This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction betwee...This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction between various structural materials and molten salts.The apparatus enables accurate detection of every phase change during hightemperature experiments,including strong reaction processes like corrosion.Molten salts,such as chlorides or fluo⁃rides,together with the structure materials,are inserted into either quartz or boron nitride capillaries,where X-ray diffraction pattern can be continuously collected,as the samples are heated to high temperature.The replacement re⁃action,when molten ZnCl2 are etching Ti3AlC2,can be clearly observed through changes in diffraction peak intensity as well as expansion in c-axis lattice parameter of the hexagonal matrix,due to the larger atomic number and ionic ra⁃dius of Zn2+.Furthermore,we investigated the high-temperature corrosion process when GH3535 alloy is in FLiNaK molten salt,and can help to optimize its stability for potential applications in molten salt reactor.Additionally,this high temperature apparatus is fully compatible with the combined usage of X-ray diffraction and Raman technique,providing both bulk and surface structural information.This high temperature apparatus has been open to users and is extensively used at BL14B1 beamline of the Shanghai Synchrotron Radiation Facility.展开更多
The pure γ-Ca2SiO4 （]t-C2S） phase was prepared at 1623 K of calcining temperature, 10 h of holding time and furnace cooling. The 13-C2S phase was obtained through γ-C2S conversion with the following calcination sy...The pure γ-Ca2SiO4 （]t-C2S） phase was prepared at 1623 K of calcining temperature, 10 h of holding time and furnace cooling. The 13-C2S phase was obtained through γ-C2S conversion with the following calcination system which was adopted at 1473 K of calcining temperature, 1 h of holding time and then water-cooling. The conversion rate of γ-C2S was studied by the Rietveld quantitative laboratory X-ray powder diffraction supported by synchrotron X-ray diffraction images. The refinement results show that the final conversion rate of γ-C2S is higher than 92%. The absolute error of the γ-C2S conversion rate between two Rietveld refinements （sample with or without α-Al2O3） is 3.6%, which shows that the Rietveld quantitative X-ray diffraction analysis is an appropriate and accurate method to quantify the γ-C2S conversion rate.展开更多
The phase transformations during thermomechanical processing can be employed to optimize mechanical properties of β-type Ti alloys.However,such understandings are still lacking for the alloy consisting of dual β+α&...The phase transformations during thermomechanical processing can be employed to optimize mechanical properties of β-type Ti alloys.However,such understandings are still lacking for the alloy consisting of dual β+α" phases in solution-treated and quenched state.In this paper,the phase transformations in a Ti38 Nb model alloy subjected to different thermomechanical processing were investigated by using synchrotron X-ray diffraction(SXRD) experiments,and their influence on the Young’s modulus was discussed.The results indicated that highdensity dislocations introduced by cold rolling still existed after annealing at temperatures lower than 573 K,which can decrease the martensitic transformation start temperature to below room temperature.With annealing temperatures increasing,the α"→β,β→ω_(iso),and β→α phase transformations occurred successively.At annealing temperature of 473 K,the specimen consisted of a trace of α"and ω phases as well as dominant β phase which was kept to room temperature by the high density of dislocations,rather than by the chemical stabilization.As a result,an ultralow Young’s modulus of 25.9 GPa was realized.Our investigation not only provides in-depth understandings of the phase transformations during thermomechanical processing of β-type Ti alloys,but also sheds light on designing biomedical Ti alloys with ultralow Young’s modulus.展开更多
