4∶30系列取代型钨磷杂多酸盐的合成相转移及晶态学研究

合成了未见文献报道的４：３０系列钨磷杂多酸盐Ｎａ１６Ｐ４Ｗ３０Ｍ４（Ｈ２Ｏ）２Ｏ１１２·ｘＨ２Ｏ（Ｍ＝Ｓｎ２＋，Ｃｄ２＋），并通过元素分析、红外光谱、紫外－可见光谱及１８３ＷＮＭＲ进行了表征．以四庚基溴化铵为相转移试剂将该系列杂多化合物转移至有机溶剂苯中，通过变温广角Ｘ－ｒａｙ衍射及偏光显微镜研究了其在苯溶液中的结晶形态．

Mineralogy and crystal chemistry of a low grade nickel laterite ore

To acquire understanding of Ni enrichment from laterite ore,the mineralogy and crystal chemistry of a low grade limonite type nickel laterite ore sample assaying 0.97% Ni from Indonesia were studied using optical microscopy,X-ray diffraction（XRD）,scanning electron microscopy（SEM） and electron probe microanalysis（EPMA）.According to EPMA results,the mineral includes 80% goethite（（Fe,Ni,Al）O（OH）） with 0.87% Ni,15% silicate minerals with lizardite（（Mg,Fe,Ni）3Si2O5（OH）） and olivine（（Mg,Fe,Ni）2SiO4）,and 1.19% Ni,and other minor phases,such as hematite,maghemite,chromite and quartz,and no Ni was detected.The mineralogy of the laterite ore indicates that due to the complicated association of the various phases and the variable distribution of Ni,this refractory laterite ore can not be upgraded by traditional physical beneficiation processes.

Dynamic recrystallization kinetics of as-cast AZ91D alloy

The flow behavior and dynamic recrystallization（DRX） behavior of an as-cast AZ91 D alloy were investigated systematically by applying the isothermal compression tests in temperature range of 220-380 ℃ and strain rate range of 0.001-1 s^-1.The effect of temperature and strain rate on the DRX behavior was discussed.The results indicate that the nucleation and growth of dynamic recrystallized grains easily occur at higher temperatures and lower strain rates.To evaluate the evolution of dynamic recrystallization,the DRX kinetics model was proposed based on the experimental data of true stress-true strain curves.It was revealed that the volume fraction of dynamic recrystallized grains increased with increasing strain in terms of S-curves.A good agreement between the proposed DRX kinetics model and microstructure observation results validates the accuracy of DRX kinetics model for AZ91 D alloy.

Rate controlling mechanisms in hot deformation of 7A55 aluminum alloy

The hot deformation behavior of 7A55 aluminum alloy was investigated at the temperature ranging from 300 ℃ to 450 ℃ and strain rate ranging from 0.01 s-1 to 1 s-1 on a Gleeble-3500 simulator. Processing maps were established in order to apprehend the kinetics of hot deformation and the rate controlling mechanism was interpreted by the kinetic rate analysis obeying power-law relation. The results indicated that one significant domain representing dynamic recrystallization （DRX） existed on the processing maps and lying in 410-450 ＆#176;C and 0.05-1 s-1. The conclusions of kinetic analysis correlated well with those obtained from processing maps. The apparent activation energy values calculated in the dynamic recrystallization （DRX） domain and the stability regions except dynamic recrystallization （DRX） domain were 91.2 kJ/mol and 128.8 kJ/mol, respectively, which suggested that grain boundary self-diffusion and cross-slip were the rate controlling mechanisms.

Evolution of twins and texture and its effects on mechanical properties of AZ31 magnesium alloy sheets under different rolling process parameters

In order to investigate the dependence of microstructure and mechanical properties on the rolling process parameters, AZ31 magnesium alloy sheets with different grain sizes, basal texture intensities and twinning types were obtained using hot rolling at various temperatures and reductions. The volume fractions of the extension, contraction and secondary twins in the as-rolled sheets depend on the grain size. The highest volume fractions of three types of twins are obtained at 523 K under the reduction of 10% when the average grain size value is the maximum. The critical reductions for complete dynamic recrystallization are 30% at 523 K and 40% at 473 K. The increase of yield strength is ascribed to both grain-refinement strengthening and basal texture strengthening at the first stage. When the grain size does not decrease with increasing the reduction, the yield strength is mainly influenced by the texture weakening.

