取向等规聚丙烯退火过程中的再晶化

采用广角X射线衍射法研究取向等规聚丙烯材料在退火过程中结晶度和织构的变化规律,并用偏光显微镜观察材料中球晶的形貌变化。结果显示,在退火初期的10 min内,试样结晶度迅速增加,材料中的轧制织构组元含量有所增大,同时材料中球晶的形貌变得清晰可辨。通过对织构组元的定量分析发现,再晶化形成的新晶体拥有与残余晶体相同的晶体取向。退火过程中的再晶化是非晶部分沿残余晶体发生择优重排的过程,新晶体的大分子链方向与残余晶体的大分子链方向相同。

FER沸石再晶化制备介孔分子筛及其催化性能

在十六烷基三甲基溴化铵存在下,在浓NaOH溶液中降解并再晶化FER沸石,得到单一有序的介孔分子筛.通过X射线衍射(XRD),傅里叶变换红外光谱(FT-IR),热重(DTG),N2吸附,NH3程序升温脱附(NH3-TPD)及水热处理等手段对合成样品的结构性能进行了详细表征,并以混合C4烃催化裂解制低碳烯烃作为探针反应考察了合成样品的催化性能.结果表明,本方法合成的样品ReFM为孔壁含FER沸石次级结构单元的高度有序的介孔材料,其具有合适的孔道和适中的酸性,在625℃混合C4烃催化裂解反应中表现出52.29%的烯烃收率.

催化裂化平衡剂再利用研究进展

综述了目前国内外催化裂化(FCC)平衡剂再利用的研究进展情况,重点介绍了实现FCC平衡剂再利用的复活技术,包括重金属脱除复活技术和再晶化复活技术。通过对现有几种FCC平衡剂再利用技术进行比较,提出了今后该技术的研发方向。

级孔HZSM-5分子筛上超临界正十二烷催化裂解

以四丙基氢氧化铵(TPAOH)和四丁基氢氧化铵为碱源,在十六烷基三甲基溴化铵存在下,通过脱硅和再晶化合成了级孔HZSM-5分子筛。采用XRD、TEM、N2吸附-脱附、原位Py-IR和NH3-TPD等方法表征了分子筛的结构和酸性,在500℃、4 MPa下考察了级孔HZSM-5分子筛涂层上超临界正十二烷催化裂解的性能。实验结果表明,用TPAOH脱硅得到的级孔HZSM-5分子筛具有较大的外比表面积、微孔体积及酸量,其活性较未处理的HZSM-5原粉提高了76%,失活速率下降了61%。再晶化后,试样表面被MCM-41和HZSM-5碎片包裹,活性反而下降。表明TPAOH可缓和脱硅过程,保护分子筛的微孔结构;开放的介孔结构和中等的强酸量,有利于改善级孔HZSM-5分子筛的催化裂解性能。

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.

Production of Mg-Al-Zn magnesium alloy sheets with ultrafine-grain microstructure by accumulative roll-bonding

Accumulative roll-bonding （ARB） was applied to Mg-Al-Zn magnesium alloy sheets to prepare ultrafine-grain microstructure. Significant grain refinement is achieved after three cycles of ARB with average grain size of about 1.3 μm. The microstructure is characterized by nearly uniform ultrafine equiaxed microstructure without twins. The evolution of the misorientation distribution during ARB was measured by EBSD. Grain refinement can be contributed to the grain subdivision induced by severe accumulated strain, the accumulated strain enhanced concurrent dynamic recovery and recrystallization as well as the complicated distribution of interface and shear strain during ARB.

Effect of one-step and two-step homogenization treatments on distribution of Al_3Zr dispersoids in commercial AA7150 aluminium alloy

Semi-quantitative electron probe microanalysis （EPMA） mapping, scanning electron microscopy （SEM） and transmission electron microscopy （TEM） were employed to study the effect of one-step and two-step treatments on the Zr distribution and Al3Zr dispersoid characteristics in as-cast commercial AA7150 aluminum alloy. It is shown that the Zr concentration in the dendrite centre regions is higher than that near the dendrite edges in the as-cast condition, and that homogenization at 460 °C for 20 h is insufficient to remove these concentration gradients. After homogenizing at 460-480 °C, a high number density of larger dispersoids can be observed in dendrite centre regions but not near dendrite edges. Furthermore, the dispersoid size increases with increasing the temperature during both one-step and two-step homogenization treatments.

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.

Grain refinement of magnesium alloys processed by severe plastic deformation

Grain refinement of AZ31 Mg alloy during cyclic extrusion compression （CEC） at 225-400 ℃ was investigated quantitatively by electron backscattering diffraction （EBSD）. Results show that an ultrafine grained microstructure of AZ31 alloy is obtained only after 3 passes of CEC at 225 ℃. The mean misorientation and the fraction of high angle grain boundaries （HAGBs） increase gradually by lowering extrusion temperature. Only a small fraction of {101^-2} twinning is observed by EBSD in AZ31 Mg alloys after 3 passes of CEC. Schmid factors calculation shows that the most active slip system is pyramidal slip {101^-1}〈1120〉and basal slip {0001}〈1120〉 at 225-350 ℃ and 400 ℃, respectively. Direct evidences at subgrain boundaries support the occurrence of continuous dynamic recrystallization （CDRX） mechanism in grain refinement of AZ31 Mg alloy processed by CEC.

