Preparation and Characterization of High Purity Enriched 10B Boric Acid via Anti-Solvent Recrystallization

Self-made enriched IUB boric acid as raw material was purified by recrystallization. The effects of final crystallization temperature, crystallization time, stirring speed, crystallization frequency and other factors on the purity were investigated. The appropriate operating condition was that the final crystallization temperature and time were 5 ℃ and 10 h respectively under a low-speed stirring for crystallizing twice, which would make the purity and yield of boric acid reach 99.94% and 95.36%, respectively. Taking this as foundation, recrystallization process was optimized with acetone as anti-solvent, whose amount was the most important index. The boric acid solution was added into acetone and recrystallized under the same condition, and the purity and yield of boric acid would reach 99.98% and 99.61%, respectively. The product detected by XRD was confirmed as boric acid crystal. Main ion concentration in the product was detected by ICP, which basically met the national standard of high purity. Crystal morphology of boric acid was observed by SEM.

An in-situ study of static recrystallization in Mg using high temperature EBSD

It has been a common method to improve the mechanical properties of metals by manipulating their microstructures via static recrystallization,i.e.,through heat treatment.Therefore,the knowledge of recrystallization and grain growth is critical to the success of the technique.In the present work,by using in-situ high temperature EBSD,the mechanisms that control recrystallization and grain growth of an extruded pure Mg were studied.The experimental results revealed that the grains of priority for dynamic recrystallization exhibit fading competitiveness under static recrystallization.It is also found that grain boundary movement or grain growth is likely to show an inverse energy gradient effect,i.e.,low energy grains tend to swallow or grow into high energy grains,and grain boundaries of close to 30°exhibit superior growth advantage to others.Another finding is that{10-12}tensile twin boundaries are sites of hardly observed for recrystallization,and are finally swallowed by adjacent recrystallized grains.The above findings may give comprehensive insights of static recrystallization and grain growth of Mg,and may guide the design of advanced materials processing in microstructural engineering.

{1012}twin–twin intersection-induced lattice rotation and dynamic recrystallization in Mg–6Al–3Sn–2Zn alloy

This study investigated the formation mechanism of new grains due to twin–twin intersections in a coarse-grained Mg–6Al–3Sn–2Zn alloy during different strain rates of an isothermal compression.The results of electron backscattered diffraction investigations showed that the activated twins were primarily{1012}tension twins,and 60°<1010>boundaries formed due to twin–twin intersections under different strain rates.Isolated twin variants with 60°<1010>boundaries transformed into new grains through lattice rotations at a low strain rate(0.01 s^(−1)).At a high strain rate(10 s^(−1)),the regions surrounded by subgrain boundaries through high-density dislocation arrangement and the 60°<1010>boundaries transformed into new grains via dynamic recrystallization.

Simulation of Dynamic Recrystallization in 7075 Aluminum Alloy Using Cellular Automaton

The evolution of microstructure during hot deformation is key to achieving good mechanical properties in aluminum alloys.We have developed a cellular automaton(CA) based model to simulate the microstructural evolution in 7075 aluminum alloy during hot deformation.Isothermal compression tests were conducted to obtain material parameters for 7075 aluminum alloy,leading to the establishment of models for dislocation density,nucleation of recrystallized grains,and grain growth.Integrating these aspects with grain topological deformation,our CA model effectively predicts flow stress,dynamic recrystallization(DRX) volume fraction,and average grain size under diverse deformation conditions.A systematic comparison was made between electron back scattered diffraction(EBSD) maps and CA model simulated under different deformation temperatures(573 to 723 K),strain rates(0.001 to 1 s^(-1)),and strain amounts(30% to 70%).These analyses indicate that large strain,high temperature,and low strain rate facilitate dynamic recrystallization and grain refinement.The results from the CA model show good accuracy and predictive capability,with experimental error within 10%.