The effect of the solute(Mo)on the stress development of nanocrystalline Ni and Ni-Mo films upon heat-ing has been investigated in real time using in situ synchrotron X-ray diffraction.The complex and distinct relatio...The effect of the solute(Mo)on the stress development of nanocrystalline Ni and Ni-Mo films upon heat-ing has been investigated in real time using in situ synchrotron X-ray diffraction.The complex and distinct relationship between the film stress and grain boundaries(GBs)has been examined by the evolution of real-time intrinsic stress in combination with the in situ grain growth and thermal characterizations.The different intrinsic stress evolutions in the Ni and Ni-Mo films during the heating process result from the modification of GBs by Mo alloying,including GB amorphization,GB relaxation,and GB segregation.It has been found that GBs play a vital role in the stress development of nanocrystalline films.The addition of a solute can not only inhibit grain growth but also influence the stress evolution in the film by changing the atomic diffusivity at the GBs.This work provides valuable and unique insights into the effect of solutes on stress development in nanocrystalline films during annealing,permitting control of the film stress through solute addition and heat treatment,which is critical for improving the design,processing,and lifetime of advanced nanocrystalline film devices at high temperatures.展开更多
The pressure effect on the crystalline structure of the I-II- V semiconductor Li（Zn,Mn）As ferromagnet is studied using in situ high-pressure x-ray diffraction and diamond anvil cell techniques. A phase transition st...The pressure effect on the crystalline structure of the I-II- V semiconductor Li（Zn,Mn）As ferromagnet is studied using in situ high-pressure x-ray diffraction and diamond anvil cell techniques. A phase transition starting at -11.6GPa is found. The space group of the high-pressure new phase is proposed as Pmca. Fitting with the Birch-Murnaghan equation of state, the bulk modulus B0 and its pressure derivative B0 of the ambient pressure structure with space group of F43m are B0 = 75.4 GPa and B0 = 4.3, respectively.展开更多
The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction....The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction.No phase transition was detected over the experimental temperature range.Using(Berman in J Petrol29:445-522,1988.10.1093/petrology/29.2.445)equations to fit the temperature-volume data,the volumetric thermal expansion coefficients at ambient conditions(α_(V0))of MgTiO_(3) and FeTiO_(3) were obtained as follows:2.55(6)×10^(-5)K^(-1)and 2.82(10)×10^(-5)K^(-1),respectively.We infer that the larger effective ionic radius of Fe^(2+)(Ⅵ)(0.78 A)than that of Mg^(2+)(Ⅵ)(0.72?)renders FeTiO_(3)has a larger volumetric thermal expansivity than MgTiO_(3).Simultaneously,the refined axial thermal expansion coefficients under ambient conditions areα_(a0)=0.74(3)×10^(-5)K^(-1)andα_(c0)=1.08(5)×10^(-5)K^(-1)for the aaxis and c-axis of MgTiO_(3),respectively,andα_(a0)=0.95(5)×10^(-5)K^(-1)andα_(c0)=0.92(12)×10^(-5)K^(-1)for the aaxis and c-axis of FeTiO_(3),respectively.The axial thermal expansivity of MgTiO_(3) is anisotropic,but that of FeTiO_(3) is nearly isotropic.We infer that the main reason for the different axial thermal expansivity between MgTiO_(3) and FeTiO_(3) is that the thermal expansion mode of the Mg-O bond in MgTiO_(3) is different from that of the Fe-O bonds in FeTiO_(3).展开更多
The phase evolution and thermal expansion behavior in superalloy during heating play an essential role in controlling the size and distribution of precipitates,as well as optimizing thermomechanical properties.Synchro...The phase evolution and thermal expansion behavior in superalloy during heating play an essential role in controlling the size and distribution of precipitates,as well as optimizing thermomechanical properties.Synchrotron X-ray diffraction is able to go through the interior of sample and can be carried out with in situ environment,and thus,it can obtain more statistics information in real time comparing with traditional methods,such as electron and optical microscopies.In this study,in situ heating synchrotron X-ray diffraction was carried out to study the phase evolution in a typicalγ′phase precipitation strengthened Ni-based superalloy,Waspaloy,from 29 to 1050°C.Theγ′,γ,M_(23)C_(6)and M C phases,including their lattice parameters,misfits,dissolution behavior and thermal expansion coefficients,were mainly investigated.Theγ′phase and M_(23)C_(6)carbides appeared obvious dissolution during heating and re-precipitated when the temperature dropped to room temperature.Combining with the microscopy results,we can indicate that the dissolution of M_(23)C_(6)leads to the growth of grain andγ′phase cannot be completely dissolved for the short holding time above the solution temperature.Besides,the coefficients of thermal expansions of all the phases are calculated and fitted as polynomials.展开更多