Effect of calcium addition on microstructure and texture modification of Mg rolled sheets

The mechanical properties and texture of AM60（Mg-6.0Al-0.3Mn,mass fraction %） and ZXM200（Mg-1.6Zn-0.5Ca-0.2Mn） Mg alloys subjected to multi-pass hot rolling were investigated.The finer recrystallized grains usually exhibit particular preferred orientations and then alter the total texture feature of rolled sheets.Ca solid solution into Mg matrix serves to the formation of texture component with c-axis rotated away from normal direction towards transverse direction and then weakens the overall texture intensity,resulting in a similar anisotropic characteristic to RE-containing Mg alloys.

Effect of nano TiN/Ti refiner on as-cast and hot-working microstructure of commercial purity aluminum

A novel type nano TiN/Ti composite grain refiner （TiN/Ti refiner） was prepared by high energy ball milling, and its effect on as-cast and hot-working microstructure of commercial purity aluminum （pure Al） was investigated. The results show that TiN/Ti refiner exhibits excellent grain refining performances on pure Al. With an addition of 0.2% TiN/Ti refiner, the average grain size of pure Al decreases to 82 μm, which is smaller than that of pure Ti and Al 5Ti 1B master alloy as refiners. The microstructure of weld joint of pure Al with 0.1% TiN/Ti refiner is fine equiaxed grains and the hardness of weld joint is higher than that of the base metal. For pure Al with 40% cold deformation and recrystallization at 250 °C for 1.0 h, the grains of the sample added 0.1% Ti powder have an obvious grain growth behavior. In contrast, oriented grains caused by deformation have been eliminated, and there is no obvious grain growth in pure Al refined with 0.1% TiN/Ti refiner, indicating that nano TiN in the refiner inhibits the growth of grain during recrystallization.

Simulated and experimental investigation on discontinuous dynamic recrystallization of a near-α TA15 titanium alloy during isothermal hot compression in βsingle-phase field

A cellular automaton（CA） modeling of discontinuous dynamic recrystallization（DDRX） of a near-α Ti-6Al-2Zr-1Mo-1V（TA15） isothermally compressed in the β single phase field was presented.In the CA model,nucleation of the β-DDRX and the growth of recrystallized grains（re-grains） were considered and visibly simulated by the CA model.The driving force of re-grain growth was provided by dislocation density accumulating around the grain boundaries.To verify the CA model,the predicted flow stress by the CA model was compared with the experimental data.The comparison showed that the average relative errors were10.2%,10.1%and 6%,respectively,at 1.0,0.1 and 0.01 s^-1 of 1020 ℃,and were 10.2%,11.35%and 7.5%,respectively,at 1.0,0.1and 0.01 s^-1 of 1050 ℃.The CA model was further applied to predicting the average growth rate,average re-grain size and recrystallization kinetics.The simulated results showed that the average growth rate increases with the increasing strain rate or temperature,while the re-grain size increases with the decreasing strain rate;the volume fraction of recrystallization decreases with the increasing strain rate or decreasing temperature.

Effect of homogenization treatment on microstructure and mechanical properties of DC cast 7X50 aluminum alloy

The evolution of the eutectic structures in the as-cast and homogenized 7X50 aluminum alloys was studied by scanning electron microscopy(SEM), transmission electron microscopy(TEM), energy dispersive spectrometer(EDS), differential scanning calorimetry(DSC), X-ray diffraction(XRD) and tensile test. The results show that the main phases are S(Al2CuMg), T(Al2Mg3Zn3) and Mg Zn2, with a small amount of Al7Cu2 Fe and Al3 Zr in the as-cast 7X50 alloy. The volume fraction of the dendritic-network structure and residual phase decreases gradually during the homogenization. After homogenization at 470 °C for 24 h and then 482 °C for 12 h, the T(Al2Mg3Zn3) phase disappears and minimal S(Al2CuMg) phase remains, while almost no change has happened for Al7Cu2 Fe. There is a strong endothermic peak at 477.8 °C in the DSC curve of as-cast alloy. A new endothermic peak appears at 487.5 °C for the sample homogenized at 470 °C for 1 h. However, this endothermic peak disappears after being homogenized at 482 °C for 24 h. The T(Al2Mg3Zn3) phase cannot be observed by XRD, which is consistent with that T phase is the associated one of S(Al2CuMg) phase and Mg Zn2 phase. The volume fraction of recrystallized grains is substantially less in the plate with pre-homogenization treatment. The strength and fracture toughness of the plate with pre-homogenization treatment are about 15 MPa and 3.3 MPa·m1/2 higher than those of the material with conventional homogenization treatment.