Beam oscillating parameters on pore inhibition,recrystallization and grain boundary characteristics of laser-arc hybrid welded AZ31 magnesium alloy

Oscillating laser-arc hybrid welding of AZ31B magnesium alloy was carried out,the effects of beam oscillation parameters on pore inhibition,microstructure,grain boundary characteristics and tensile properties were investigated.The results showed that the pore formation can be inhibited with oscillating frequency higher than 75 Hz and radius smaller than 0.5 mm.The columnar grains neighboring the fusion line can be broken by the beam oscillation behavior,while the grain growth was promoted with the increase of frequency or radius.It should be noted that the coincidence site lattice(CSL)boundaries were mainlyΣ13b andΣ29 boundaries,which were contributed by{10■2}tensile twins and{11■2}compression twins,respectively.The total fraction of CSL boundaries reached maximum at radius of 0.25 mm and frequency of 75 Hz,which was also confirmed as the optimized parameters.In this case,the elongation rate increased up to 13.2%,12.8%higher than that of the weld without beam oscillation.Finally,the pore formation and inhibition mechanisms were illustrated according to the state of melt flow and keyhole formation,the abnormal growth was discussed basing on secondary recrystallization,and the relationship among the pore formation,grain size,boundary characteristics and weld toughness were finally established.

High temperature deformation and recrystallization behavior of magnesium bicrystals with 90°<1010>and 90°<1120>tilt grain boundaries

The deformation mechanisms and dynamic recrystallization(DRX)behavior of specifically grown bicrystals with a symmetric 90°<1010>and 90°<1120>tilt grain boundary,respectively,were investigated under deformation in plane strain compression at 200℃and 400℃.The microstructures were analyzed by panoramic optical microscopy and large-area electron backscatter diffraction(EBSD)orientation mapping.The analysis employed a meticulous approach utilizing hundreds of individual,small EBSD maps with a small step size that were stitched together to provide comprehensive access to orientation and misorientation data on a macroscopic scale.Basal slip primarily governed the early stages of deformation at the two temperatures,and the resulting shear induced lattice rotation around the transverse direction(TD)of the sample.The existence of the grain boundary gave rise to dislocation pile-up in its vicinity,leading to much larger TD-lattice rotations within the boundary region compared to the bulk.With increasing temperature,the deformation was generally more uniform towards the bulk due to enhanced dislocation mobility and more uniform stress distribution.Dynamic recrystallization at 200℃was initiated in{1011}-compression twins at strains of 40%and higher.At 400℃,DRX consumed the entire grain boundary region and gradually replaced the deformed microstructure with progressing deformation.The recrystallized grains displayed characteristic orientations,such that their c-axes were perpendicular to the TD and additionally scattered between 0°and 60°from the loading axis.These recrystallized grains displayed mutual rotations of up to 30°around the c-axes of the initial grains,forming a discernible basal fiber texture component,prominently visible in the{1120}pole figure.It is noteworthy that the deformation and DRX behaviors of the two analyzed bicrystals exhibited marginal variations in response to strain and deformation temperature.

Effect of deformation parameters on the austenite dynamic recrystallization behavior of a eutectoid pearlite rail steel

Understandings of the effect of hot deformation parameters close to the practical production line on grain refinement are crucial for enhancing both the strength and toughness of future rail steels.In this work,the austenite dynamic recrystallization(DRX)behaviors of a eutectoid pearlite rail steel were studied using a thermo-mechanical simulator with hot deformation parameters frequently employed in rail production lines.The single-pass hot deformation results reveal that the prior austenite grain sizes(PAGSs)for samples with different deformation reductions decrease initially with an increase in deformation temperature.However,once the deformation temperature is beyond a certain threshold,the PAGSs start to increase.It can be attributed to the rise in DRX volume fraction and the increase of DRX grain with deformation temperature,respectively.Three-pass hot deformation results show that the accumulated strain generated in the first and second deformation passes can increase the extent of DRX.In the case of complete DRX,PAGS is predominantly determined by the deformation temperature of the final pass.It suggests a strategic approach during industrial production where part of the deformation reduction in low temperature range can be shifted to the medium temperature range to release rolling mill loads.

