Microstructures and micromechanical behaviors of high -entropy alloys investigated by synchrotron X-ray and neutron diffraction techniques: A review

High-entropy alloys(HEAs)possess outstanding features such as corrosion resistance,irradiation resistance,and good mechan-ical properties.A few HEAs have found applications in the fields of aerospace and defense.Extensive studies on the deformation mech-anisms of HEAs can guide microstructure control and toughness design,which is vital for understanding and studying state-of-the-art structural materials.Synchrotron X-ray and neutron diffraction are necessary techniques for materials science research,especially for in situ coupling of physical/chemical fields and for resolving macro/microcrystallographic information on materials.Recently,several re-searchers have applied synchrotron X-ray and neutron diffraction methods to study the deformation mechanisms,phase transformations,stress behaviors,and in situ processes of HEAs,such as variable-temperature,high-pressure,and hydrogenation processes.In this review,the principles and development of synchrotron X-ray and neutron diffraction are presented,and their applications in the deformation mechanisms of HEAs are discussed.The factors that influence the deformation mechanisms of HEAs are also outlined.This review fo-cuses on the microstructures and micromechanical behaviors during tension/compression or creep/fatigue deformation and the application of synchrotron X-ray and neutron diffraction methods to the characterization of dislocations,stacking faults,twins,phases,and intergrain/interphase stress changes.Perspectives on future developments of synchrotron X-ray and neutron diffraction and on research directions on the deformation mechanisms of novel metals are discussed.

Creep rupture properties and microstructure stability of the GH984G alloy tube

GH984G alloy is a significant candidate material for 650-700℃ ultra-supercritical coal-fired generating units.In this paper,creep rupture properties and microstructure stability of the GH984G alloy tube were studied,and the findings indicated excellent creep rupture properties at 700℃.Furthermore,the extrapolated strength for 100000 h was found to be 153.8 MPa,which satisfies the requirements for the long-term performance of high-temperature materials in power stations.Aging at 700℃ with the extension of time,the grain boundary carbides and the particle size of the γ′phase on the matrix gradually coarsen,but its spherical morphology remains uniformly distributed.However,no harmful phase precipitates were found even after aging at 700℃ for up to 19144 h.Excellent microstructure stability guarantees the 700℃ creep rupture properties of the GH984G alloy tube.

Microstructure Distribution Characteristics of High-Strength Aluminum Alloy Thin-Walled Tubes during Multi-Passes Hot Power Backward Spinning Process

The microstructure of the thin-walled tubes with high-strength aluminum alloy determines their final forming quality and performance. This type of tube can be manufactured by multi-pass hot power backward spinning process as it can eliminate casting defects, refine microstructure and improve the plasticity of the tube. To analyze the microstructure distribution characteristics of the tube during the spinning process, a 3D coupled thermo-mechanical FE model coupled with the microstructure evolution model of the process was established under the ABAQUS environment. The microstructure evolution characteristics and laws of the tube for the whole spinning process were analyzed. The results show that the dynamic recrystallization is mainly produced in the spinning deformation zone and root area of the tube. In the first pass, the dynamic recrystallization phenomenon is not obvious in the tube. With the pass increasing, the trend of dynamic recrystallization volume percentage gradually increases and extends from the outer surface of the tube to the inner surface. The fine-grained area shows the states of concentration, dispersion, and re-concentration as the pass number increases. .

Microstructure and mechanical properties of BFe10 cupronickel alloy tubes fabricated by a horizontal continuous casting with heating-cooling combined mold technology

A new horizontal continuous casting method with heating-cooling combined mold （HCCM） technology was explored for fabri- cating high-quality thin-wall cupronickel alloy tubes used for heat exchange pipes. The microstructure and mechanical properties of BFe 10 cupronickel alloy tubes fabricated by HCCM and traditional continuous casting （cooling mold casting） were comparatively investigated. The results show that the tube fabricated by HCCM has smooth internal and external surfaces without any defects, and its internal and external surface roughnesses are 0.64 μm and 0.85 μm, respectively. The tube could be used for subsequent cold processing without other treatments such as surface planning, milling and acid-washing. This indicates that HCCM can effectively reduce the process flow and improve the pro- duction efficiency of a BFel0 cupronickel alloy tube. The tube has columnar grains along its axial direction with a major casting texture of {012}〈 621 〉. Compared with cooling mold casting （6 = 36.5%）, HCCM can improve elongation （3 = 46.3%） by 10% with a slight loss of strength, which indicates that HCCM remarkably improves the cold extension performance of a BFe 10 cupronickel alloy tube.

