ferrous sulfate was slow,which helped to maintain a low supersaturation environment,thereby affording the production of high-grade hematite.

Purification and separation of durene by static melt crystallization

The purification and separation of durene from the mixture containing durene isomers were studied.Since the boiling points of tetramethyl benzene isomers are very close but their melting points are of great differences,static melt crystallization was applied to separate and purify durene from its isomers.Crystallization experiments were carried out under various operating conditions.The effects of cooling rate,crystallization temperature,sweating temperature and sweating time on the yield and purity of crystal were investigated.Orthogonal experimental design method was adopted to analyze the factors that may affect the yield of durene.Under the optimal crystallization conditions,the purity of durene could reach as high as 99.06%with the yield of 75.3%through one crystallization process.By fitting purification data based on sweating time in isothermal operations,the purification rate coefficient was obtained.

Preparation of spherical cobalt carbonate powder with high tap density

Spherical cobalt carbonate with high tap density, good crystallization and uniform particle size was prepared by controlled chemical crystal method using cobalt chloride and ammonium bicarbonate as cobalt source and precipitator. The effects of pH value and reaction time on crystallization and physical properties of cobalt carbonate were studied. The results show that the key factors influencing the preparation process of spherical cobalt carbonate with high tap density and good crystallization are how to control pH value (7.25±0.05) and keep some reaction time (about 10 h). Co4O3 was prepared by sintering spherical morphology CoCO3 samples at varied temperatures. The results show that as the decomposition temperature increases, the as-obtained Co4O3 products with porous structure transform into polyhedral structure with glazed surface, and simultaneously the cobalt content and tap density increase. However, the specific surface area shows a trend of decrease.

Hydrothermal Synthesis and Structure of a New Molybdenum Phosphate: (NH_3CH_2CH_2NH_3)_(2.5)[Mo_5O_(15)(PO_4) (HPO_4)]·7.5H_2O

The title compound (C5N5H41P2Mo5O30.5) was synthesized under hydrothermal condition and its crystal structure was determined by X-ray diffraction. It belongs to triclinic system, space group P , with a=9.9645(6), b=10.8666(7), c=15.814(1)? α=71.482(3), β=88.528(2), γ=78.448(2)°, V=1589.4(2)3, Dc=2.510g/cm3, Z=2,μ=2.138mm-1,λ(MoKα) = 0.71073 ? F(000)=1180. The final R and wR were 0.0396 and 0.1052 for 6626 observed reflections with I ≥2σ(I), respectively. The result of the structure analysis indicates that the [Mo5O15(PO4) (HPO4)]5- anion in the title compound consists of five edge-sharing or corner-sharing MoO6 octahedra and two corner-sharing PO4 tetrahedra. Each MoO6 octahedron adopts distorted octahedral geometry.

First-principles calculations of structural, electronic, elastic and thermal properties of phase M_2SiC(M=Ti,V,Cr,Zr,Nb,Mo,Hf,Ta and W)

The structural,electronic and elastic properties of the M_2SiC phases were studied,where M are 3d,4d,and 5d early transition metals.The valence electron concentration(VEC) effect of Ti,V,Cr,Zr,Nb,Mo,Hf,Ta and W on these properties was examined.The C_(44) saturates for a VEC value in surrounding of 8.5 for each serie.Hf-s,Ta-s and W-s electrons mainly contribute to the density of states at the Fermi level,and should be involved in the conduction properties.The distortion increases with increasing VEC and decreasing k_c/k_a factor except for the series M=Ti,V and Cr,where it is lower at the VEC value of 8.5(it follows a parabolic variation).The M_2SiC was characterized by a profound anisotropy for the shear planes(1010) and compressibility in the direction is higher than that along the cone except for W_2SiC,where it is lower.