Influence of thermomechanical treatment on recrystallization and softening resistance of Cu-6.5Fe-0.3Mg alloy

The recrystallization and softening resistance of a Cu-6.5Fe-0.3Mg(mass fraction,%)alloy prepared by Process 1(cold rolling heat treatment)and Process 2(hot/cold rolling heat treatment)were studied using Vickers hardness tests,tensile tests,scanning electron microscopy and transmission electron microscopy.The softening temperature,hardness and tensile strength of the alloy prepared by Process 2 were 110°C,HV 15 and 114 MPa higher,respectively,than those of the alloy prepared by Process 1 after aging at 300°C.The recrystallization activation energy of the alloys prepared by Process 1 and Process 2 were 72.83 and 98.11 kJ/mol,respectively.The pinning effects of the precipitates of the two alloys on grain boundaries and dislocations were basically the same.The softening mechanism was mainly attributed to the loss of dislocation strengthening.The higher Fe fiber density inhibited the average free migration path of dislocations and grain boundary migration in the alloy,which was the main reason for higher softening temperature of the alloy prepared by Process 2.

Dissolution and reprecipitation of 14H-LPSO structure accompanied by dynamic recrystallization in hot-extruded Mg_(89)Y_(4)Zn_(2)Li_(5) alloy

We investigate the variation induced in long-period stacking ordered(LPSO)structures,dynamic recrystallization(DRX),and mechanical performance of hot-extruded Mg89Y4Zn2Li5 alloys fabricated at different extrusion speeds(Ve=0.4,0.8,1.0,1.2 mm/s)and die angles(α=30°,60°,90°)under 400℃,the dissolution and reprecipitation of 14H LPSO structure accompanied by DRX process are then clarified in detail.Upon all extrusion conditions,the block 18R LPSO structures elongate in the extrusion direction,while the lamellar 14H LPSO structures dissolve under the deformation strain.In addition,due to discontinuous and continuous DRX mechanisms,all hot-extruded alloys have a full DRX microstructure consisting of equiaxed recrystallized grains,but the DRX grain size reduces when both extrusion speed and die angle decrease.Note that,in the interior of DRX grains,thin LPSO lamellae mixing 14H,18R and 24R structures nucleate and dynamically precipitate due to the dissolution of the original lamellar 14H LPSO structures.Furthermore,the hot-extruded Mg_(89)Y_(4)Zn_(2)Li_(5)alloy becomes stronger as decreasing of the extrusion speed and die angle,whereas the ductility remains nearly constant.Finally,the hotextruded Mg_(89)Y_(4)Zn_(2)Li_(5)alloy achieves an excellent strength-ductility balance at a relatively low extrusion speed(0.4 mm/s)and small die angle(30°)mainly due to the elongated 18R LPSO structure,fine and full DRX microstructure,thin mixed LPSO precipitates in the DRX grains,twins and dislocations.

Towards tailoring basal texture of rolled Mg alloy sheet by recrystallization for high room-temperature formability: A review

Room-temperature(RT) formability is a key factor to broaden the applications of rolled Mg alloy sheets in the industry. However, rolled Mg alloy sheets generally form strong basal texture, where the(0001) poles align parallel to the normal direction(ND). This hinders the activation of(0001) [1120] basal slip, limiting the RT formability. Therefore, texture weakening, i.e., the inclination of the(0001) poles from the ND, plays an important role to improve the RT formability. Recrystallization is crucial to control the textural development in Mg,and currently, the texture weakening is commonly achieved using static recrystallization(SRX). However, the type of slipping and twinning,which are activated during rolling, affect the textural features after SRX. It is also demonstrated that shear bands and preferential grain growth are important factors to tailor the texture during SRX. Indeed, dynamic recrystallization(DRX) easily occurs during rolling in Mg, which also affects the final rolling texture, while the effect of DRX on the textural formation is not extensively studied for the development of RT-formable Mg alloy sheets. Therefore, the effect of these factors on the textural development in rolled Mg is reviewed in this manuscript.Additionally, the ideal microstructure and texture for RT-formable Mg alloy sheets are still controversial. The RT-formability includes stretch forming(biaxial tension), bending(plane strain tension), and deep-drawing. In particular, the stretch forming is commonly used to evaluate the RT-formability of rolled Mg. Although the stretch formability has been improved by recent studies, the further improvement is necessary owing to the relatively low formability of rolled Mg compared with that of rolled Fe and Al. Based on the relationship between the microstructure/texture and stretch formability provided in the literature, the design guidance for high stretch formability is proposed in this review.