Microstructure evolution of a recycled Al-Fe-Si-Cu alloy processed by tube channel pressing

Although excellent recyclability is one of the advantages of Al alloys, a recycling process can reduce different properties of these alloys by adding coarse AlFeSi particles into the alloys' microstructures. One of the well-known methods for modifying the microstructure of metallic materials is the imposition of severe plastic deformation(SPD). Nevertheless, the microstructure evolutions of recycled Al alloys containing extraordinary fractions of AlFeSi particles during SPD processing have seldom been considered. The aim of the present work is to study the microstructure evolution of a recycled Al–Fe–Si–Cu alloy during SPD processing. For this purpose, tubular specimens of the mentioned alloy were subjected to different numbers of passes of a recently developed SPD process called tube channel pressing(TCP); their microstructures were then studied using different techniques. The results show that coarse AlFeSi particles are fragmented into finer particles after processing by TCP. However, decomposition and dissolution of AlFeSi particles through TCP processing are negligible. In addition, TCP processing results in an increase in hardness of the alloy, which is attributed to the refinement of grains, to an increase of the dislocation density, and to the fragmentation of AlFeSi particles.

MICROSTRUCTURE AND MECHANICAL PROPERTIES OF AZ91D EXTRUDED TUBE

The effect of extrusion ratio on microstruetures and mechanical properties of magnesium alloy AZ91D extruded tube at 430℃ has been studied. After the evolution of microstracture and mechanical properties of AZ91D during extrusion were studied, the following parameters were obtained： tensile strength reached the climax value of 306.9MPa and elongation peak value of 10.1% at an extrusion ratio of 7.125, and with the increase of the extrusion ratio to 7.45, yield strength reached a top value of 285.795MPa with decreased tensile strength and elongation. It was concluded that mechanical properties of magnesium alloys AZ91D could be enhanced by adjusting the extrusion ratio near recrystallization.

Microstructure Evolution of Sandstone Cemented by Microbe Cement Using X-ray Computed Tomography

The bio-sandstone, which was cemented by microbe cement, was firstly prepared, and then the microstructure evolution process was studied by X-ray computed tomography （X-CT） technique. The experimental results indicate that the microstructure of bio-sandstone becomes dense with the development of age. The evolution of inner structure at different positions is different due to the different contents of microbial induced precipitation calcite. Besides, the increase rate of microbial induced precipitation calcite gradually decreases because of the reduction of microbe absorption content with the decreasing pore size in bio-sandstone.

Microstructure and properties of TP2 copper tube with La microalloying by horizontal continuous casting

The TP2 copper tube was prepared with La microalloying by horizontal continuous casting(HCC). The absorptivity of La and its effects on microstructure, tensile and corrosion properties of HCC TP2 copper tube were studied by means of the inductively coupled plasma optical emission spectrometer(ICP-OES), optical microscope(OM), scanning electron microscope(SEM) and potentiodynamic polarization measurements. The results show that the absorptivity of La in the HCC TP2 copper tube is about 15% under antivacuum conditions due to the good chemical activities of La. The impurity elements in copper tube such as O, S, Pb and Si can be significantly reduced, and the average columnar dendrite spacing of the copper tube can also be reduced from 2.21 mm to 0.93 mm by adding La. The ultimate tensile strength and the elongation with and without La addition are almost unchanged. However, the annual corrosion rate of the HCC TP2 copper tube is reduced from 10.18 mm·a^(-1) to 9.37 mm·a^(-1) by the purification effect of trace La.

Microstructure and performance of biodegradable magnesium alloy tubes fabricated by local-heating-assisted dieless drawing