Microstructure and mechanical properties of as-cast and extruded biomedical Mg-Zn-Y-Zr-Ca alloy at different temperatures

A type of biomedical magnesium alloy Mg-3Zn-1Y-0.6Zr-0.5Ca was cast and extruded at three extrusion temperatures of 270, 300 and 330 °C. The microstructure and mechanical properties of the cast and extruded alloys, tailored at different extrusion parameters, were investigated using tensile tests, optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, X-ray diffractometry, transmission electron microscopy and electron backscattered diffraction. Optimum comprehensive mechanical properties are achieved in the alloy extruded at 270 °C, the ultimate tensile strength and the elongation reach 315 MPa and 26%, respectively, which is deemed to be associated with the grain refinement, weak basal texture and second phases strengthening. After hot extrusion, extensive dynamic recrystallization is found in the Mg-3Zn-1Y-0.6Zr-0.5Ca alloy. Continuous Mg3YZn6 phase bands are gradually broken into discontinuous chain-like or dot-like structures, and the grains distribute more uniformly. The as-extruded Mg-3Zn-1Y-0.6Zr-0.5Ca alloy exhibits a weak texture with (0001) basal planes parallel to the extrusion direction.

Microstructure and mechanical properties of Al-6Zn-2.5Mg-1.8Cu alloy prepared by squeeze casting and solid hot extrusion

Al-6Zn-2.5Mg-1.8Cu alloy ingots were prepared by squeeze casting under different specific pressures,and the fresh ingot with best mechanical properties was solid hot extruded.With the increase of the specific pressure from 0 to 250 MPa,the dendrites became round and small.Because the applied pressure increased the solid solubility of alloying elements,the number of MgZn2 phases decreased.When the specific pressure increased from 250 MPa to 350 MPa,the grain size increased.After solid hot extrusion,the a（Al） grains were refined obviously and the MgZn2 phases were uniformly dispersed in the microstructure.After solid hot extrusion,the ultimate tensile strength was 605.67 MPa and the elongation was 8.1%,which were improved about 32.22%and15.71%,respectively,compared with those of the metal mold casting alloy.The fracture modes of the billet prepared by the metal mold casting and by squeeze casting were intergranular and quasi-cleavage fractures,respectively,whereas,that of the solid hot extrusion was mainly dimple fracture.The refined crystalline strengthening was the main reason to improve the strength and elongation of alloy.

Preparation of tetrapod-like ZnO whiskers from waste hot dipping zinc

Large and uniform tetrapod-like ZnO whiskers （T-ZnO） were prepared from waste hot dipping zinc by vapor oxidation and examined by means of X-ray diffraction and ICP-AES analysis and scanning electron microscope. The products are pure hexagonal wurtzite crystals with tetrapod shape and edge size of center body 56 μm and needle length of 100130 μm. The size and shape of ZnO particles are fully controlled by the growth conditions and T-ZnO can be obtained only at 8501 000 ℃ and total gas flow rate ranging from 40 to 250 L·h-1 in which the size of the T-ZnO particles varies slightly with temperature. The process of the formation of T-ZnO is that T-ZnO may nucleate at the initial stage with a complete tetrapod shape and develop to the large size, but not the process of （preferential） growth of octahedral nuclei and subsequent growth of the needles. The experiment presents a new method to prepare T-ZnO economically by using the waste hot dipping zinc.