Processing map and dynamic recrystallization behaviours of 316LN-Mn austenitic stainless steel

The hot deformation behaviours of 316LN-Mn austenitic stainless steel were investigated by uniaxial isothermal compression tests at different temperatures and strain rates.The microstructural evolutions were also studied using electron backscatter diffraction.The flow stress decreases with the increasing temperature and decreasing strain rate.A constitutive equation was established to characterize the relationship among the deformation parameters,and the deformation activation energy was calculated to be 497.92 k J/mol.Processing maps were constructed to describe the appropriate processing window,and the optimum processing parameters were determined at a temperature of 1107-1160℃ and a strain rate of 0.005-0.026 s^(-1).Experimental results showed that the main nucleation mechanism is discontinuous dynamic recrystallization(DDRX),followed by continuous dynamic recrystallization(CDRX).In addition,the formation of twin boundaries facilitated the nucleation of dynamic recrystallization.

Origin of extension twinning-mediated static recrystallization and unique parallel alignment of(0001) poles to transverse direction in Mg-3Al-0.4Mn(mass%) alloy sheet

The origin of unique parallel alignment of(0001) poles to transverse direction(TD) was investigated using Mg-3Al-0.4Mn(mass%)alloy sheets rolled with different process conditions. When rolling was performed with intermediate reheating, the alloy showed a sluggish static recrystallization(SRX) behavior during post-annealing, facilitating the nucleation and growth of statically recrystallized grains from extension twins. This resulted in the apparent texture component with the parallel alignment of the(0001) poles to the TD, and the sheet exhibited good ductility for both the rolling direction(RD) and TD. In contrast, continuous rolling without intermediate reheating led to the formation of severely deformed regions near double twins. SRX was promoted at such regions, forming a typical basal textural feature with weak RD-split of the(0001) poles. Although extension twins were formed after the continuous rolling, SRX was facilitated at the severely deformed regions with double twins, and the formation of the unique alignment of the(0001) poles to the TD was suppressed. The RD-split texture led to the large elongation to failure along the RD, while it along the TD decreased owing to the narrow distribution of the(0001)poles toward the TD, resulting in the in-plane anisotropy in ductility.

Variations in dynamic recrystallization behavior and mechanical properties of AZ31 alloy with extrusion temperature

This study investigates the effects of extrusion temperature on the dynamic recrystallization(DRX)behavior of a Mg-3Al-1Zn-0.3Mn(AZ31,wt%)alloy during hot extrusion and on the microstructural characteristics and mechanical properties of materials extruded at 350 and 450℃.An increase in the extrusion temperature causes a decrease in the amount of strain energy accumulated in the material during extrusion,because of promoted activation of pyramidal<c+a>slip and dynamic recovery.This reduced strain energy weakens the DRX behavior during extrusion,which eventually results in a decrease in the area fraction of recrystallized grains of the extruded material.The material extruded at 450℃has coarser grains and a stronger basal fiber texture than that extruded at 350℃.As the extrusion temperature increases from 350 to 450℃,the tensile yield strength(TYS)of the extruded material increases from 191.8 to 201.5 MPa,whereas its compressive yield strength(CYS)decreases from 122.5 to 111.0 MPa;consequently,its tension-compression yield stress ratio(CYS/TYS)decreases from 0.64 to 0.55.The increase in the TYS is attributed mainly to the stronger texture hardening and strain hardening effects of the extruded material,and the decrease in the CYS is attributed to the reduced twinning stress resulting from grain coarsening and texture intensification.The microstructural and textural evolutions of the materials during extrusion and the deformation and hardening mechanisms of the extruded materials are discussed in detail.