Synthesis of lithium difluoro(oxalate)borate(LiODFB), phase diagram and ions coordination of LiODFB in dimethyl carbonate

A new two-step synthetic method was successfully developed to simplify the recrystallization process of lithium difluoro(oxalate)borate(LiODFB).Meanwhile,the purity of LiODFB as-prepared was determined by NMR,ICP-AES and Karl Fisher measurements,respectively.The as-prepared LiODFB presents a high purity up to 99.95%.Its metal ions and water contents are under good control as well.Besides,its structure information and thermal properties were confirmed by FTIR,Raman and DSC-TGA analyses,respectively.LiODFB exerts fine thermostability and hypo-water-sensitivity and its structure information agrees well with previous literature.Furthermore,a combination of phase diagram and Raman spectroscopy were utilized to study the thermal phase behavior and ions coordination of LiODFB-DMC binary system to optimize the synthesis and recrystallization process.Although there are three types of molecular interaction forms(CIPs,AGG-IIa,AGG-IIIb)in LiODFB-DMC binary system,LiODFB can only be isolated as large single crystal solvate as LiODFB·(DMC)3/2 by slowly cooling subjected to the nucleation kinetics.Therefore,the fundamental information of our work is helpful in accelerating the application of LiODFB in Li-ion secondary batteries.

Synthesis of γ-Al_2O_3 nanoparticles by chemical precipitation method

Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI（OH）3 sols are produced by using 0.1 mol/L Al（NO3）3·9H2O and 0.16 mol/L （NH4）2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%（volume fraction） surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.

Effect of the Alumosilicate Gels pH on Zeolite Phase Composition for the Co-crystallization of BEA/MOR Zeolites in Na2O-TEABr-Al2O3-SiO2-H2O System

This paper deals with the method of zeolites BEA （beta） and MOR （mordenite） synthesis and the co-crystallization method of zeolites BEA/MOR. Synthesized zeolites were studied based on the SEM （scanning electron microscopy）, XRD （x-ray diffraction） and chemical analysis. The porous structure of these zeolites was investigated by nitrogen low-temperature adsorption. It has been illustrated that regulation of the BEA/MOR co-crystalline zeolites phase composition is possible due to variations of the initial alumosilicate gels composition and hydrogen ions concentration. Zeolites containing the co-crystalline phases of BEA/MOR could to be attractive in the processes using the catalysts, which based on the pure phases BEA or MOR zeolites.

Preparation and structure characteristics of nano-Bi_2O_3 powders with mixed crystal structure

The nano-Bi2O3 powders were prepared by a chemical precipitation method with Bi（NO3）3, HNO3 and NaOH as reactants. The structural characteristics and morphology of nano-Bi2O3 powders were investigated by X-ray diffraction and transmission electron microscopy, respectively. The results show that under the optimum condition that 300g/L Bi（NO3）3 reacts at 90℃ for 2h, the Bi2O3 powders with 60nm on the average and 99.5% in purity are obtained. The prepared nano-Bi2O3 powders contain a mixed crystal structure of monoclinic and triclinic instead of traditional structure of monoclinic α-Bi2O3. And the mixed crystal structure is stable in air. The reason for the appearance of the mixed crystal structure may be that the ionic radius ratio of Bi 3+ to O 2- changes easily during the formation of nano-Bi2O3 particles by a chemical precipitation method.

Influence of ZrO_2 on sintering and crystallization of CaO-Al_2O_3-SiO_2 glass-ceramics

ZrO2 was added into CaO-Al2O3-SiO2 glass-ceramics and the effect of ZrO2 on sintering and crystallization of CaO-Al2O3-SiO2 glass ceramics was investigated. The results show that the sintering shrinkage ratio of glass particles decreases with the increase of the content of ZrO2. ZrO2 has an unfavourable effect on sintering shrinkage ratio of glass particles. The sintering shrinkage ratio of glass particles increases with the increase of sintering temperature. The increase of sintering temperature favors the decrease of the liquid phase viscosity of glass particles. ZrO2 has little effect on crystallization of main crystalline phase （β-wollastonite）. However, it promotes the crystallization at relatively low temperature.

Effect of rolling temperature on microstructure and texture of twin roll cast ZK60 magnesium alloy

Twin roll cast ZK60 alloy strip/sheet with final thickness of 0.5 mm was prepared, and effect of rolling temperature on microstructure and texture development was investigated using OM and XRD technique, microstructure and texture were measured on specimens subjected to rolling experiment at different rolling temperature, and macrotexture was also evaluated by X-ray diffraction method. In addition, the （1010）and （0002） pole figures were measured, and the tensile test was performed to reveal the influence of rolling temperature on mechanical properties. The results show that the microstrucmre of ZK60 alloy sheet consisted of fibrous structure with elongated grains, and shear bands along the rolling direction after warm rolling. Dynamic recrystallization could be found during the warm rolling process at rolling temperature 350℃ and above. And many fine recrystallized grain could be observed in the shear bands area. It is a little difficult to see the recrystallized grain in the sheet warm rolled at 300℃ because of higher density of shear bands. The warm rolled ZK60 alloy sheet exhibited strong （0002） pole texture, the intensity of （0002） pole figure decreases with the increasing of rolling temperature and the basal pole tilted slightly to the transverse direction after warm rolling.