Magnesium(Mg)alloy stents are expected to be the next generation of stents because of good biocompatibility and biodegradability.Compared with cold drawing,dieless drawing with local heating is an effective method for manufacturing the Mg alloy microtubes since a large reduction in area can be achieved in a single pass.However,the microstructure and properties of dieless drawn tubes have not been clarified,leading to the problems in practical application of dieless drawn tubes.In this study,the microstructure and performance of dieless drawn tubes are clarified.The results show that temperature and speed in the dieless drawing process are two factors in determining the grain size of dieless drawn tubes since decreasing the temperature or increasing the speed promotes the generation of fine-grained microstructure.Twins are also generated during the dieless drawing process,which 1)disintegrates grains leading to refinement and 2)causes Hall-Petch law effect on dieless drawn tubes.Tensile tests show that grain size is the main factor in determining the mechanical properties of dieless drawn tubes,namely,0.2%proof stress 135-180MPa,ultimate tensile strength(UTS)200-250MPa,and elongation 8-12%.In 0.9 wt%NaCl solution,localized corrosion is the key factor in initiating the corrosion of dieless drawn tubes,but refined grains and fewer twins can alleviate local corrosion.These results imply that dieless drawn tubes are promising in the clinical application of Mg alloy stents for cardiovascular disease.

Application of X-ray Computed Tomography in Characterization Microstructure Changes of Cement Pastes in Carbonation Process

The microstructure characteristics and meso-defect volume changes of hardened cement paste before and after carbonation were investigated by three-dimensional （3D） X-ray computed tomograpby （XCT）, where three types water-to-cement ratio of 0.53, 0.35 and 0.23 were considered. The high-resolution 3D images of microstructure and filtered defects were reconstructed by an XCT VG Studio MAX 2.0 software, The meso- defect volume fractions and size distribution were analyzed based on 3D images through add-on modules of 3D defect analysis. The 3D meso-defects volume fractions before carbonation were 0.79%, 0.38% and 0.05% corresponding to w/c ratio=0.53, 0.35 and 0.23, respectively. The 3D meso-defects volume fractions after carbonation were 2.44%, 0.91% and 0.14% corresponding to w/c ratio=0.53, 0.35 and 0.23, respectively. The experimental results suggest that 3D meso-defects volume fractions after carbonation for above three w/c ratio increased significantly. At the same time, meso-cracks distribution of the carbonation shrinkage and gray values changes of the different w/c ratio and carbonation reactions were also investigated.

Effect of extrusion ratios on hardness,microstructure,and crystal texture anisotropy in pure niobium tubes subjected to hydrostatic extrusion

Nb tubes were fabricated through hydrostatic extrusion at extrusion ratios of 3.1 and 6.1 at ambient temperature,and then their microstructure,texture,and Vickers hardness were investigated based on electron back-scattered diffraction(EBSD)data.The fraction of low-angle boundaries(LABs)largely decreased with a sharp decrease in mean grain sizes after hydrostatic extrusion and was not proportional to extrusion ratios,assuming that mixed-asymmetrical junctions forming LABs dissociate at high extrusion ratios from the external stress(>981 MPa)with thermal activation by the generated heat.The correlation between grain size and Vickers hardness followed the Hall−Petch relationship despite the texture gradient of theá111ñcyclic fiber textural microstructure at low extrusion ratios and theá100ñtrue fiber textural microstructure at high extrusion ratios.The increase in hydrostatic pressure on the Nb tubes contributed to texture evolution in terms of extrusion ratios due to the difference between{110}<111>and{112}<111>components based on EBSD data.

Enhanced in-vitro degradation resistance and cytocompatibility of a thermomechanically processed novel Mg alloy:Insights into the role of microstructural attributes

The role of microstructural features on in-vitro degradation and surface film development of a thermomechanically processed Mg-4Zn-0.5Ca-0.8Mn alloy has been investigated employing electrochemical studies,scanning electron microscopy and X-ray photoelectron spectroscopy.The specimen forged at 523 K temperature developed a coarse unimodal microstructure consisting of basal oriented grains,whereas the specimens forged at 623 K and 723 K temperatures exhibited bimodal microstructures containing randomly oriented fine grains and basal oriented coarse grains.The bimodal microstructures exerted higher resistance to corrosion compared to the unimodal microstructure in presence of a protective surface film.The optimum size distribution of fine and coarse grains as well as the prevalence of basal oriented grains led to the lowest anodic current density in the specimen forged at 623 K.The morphology of Ca_(2)Mg_(6)Zn_(3)precipitates governed the cathodic kinetics by controlling the anode to cathode surface area ratio.Despite the specimen forged at 723 K comprised comparatively lower fraction of precipitates than at 623 K,the mesh-like precipitate morphology increased the effective cathodic surface area,leading to enhanced localised corrosion in the former specimen.Optimal microstructural features developed at 623 K forging temperature formed a well-protective surface film with lower Mg(OH)_(2)to MgO ratio,exhibiting distinctly high polarization resistance and superior cytocompatibility in terms of cell-proliferation and cell-differentiation.