Controlling dynamic recrystallization via modified LPSO phase morphology and distribution in Mg-Gd-Y-Zn-Zr alloy

Featured initial microstructures of Mg-11Gd-4Y-2Zn-0.5Zr alloy(wt%) were obtained by adjusting temperatures of solid solution and cooling methods, including island intergranular 18R and 14H LPSO phases with low-density stacking faults, differentially spaced lamellar intragranular 14H-LPSO phases, and network intergranular 18R-LPSO phases with high-density intragranular stacking faults. Effects of these featured LPSO phases and stacking faults on dynamic recrystallization(DRX) behavior were investigated via hot compression. Promoted DRX behavior via particle stimulated nucleation(PSN) is introduced by coexisting intergranular island 18R and 14H LPSO phases and intragranular wide spacing lamellar 14H-LPSO phases, contributing the highest DRX fraction of 42.6%. Conversely, it is found that DRX behavior with network intergranular 18R-LPSO phases and dense intragranular stacking fault is considerably inhibited with the lowest fraction of 22.8%. That is, the restricted DRX due to dislocations pinning by stacking faults overwhelms the enhanced DRX behavior via PSN of island intergranular 18R and 14H LPSO phases. Specially, compared with dense intragranular lamellar 14H-LPSO phases, high-density stacking faults exert a larger inhibition effect on DRX behavior.

Characterization of recrystallized itraconazole prepared by cooling and anti-solvent crystallization

The objective of the present study was to alter the crystal habit of itraconazole(ITZ)by cooling and anti-solvent crystallization and characterize its properties.ITZ was recrystallized in different solvents and the effects of each solvent on morphology of crystals,dissolution behavior and solid state of recrystallized drug particles were investigated.The results revealed that ITZ crystals recrystallized by cooling and anti-solvent crystallization showed the different crystal habits from the untreated ITZ.Using cooling crystallization tended to provide needle-shaped crystals while the crystals obtained from anti-solvent crystallization showed more flaky,plate shape.This indicated the importance of preparation method on nucleation and crystal growth.No change in drug polymorphism was observed,according to determination of thermal property and crystalline state by differential scanning calorimetry and powder X-ray diffractometry,respectively.The recrystallized ITZ showed higher drug dissolution than untreated ITZ and the highest drug dissolution was observed from the samples recrystallized in the presence of PEG 200,which provided the small plate-shaped crystals with tremendously increased in surface area.However,the increasing of drug dissolution is relatively small,therefore,further development may be required.

Influence of Ca addition on the dynamic and static recrystallization behavior of direct extruded flat profiles of Mg-Y-Zn alloy

This paper investigates the influence of addition of Ca in a Y-Zn-containing magnesium alloy on the dynamic and static recrystallization behaviors and reveals the formation mechanism of the quadrupole texture during thermomechanical processing. Direct extrusion of flat bands has been conducted at various process conditions to study the difference between the two alloys WZ10 and WZX100 in terms of microstructure and texture development. It can be shown that, Ca addition promotes the DRX of WZ10 alloy. During additional heat treatment,the absence of Y segregation at the grain boundaries and the associated lack of solute drag to the boundary mobility leads to a pronounced grain growth during SRX in WZX100 alloy. Furthermore, it is shown that the addition of Ca to Y-Zn is not beneficial in terms of formability.It is demonstrated that alloying elements can have different effects depending on the recrystallization mechanisms. Partially recrystallized microstructure is a prerequisite at the as-extruded status to form the quadrupole texture and during subsequent annealing, which stands for high formability.