Dynamic recrystallization and mechanical properties of high-strain-rate hot rolled Mg-5Zn alloys with addition of Ca and Sr

Effects of the sole and the combined addition of Ca and Sr on microstructure and mechanical properties of as-cast and as-rolled Mg-5 Zn alloys were carefully investigated by OM,SEM,hot-compression testing and tensile testing.Ca is more effective than Sr in the microstructural refinement of as-cast alloys.High-strain-rate rolling(HSRR)produces more deformed twins and thus provides more nucleation sites for dynamic recrystallization(DRX).The addition of Ca and Sr can promote dynamic precipitation during HSRR,the precipitation process would consume the storage energy and thus increases the critical strain value of DRX,resulting in the retarded DRX effect by the addition of Ca and/or Sr.The as-rolled Mg-5 Zn-0.4 Ca-0.2 Sr alloy exhibits a good combination of strength and ductility,with the ultimate tensile strength of 317 MPa,the yield strength of 235 MPa and the elongation to rupture of 24%.

Fabrication of fine-grained,high strength and toughness Mg alloy by extrusion−shearing process

A novel extrusion-shearing(ES) composite process was designed to fabricate fine-grained, high strength and tough magnesium alloy. The structural parameters of an ES die were optimized by conducting an orthogonal simulation experiment using finite element software Deform-3D, and Mg-3 Zn-0.6 Ca-0.6 Zr(ZXK310) alloy was processed using the ES die. The results show that the optimized structural parameters of ES die are extrusion angle(α) of 90°, extrusion section height(h) of 15 mm and inner fillet radius(r) of 10 mm. After ES at an extrusion temperature and a die temperature of 350 °C, ZXK310 alloy exhibited good ES forming ability, and obvious dynamic recrystallization occurred in the forming area. The grain size decreased from 1.42 μm of extrusion area to 0.85 μm of the forming area. Owing to the pinning of second phase and formation of ultrafine grains, the tensile strength, yield strength and elongation of alloy reached 362 MPa, 289 MPa and 21.7%, respectively.

A discontinuous dynamic recrystallization model incorporating characteristics of initial microstructure

In order to describe and predict the kinetic process of discontinuous dynamic recrystallization （DDRX） during hot workingfor metals with low to medium stacking fault energies quantitatively, a new physically-based model was proposed by considering thecharacteristics of grain size distribution, capillary effect of initial grain boundaries （GBs） and continuous consumption of GBs. UsingIncoloy 028 alloy as a model system, experiments aiming to provide kinetic data （e.g., the size and volume fraction of recrystallizedgrain） and the associated microstructure were performed. Good agreement is obtained between model predictions and experimentalresults, regarding flow stress, recrystallized fraction and grain size evolution. On this basis, a thermo-kinetic relationship upon thegrowth of recrystallized grain was elucidated, i.e., with increasing thermodynamic driving force, the activation energy barrierdecreases.

Effect of annealing temperature on microstructure and mechanical properties of cold-rolled commercially pure titanium sheets

The strength of traditional commercially pure titanium(CP-Ti) alloys often fails to meet the demand of structural materials. In order to enhance their mechanical properties, the cold-rolled CP-Ti alloys were annealed at different temperatures, and the recrystallization behavior and texture evolution were investigated. It was found that the bimodal microstructure(equiaxed and elongated grains) was formed after partial recrystallization, and the corresponding sample exhibited an excellent combination of ultimate tensile strength(702 MPa) and total elongation(36.4%). The recrystallization nucleation of CP-Ti sheets occurred preferentially in the high strain and the high-angle grain boundaries(HAGBs) regions. Meanwhile, the internal misorientations of the deformed heterogeneous grains increased and transformed into HAGBs, which further promoted the recrystallization nucleation. The main recrystallization texture was basal TD-split texture transformed from cold-rolled basal RD-split texture, and the oriented nucleation played a dominated role during recrystallization.

Growth Front Evolution of GaN Thin Films on Sapphire Substrate During HVPE

The growth front evolution of GaN thin films deposited on sapphire substrate by hydride vapor phase epitaxity has been studied with atomic force microscope. The evolution of the surface morphology presents four features of stage with the growth process. In initial growth stage, the surface is granular, and the typical grain diameter is about 250 nm for t =0.1 min. 3D growth plays a key role before the films come up to full coalescence, which causes a rough surface. After 0. 1 min the growth dimension decreases with the increase of lateral over growth, the surface roughness obviously decreases. From 0.4 min to 3 rain, the growth front roughness increases gradually, and the evolution of the surface roughness exhibits the characteristics of self-affined fractal. Beyond 3 min, the root-mean-square decreases gradually, which means the deposition behavior from hyper-2D growth gradually turns into layer growth mode with the increase of growth time.