Effects of Ca addition on tensile properties and microstructures of hot-extruded AZ91 alloy tube

As-cast AZ91+XCa (X=0, 0.5%, 1.0%, 1.5%, mass fraction) magnesium alloys were extruded into tube at 380℃with an extrusion ratio of 6:1. The tensile properties and microstructures of extruded AZ91+XCa alloy tubes were investigated. The microstructural observation indicates that Ca can obviously refine bothα-Mg grains and Mg17Al12 phase of AZ91 magnesium alloy. XRD analysis shows that the microstructure of AZ91+0.5Ca alloy consists ofα-Mg solid solution and Mg17Al12 phase, while AZ91+1.5Ca alloy contains additionally Al2Ca phase. The tensile experimental results show that for the AZ91 alloy, the addition of Ca has little influence on the ambient temperature tensile properties but can improve the elevated temperature tensile properties. For the extruded AZ91+XCa alloys, the elevated temperature tensile strength decreases, and elongation increases with increasing the Ca content. The improvement in elevated temperature tensile strength of the alloy can be attributed to the presence of a Ca-containing phase, which can increase the microstructural stability of the alloy at elevated temperature.

Process parameter effects on microstructure and mechanical properties of tubes processed via friction assisted tube straining method

This paper investigates process parameter effects on microstructure and mechanical properties of the tubes processed via recently developed friction assisted tube straining(FATS)method.For this purpose,design of experiment was used to arrange finite element analyses and experimental tests.Numerical and experimental tests were executed by changing rotary speed,feed rate and die angle.Taguchi design results show that increasing feed rate and decreasing rotary speed enhance Zener-Hollomon(Z)parameter and decrease average grain size,while die angle has no considerable effect.Increasing Z value reduces grain size and enhances flow stress of the processed samples,while the experiment with the highest Z value refines initial microstructure from 40 to 8μm and increases flow stress by 5 times.

Microstructure and mechanical properties evolution of 65Cu-35Zn brass tube during cyclic rotating−bending process

The cyclic rotating−bending(CRB)processes under different deformation conditions were carried out to refine the microstructure and improve the mechanical properties of the 65Cu−35Zn brass tubes.The microstructure and the mechanical properties in the axial direction of the tubes after the CRB process were studied with the OM,EBSD and conventional tensile test.To obtain the accumulated effective plastic strain of the tube during the CRB process,the FEM simulation was also executed.The results show that the average grain size decreases with the increase of rotation time at RT,and with the decrease of bending angle at 200℃.With the increase of accumulated effective plastic strain during the CRB process,the reduction rate of average grain size of the brass tube increases,the tensile strength of the brass tube increases in wave shape and the elongation increases first and then sharply decreases.

Microstructure of Pd_(77.5)Au_6Si_(16.5) Alloy Droplet Solidified in a Drop Tube Process

The microstructure development of Pd77.5Au6Si16.5 alloy droplet solidified in a drop tube process was studied. It was found that two distinct microstructures, i.e. (Pd,Au)3Si primary phase and Pd+(Pd,Au)3Si eutectic can be obtained when the droplet diameter is within the range between 2.3~0.4 mm. The morpologies of the (Pd,Au)3Si developed from dendrite trunk-like with single branching only into dendrite cluster-like with ternary branching with the decrease of the droplet diameter. When the droplet diameter is about 0.25 mm, the primary phase (Pd,Au)3Si almost disappears and the microstructure mainly shows Pd+(Pd,Au)3Si eutectic. The morphology of the eutectic transforms from fiber-like to plate-like with the decrease of the droplet diameter in the range between 2.3-0.25 mm. When the droplet diameter is about 0.19 mm, the microstructure is only the single phase of Pd solid solution

Studies of Microstructure of Kernels of Macadamia integrifolia and Its Hybrids through MRI, X-Ray Tomography and Confocal Microscopy