Microstructure and texture evolution in titanium subjected to friction roll surface processing and subsequent annealing

Commercial purity and high purity titanium sheets were initially strained by a new technique, named as friction roll surface processing （FRSP）. Severe strain was imposed into the surface layer and strain gradient was formed through the thickness of the sheet. The microstructure and texture in as-strained state were investigated by optical microscopy and X-ray diffraction technique On the surface of the sheets, ultra-fine grains were found to have a sharp texture with a preferred orientation strongly related to the FRSP direction. The evolution of microstructure and crystallographic texture of FRSPed samples during recrystallization were also studied by electron back-scattered diffraction （EBSD） technique after being annealed at selected temperatures and time. The results indicated that the preferred orientations resulting from FRSP and annealing in the surface layer were formed during rolling and its recrystallization textures were reduced by FRSP. In addition, the texture evolved stably without change in main components during the annealing.

Solidification process and microstructure evolution of bulk undercooled Co-Sn alloys

A series of Co-Sn alloys with Sn content ranging from 12% to 32%（mole fraction） were undercooled to different degrees below the equilibrium liquidus temperature and the solidification behaviors were investigated by monitoring the temperature recalescence and examing the solidification microstructures.A boundary clearly exists,which separates the coupled growth zone from the decoupled growth zone of eutectic phases for the alloys with Sn content ranging from 14% to 31%（mole fraction）.The other Co-Sn alloys out of this content range are hard to be undercooled into the coupled growth zone in the experiment.It is found that the so-called non-reciprocal nucleation phenomenon does not happen in the solidification of undercooled Co-Sn off-eutectic alloys.

Microstructure evolution and mechanical properties of ZK60 magnesium alloy produced by SSTT and RAP route in semi-solid state

The microstructure evolution and mechanical properties of a ZK60 magnesium alloy produced by the semi-solid thermal transformation （SSTT） route and the recrystallization and partial melting （RAP） route were studied, respectively. The microstructure evolution during partial remelting was studied at different temperatures for different time. The tensile mechanical properties of thixoformed components by the two routes at room temperature were examined. The results show that coalescence is dominant in the SSTT alloy and Ostwald ripening is dominant in the RAP alloy. Compared with the SSTT route, the RAP route can produce finer semi-solid microstructure under the similar isothermal holding condition. The microstructure of the RAP alloy is much more spheroidized compared with the SSTT alloy. Thixoforming for the ZK60 magnesium alloy produced by the SSTT and RAP route results in successful filling of the die, and the thixoforming process improves the mechanical properties of ZK60 magnesium alloy. The RAP alloy shows significantly advantageous mechanical properties over that of the SSTT alloy.

Hot deformation and processing map of GH3535 superalloy

The hot deformation behavior of GH3535 superalloy was investigated by hot compression tests in the temperature range of 1000-1200 °C and strain rate range of 0.01-50 s-1. The activation energy is about 356.3 k J/mol, and the flow curves and processing map were developed on the basis of experimental data. The processing map exhibits a stable domain which occurs in the strain rate range of 0.01-1 s-1 at all the temperatures and a instable domain which occurs in the strain rate range of 1-50 s-1. Microstructural observations reveal that the full dynamic recrystallization（DRX） occurs in the conditions of（1150 °C, 0.01 s-1）,（1200 °C, 0.01 s-1） and（1200 °C, 0.1 s-1） with different grain sizes and undissolved carbides. The flow localization and cracks occur in the regime of flow instability.

Static globularization and grain morphology evolution ofαandβphases during annealing of hot-rolled TC21 titanium alloy

A lamellar-structure TC21 titanium alloy was hot-rolled and subsequently annealed at 820,880 and 940℃ for 1 and 6 h,and the effects of annealing parameters on static globularization and morphology evolution of bothαandβphases were studied.The results show thatαglobularization process is sluggish due to the limited boundary splitting at 820℃.With increasing temperature to 880℃,the accelerated boundary splitting and termination migration promote theαglobularization.At 820 and 880℃,the static recovery(SRV)and recrystallization(SRX)induce the grain refinement of interlamellarβphase.However,the excessively high temperature of 940℃ results in the coarsening ofαgrains due to the assistance of Ostwald ripening,and produces coarseβgrains mainly due to the absence of SRX in interlamellarβphases.Conclusively,880℃ is an appropriate annealing temperature to produce a homogeneous microstructure in which globularizedαand refinedβgrains distribute homogeneously.

Effect of thermal-mechanical processing on microstructure and mechanical properties of duplex-phase Mg-8Li-3Al-0.4Y alloy

The effect of thermal-mechanical processing on the microstructure and mechanical properties of the duplex phase Mg-8Li-3Al-0.4Y alloy was investigated.The as-cast alloy was composed ofα-Mg,β-Li,AlLi,Al2Y and MgAlLi2phases.Annealing of the cold rolled alloy at350°C for60min was considered to be optimum.This caused full static recrystallization and spheroidization.A significantβ-Li loss occurred when the annealing time was increased to90min.The optimized annealing treatment produced the following values of the yield strength,ultimate strength and elongation:148MPa,184MPa and35%,respectively.The texture evolution of theα-phase and theβ-phase changed remarkably during thermal-mechanical processing.