Characterization of calcium deposition induced by Synechocystis sp. PCC6803 in BG11 culture medium

Calcium carbonate （CaCO3） crystals in their preferred orientation were obtained in BG11 culture media inoculated with Synechocystis sp. PCC6803 （inoculated BG11）. In this study, the features of calcium carbonate deposition were investigated. Inoculated BGll in different calcium ion concentrations was used for the experimental group, while the BGll culture medium was used for the control group. The surface morphologies of the calcium carbonate deposits in the experimental and control groups were determined by scanning and transmission electron microscopy. The deposits were analyzed by electronic probe micro-analysis, Fourier transform infrared spectrum, X-ray diffraction, thermal gravimetric analysis and differential scanning calorimetry. The results show that the surfaces of the crystals in the experimental group were hexahedral in a scaly pattern. The particle sizes were micrometer-sized and larger than those in the control group. The deposits of the control group contained calcium （Ca）, carbon （C）, oxygen （O）, phosphorus （P）, iron （Fe）, copper （Cu）, zinc （Zn）, and other elements. The deposits in the experimental group contained Ca, C, and O only. The deposits of both groups contained calcite. The thermal decomposition temperature of the deposits in the control group was lower than those in the experimental group. It showed that the CaCO3 deposits of the experimental group had higher thermal stability than those of the control group. This may be due to the secondary metabolites produced by the algae cells, which affect the carbonate crystal structure and result in a close-packed structure. The algae cells that remained after thermal weight loss were heavier in higher calcium concentrations in BGll culture media. There may be more calcium- containing crystals inside and outside of these cells. These results shall be beneficial for understanding the formation mechanism of carbonate minerals.

Effect of P addition on mineral transition of CaO-Al_2O_3-SiO_2 system during high-temperature sintering

The mineral transition, microstructure and self-pulverization as well as the Al2O3 leaching performance of calcium aluminate clinkers with different P additions in CaO-Al2O3-SiO2 system during high-temperature sintering were systematically studied by XRF, XRD, SEM-EDS and DSC-TG technologies. The clinkers sintered at 1350 °C mainly contain 12CaO·7Al2O3, CaO·Al2O3,β-2CaO·SiO2 and γ-2CaO·SiO2. The content of β-2CaO·SiO2 increases while the content of γ-2CaO·SiO2 decreases as the P addition increases. The self-pulverization property of clinkers deteriorates with increasing P addition. P distributes evenly in the clinkers, and inhibits the transformation of β-2CaO·SiO2 to γ-2CaO·SiO2. The cell volumes of 12CaO·7Al2O3 and CaO·Al2O3 decrease and increase respectively as the P addition increases, and P decreases their formation temperatures. The Al2O3 leaching rate of calcium aluminate clinkers decreases obviously with increasing P addition, which decreases form 95.01% to 83.84% as the P addition increases from 0 to 0.85%.

Synthesis and Crystal Structure of N-cyclopropyl-9 -(3,4-dicholophenyl)-1,2,3,4,5,6,7,8,9,10-decahydroacridine -1,8-dione under Microwave Irradiation

The N-cyclopropyl-9-（3,4-dicholophenyl）- 1,2,3,4,5,6,7,8,9,10-decahydroacri- dine-1,8-dione was synthesized by the reaction of 1,3-cyclohexanedione, N-cyclopropylamine and 3,4-dicholoaldehyde in water and glycol under microwave irradiation. Its crystal structure was determined by single-crystal X-ray diffraction analysis. It possesses P212121 space group, with a = 9.9103（5）, b = 13.3597（8）, c = 14.5633（8）A, V= 1928.16（18）A3 ,Mr = 402.30, Z = 4, Dc= 1.386 g/cm^3, 2 = 0.7107A,μ（MoKα）=0.354mm^-1 and F （000） = 840. The structure was refined to R = 0.0280 and wR = 0.0757. In the structure, the pyridine ring adopts a boat conformation.