Rice Husk Ash:A New Silicon Source for Preparing SAPO-34 Catalysts Used in the Methanol-to-Olefins Reaction

SAPO-34 molecular sieves were synthesized directly by hydrothermal method with rice husk ash(RHA)used as the silicon source.The crystal structure,composition,surface morphology and acidity of the synthesized products weresieves had a high crystallinity,without any impure phase.Compared with the SAPO-34 prepared by the silica sol,RHA-SAPO-34 had similar acid properties in strength.The methanol to olefins(MTO)experiments showed that the SAPO-34molecular sieve synthesized from RHA exhibited both a good catalytic activity and ethylene selectivity.

Mechanical properties of Mg-Gd-Zr alloy by Nd addition combined with hot extrusion

The effect of Nd addition on the microstructure and mechanical properties of as-extruded Mg-9Gd-0.5Zr(wt.%) alloy was investigated. The Mg-9Gd-0.5Zr and Mg-9Gd-2Nd-0.5Zr alloys were extruded at 673 K. The elongated non-dynamic recrystallized(un-DRXed) grains disappear after adding Nd, and uniformly distributed dynamic recrystallized grains with a grain size of 1.68 μm were obtained in the alloy. In addition, numerous nano-Mg5(Gd,Nd)particles were found to precipitate dynamically in the Mg-9Gd-2Nd-0.5Zr alloy, which gave rise to the dynamic recrystallization process via providing nucleation energy through hindering the release of deformation energy and promoting an increase in the strength through the Orowan strengthening mechanism. Moreover, the dynamically recrystallized(DRXed) grains have a weak texture, which plays a significant role in improving the ductility. Therefore,the Nd addition favors the improvement of strength and elongation for the as-extruded Mg-9Gd-0.5Zr alloy,simultaneously.

Microstructure and mechanical properties of TA15/TC11 graded structural material by wire arc additive manufacturing process

A graded structural material(GSM)with a material transition from TA15 to TC11 was fabricated by wire arc additive manufacturing(WAAM)method.The grain morphology,chemical composition,microstructure and mechanical properties of the as-deposited GSM were all characterized to investigate their variations along the deposition direction.The results indicate that from TA15 to TC11,the grain size decreases and a transition from columnar grains to equiaxed grains occurs.The content of alloy element alters greatly within a short distance,and the width of the mutation zone is 800μm.Both TA15 and TC11 regions exhibit basketweave microstructure withα-phase andβ-phase.However,during the transition from TA15 to TC11,theα-lath becomes fine,which leads to an increase in microhardness.The tensile test shows that the bonding strength at the interface is higher than the longitudinal strength of TA15,and the lateral elongation at the interface is higher than that of TA15 and TC11.

Effect of Al addition on microstructure and mechanical properties of Mg−Zn−Sn−Mn alloy

The microstructure and properties of the as-cast,as-homogenized and as-extruded Mg−6Zn−4Sn−1Mn(ZTM641)alloy with various Al contents(0,0.5,1,2,3 and 4 wt.%)were investigated by OM,XRD,DSC,SEM,TEM and uniaxial tensile tests.The results show that when the Al content is not higher than 0.5%,the alloys are mainly composed of α-Mg,Mg_(2)Sn,Al_(8)Mn_(5)and Mg_(7)Zn_(3)phases.When the Al content is higher than 0.5%,the alloys mainly consist ofα-Mg,Mg_(2)Sn,MgZn,Mg_(32)(Al,Zn)_(49),Al_(2)Mg_(5)Zn_(2),Al_(11)Mn_(4)and Al_(8)Mn_(5)phases.A small amount of Al(≤1%)can increase the proportion of fine dynamic recrystallized(DRXed)grains during hot-extrusion process.The roomtemperature tensile test results show that the ZTM641−1Al alloy has the best comprehensive mechanical properties,in which the ultimate tensile strength is 332 MPa,yield strength is 221 MPa and the elongation is 15%.Elevatedtemperature tensile test results at 150 and 200℃ show that ZTM641−2Al alloy has the best comprehensive mechanical properties.