Dynamic Recrystallization Behavior of Q370qE Bridge Steel

Bridge steel has been widely used in recent years for its excellent performance. Understanding the high-temperature Dynamic Recrystallization (DRX) behavior of high-performance bridge steel plays an important role in guiding the thermomechanical processing process. In the present study, the hot deformation behavior of Q370qE bridge steel was investigated by hot compression tests conducted on a Gleeble 3800-GTC thermal-mechanical physical simulation system at temperatures ranging from 900 ℃ to 1100 ℃ and strain rates ranging from 0.01 s^(−1) to 10 s^(−1). The obtained results were used to plot the true stress-strain and work-hardening rate curves of the experimental steel, with the latter curves used to determine the critical strains for the initiation of DRX. The Zener-Hollomon equation was subsequently applied to establish the correspondence between temperature and strain rate during the high-temperature plastic deformation of bridge steel. In terms of the DRX volume fraction solution, a new method for establishing DRX volume fraction was proposed based on two theoretical models. The good weathering and corrosion resistance of bridge steel lead to difculties in microstructure etching. To solve this, the MTEX technology was used to further develop EBSD data to characterize the original microstructure of Q370qE bridge steel. This paper lays the theoretical foundation for studying the DRX behavior of Q370qE bridge steel.

Flow softening and dynamic recrystallization behavior of a Mg-Gd-Y-Nd-Zr alloy under elevated temperature compressions

Flow softening behavior of a homogenized Mg-7Gd-4Y-1Nd-0.5Zr alloy under compression to a final strain of∼1.8 at elevated temperatures of 450∼550℃ and a constant strain rate of 2s^(−1) has been investigated by optical microscopy,scanning electron microscopy,electron back-scattered diffraction and transmission electron microscopy.The results show that true stress first rises to the peak point and then drops to the bottom value and increases again with further increasing strain at each temperature.Twinning dynamic recrystallization(DRX)and continuous DRX contribute to the formation of new fine grains at temperatures 450∼475℃ when the restoration is caused by both DRX and texture change due to extension twinning,resulting in the larger softening degrees compared with the softening effects owing to continuous DRX and discontinuous DRX at 500∼550℃ when twinning activation is suppressed.500℃ is the transition temperature denoting a significant decline in the contribution of twinning and TDRX to the strain with increasing temperature.The cuboid-shape phase exists in both homogenized and compressed samples,while the compositions are varied.

Simulation on dynamic recrystallization behavior of AZ31 magnesium alloy using cellular automaton method coupling Laasraoui Jonas model

The dynamic recrystallization （DRX） process of AZ31 magnesium alloy including microstructure and dislocation density evolution during hot compression was simulated by adopting the cellular automaton （CA） method coupling the Laasraoui-Jonas model （LJ model）. The reliability of simulation depended on the accuracy of the hardening parameter, the recovery parameter and the strain rate sensitivity in the LJ model. The hardening parameter was calculated in terms of the LJ model and the Kocks-Mecking model （KM model）, and then the recovery parameter and the strain rate sensitivity were obtained by using the equation of steady state flow stress for DRX. Good agreements between the simulations and the experimental observations were achieved.

Modeling of strain hardening and dynamic recrystallization of ZK60 magnesium alloy during hot deformation

The flow stress behavior of ZK60 alloy at elevated temperature was investigated. The strain hardening and dynamic recrystallization of the alloy were modeled by Kocks-Meching model and Avrami equation, respectively. A new constitutive equation during hot deformation was constructed to predict the flow stress considering the dynamic recrystallization. The results show that the flow stress curves predicted by the proposed equation have high correlation coefficients with the experimental data, which confirms that the developed model is accurate and effective to establish the flow stress equation of ZK60 magnesium alloy during hot deformation. Microstructure observation shows that dynamic recovery occurs in the initial stage of hot deformation. However, the microstructure turns to recrvstallization structure as the strain increases.