The aim of this study was to apply the existing techniques that enable examination ofmacadamia kernels to provide a better understanding of physico-chemical properties of kernels during postharvest processing. These techniques, such as X-ray tomography, could be applied for quality monitoring in the macadamia industry. The objectives of this study were to investigate the browning centre symptoms that usually occur in macadamia nuts-in-shell. The applied techniques included confocal microscopy, X-ray tomography and magnetic resonance imaging （MRI）. Five different varieties of macadamia nuts （A38, 246, 816, 842 and Daddow） were selected to include distinct characteristics, such as drop pattern and growing location. Analysis of the microstructure of kernels by confocal microscopy showed the distribution of possible brown pigment compounds as well as the distribution of lipids, carbohydrates and proteins inside macadamia cells. Physical properties data, including shell density and seed to volume ratio, were obtained by X-ray tomography. Magnetic resonance diffusion tensor imaging used in this study showed marked differences in microstructure which indicate that different varieties exhibit different microstructures expressed as fraction ofanisotropy and apparent diffusion coefficient that appear to be related to the occurrence of the brown centre. Hence, the findings of this study have potential to improve the existing postharvest techniques used in the macadamia processing industry. They will be of benefit to the industry in terms of improved quality control and cost reduction.

Effect of Three-High Rotary Piercing Process on Microstructure,Texture and Mechanical Properties of Magnesium Alloy Seamless Tube

Mg alloy seamless tubes(MASTs)were prepared through three-high rotary piercing process,effect of billet temperature,feed angle and plug advance on microstructure,texture and mechanical properties of tubes were investigated.The effect on the deformation mechanism and improving mechanical properties mechanism of this process for MASTs were studied.The results show that the grain size could be refined to 11.3-31.1%of the initial grain size and the microstructure was more uniform due to the accumulation of strain.The formation of high strain gradient at the grain boundary activated the non-basal slip.This piercing process could change the grain orientation of as-extruded billet and eliminate the initial basal texture to produce new favorable texture.And the process could accelerate the continuous dynamic recrystallization process.After piercing,yield strength of pierced tubes decreased by 6.7%,ultimate tensile strength(UTS)and elongation increased by 32.4 and 45%,respectively,at optimal parameters.The plate-shapedβ_(1)-Mg_(17)Al_(12) orientation transformed from basal plates to prismatic plates,facilitating the increase in UTS and ductility.The decrease size of nanoscale precipitates could reduce the cracking possibility.The critical resolved shear stress ratios of pyramidal(10−11)slip and(11−22)slip to basal slip for the sample including prismatic plates both decreased compared to that including basal plates.This could enhance the ductility of tube sample.Moreover,grain boundary sliding could contribute to a better ductility via coordinating deformation and reducing stress concentration during piercing process.

Processing and Microstructural Evolution of Superalloy Inconel 718 during Hot Tube Extrusion

The processing parameters of tube extrusion for superalloy Inconel 718 (IN 718), such as slug temperature, tools temperature, choice of lubricant, extrusion ratio and extrusion speed, were determined by experiment in this paper. An appropriate temperature range recommended for the slug is 1080-1120℃, and the temperature range recommended for the tools is 350-500℃. The microstructural evolution of superalloy IN 718 during tube extrusion was analyzed. With the increase of the deformation the cross crystal grains were slightly refined. While the vertical crystal grain is elongated evidently and the tensile strength increased along the axial rake. Glass lubricants have to be spread on the slug surface after being heated to 150-200℃, vegetable oil or animal oil can be used as the lubricant on the surface of the tools to reduce the extrusion force remarkably.

Improvements to conventional X-ray tube-based cone-beam computed tomography system

Conventional X-ray tube-based cone-beam computed tomography(CX-CBCT) systems have great potential in industrial applications. Such systems can rapidly obtain a three-dimensional(3D) image of an object.Conventional X-ray tubes fulfill the requirements for industrial applications, because of their high tube voltage and power. Continuous improvements have been made to CX-CBCT systems, such as imaging time shortening,acquisition strategy optimization, and imaging software development, etc. In this study, a CX-CBCT system is developed. Additionally, some improvements to the CX-CBCT system are proposed based on the hardware conditions of the X-ray tube and detector. A near-detector(ND)geometry condition is employed to obtain a sharper image and larger detection area. An improved acquisition strategy is proposed to simplify operations and reduce total imaging time. In the ND geometry condition, a simplified method called FBP slice stacking(SS-FBP) is proposed, which can be applied to 3D image reconstruction. SS-FBP is timesaving relative to traditional methods. Furthermore, imaging software for the CX-CBCT system is developed in the MATLAB environment. Several imaging experiments were performed. The results suggest that the CX-CBCT system works properly, and that the above improvements are feasible and practical.