Influence of dynamic recrystallization on microstructure and mechanical properties of welding zone in Al-Mg-Si aluminum profile during porthole die extrusion

The effect of dynamic recrystallization(DRX)on the microstructure and mechanical properties of 6063 aluminum alloy profile during porthole die extrusion was studied through experiment and simulation.The grain morphology was observed by means of electron backscatter diffraction(EBSD)technology.The results show that,at low ram speeds,increasing the ram speed caused an increase in DRX fraction due to the increase of temperature and strain rate.In contrast,at high ram speeds,further increasing ram speed had much less effect on the temperature,and the DRX faction decreased due to high stain rates.The microhardness and fraction of low angle boundaries in the welding zones were lower than those in the matrix zones.The grain size in the welding zone was smaller than that in the matrix zone due to lower DRX fraction.The decrease of grain size and increase of extrudate temperature were beneficial to the improvement of microhardness.

Relationship Between Iron Oxides and Surface Charge Characteristics in Soils

The relationship between iron oxides and surface charge characteristics in variable charge soils ( latosol and red earth ) was studied in following three ways. ( 1 ) Remove free iron oxides ( Fed ) and amorphous iron oxides ( Feo ) from the soils with sodium dithionite and acid ammonium oxalate solution respectively. ( 2 ) Add 2% glucose ( on the basis of air-dry soil weight ) to soils and incubate under submerged condition to activate iron oxides, and then the mixtures are dehydrated and air-dried to age iron oxides. ( 3 ) Precipitate various crystalline forms of iron oxides onto kaolinite. The results showed that free iron oxides ( Fed ) were the chief carrier of variable positive charges. Of which crystalline iron oxides ( Fed-Feo ) presented mainly as discrete particles in the soils and could only play a role of the carrier of positive charges, and did little influence on negative charges. Whereas the amorphous iron oxides ( Feo ) , which presented mainly as a coating with a large specific surface area, not only had positive charges, but also blocked the negative charge sites in soils. Submerged incubation activated iron oxides in the soils, and increased the amount of amorphous iron oxides and the degree of activation of iron oxide, which resulted in the increase of positive and negative charges of soils. Dehydration and air-dry aged iron oxides in soils and decreased the amount of amorphous iron oxides and the degree of activation of iron oxide, and also led to the decrease of positive and negative charges. Both the submerged incubation and the dehydration and air-dry had no significant influence on net charges. Precipitation of iron oxides onto kaolinite markedly increased positive charges and decreased negative charges. Amorphous iron oxide having a larger surface area contributed more positive charge sites and blocked more negative charge sites in kaolinite than crystalline goethite.

Effect of Si and Ti on dynamic recrystallization of high-performance Cu-15Ni-8Sn alloy during hot deformation

Effect of Si and Ti on dynamic recrystallization(DRX)of Cu-15Ni-8 Sn alloy was studied using hot compression tests over deformation temperature range of 750-950℃and strain rate range of 0.001-10 s^-1.The results show that the dynamic recrystallization behavior during hot deformation is significantly affected by the trace elements of Si and Ti.The addition of Si and Ti promotes the formation of Ni16Si7Ti6 particles during hot deformation,which promotes the nucleation of dynamic recrystallization by accelerating the transition from low-angle boundaries(LABs)to high-angle boundaries(HABs).Ni16Si7Ti6 particles further inhibit the growth of recrystallized grains through the pinning effect.Based on the dynamic recrystallization behavior,a processing map of the alloy is built up to obtain the optimal processing parameters.Guided by the processing map,a hot-extruded Cu-15 Ni-8Sn alloy with a fine-grained microstructure is obtained,which shows excellent elongation of 30%and ultimate tensile strength of 910 MPa.