In situ synchrotron X-ray diffraction experiments of SWCNT （single-walled carbon nanotube） electrode in alkali halide aqueous electrolyte at several applied potentials were performed, and the change in the diffracti...In situ synchrotron X-ray diffraction experiments of SWCNT （single-walled carbon nanotube） electrode in alkali halide aqueous electrolyte at several applied potentials were performed, and the change in the diffraction pattern of SWCNTs was observed. It was found that the position of the 100 diffraction peak does not change with applied potential while the peak intensity decreases with anion adsorption. It was concluded that the space inside the tube would be the important ion adsorption site for the well-gown SWCNT bundles.展开更多
Pyrrhotite naturally occurs in various superstructures including magnetic(4C)and non-magnetic(5C,6C)types,each with distinct physicochemical properties and flotation behaviors.Challenges in accurately identifying and ...Pyrrhotite naturally occurs in various superstructures including magnetic(4C)and non-magnetic(5C,6C)types,each with distinct physicochemical properties and flotation behaviors.Challenges in accurately identifying and quantifying these superstructures hinder the optimization of pyrrhotite depression in flotation processes.To address this critical issue,synchrotron X-ray powder diffraction(S-XRPD)with Rietveld refinement was employed to quantify the distribution of superstructures in the feed and flotation concentrates of a copper–gold ore.To elucidate the mechanisms influencing depression,density functional theory(DFT)calculations were conducted to explore the electronic structures and surface reactivity of the pyrrhotite superstructures toward the adsorption of water,oxygen and hydroxyl ions(OH-)as dominant species present in the flotation process.S-XRPD analysis revealed that flotation recovery rates of pyrrhotite followed the order of 4C<6C<5C.DFT calculations indicated that the Fe 3d and S 3p orbital band centers exhibited a similar trend relative to the Fermi level with 4C being the closest.The Fe3d band center suggested that the 4C structure possessed a more reactive surface toward the oxygen reduction reaction,promoting the formation of hydrophilic Fe-OH sites.The S 3p band center order also implied that xanthate on the non-magnetic 5C and 6C surfaces could oxidize to dixanthogen,increasing hydrophobicity and floatability,while 4C formed less hydrophobic metal-xanthate complexes.Adsorption energy and charge transfer analyses of water,hydroxyl ions and molecular oxygen further supported the high reactivity and hydrophilic nature of 4C pyrrhotite.The strong bonding with hydroxyl ions indicated enhanced surface passivation by hydrophilic Fe–OOH complexes,aligning with the experimentally observed flotation order(4C<6C<5C).These findings provide a compelling correlation between experimental flotation results and electronic structure calculations,delivering crucial insights for optimizing flotation processes and improving pyrrhotite depression.This breakthrough opens up new opportunities to enhance the efficiency of flotation processes in the mining industry.展开更多
Magnesium(Mg)alloys typically exhibit anisotropic mechanical behaviors due to their hexagonal close-packed(hcp)crystal structures,often leading to tension-compression asymmetries.Understanding of the asymmetrical and ...Magnesium(Mg)alloys typically exhibit anisotropic mechanical behaviors due to their hexagonal close-packed(hcp)crystal structures,often leading to tension-compression asymmetries.Understanding of the asymmetrical and related deformation mechanisms is crucial for their structural applications,particularly in the lightweight transportation industries.Nevertheless,the underlying deformation mechanisms(e.g.,slip versus twinning)at each deformation stage during tension and compression have not been fully understood.In this study,we employed tensile and compressive tests on extruded Al and Mn containing Mg alloy,i.e.,an AM alloy Mg-0.6Mn-0.5Al-0.5Zn-0.4Ca,during the synchrotron X-ray diffraction.Our results show that distinct deformation behaviors and mechanisms in tension and compression are associated with the strong texture in the extruded samples:(i)The tensile deformation is dominated by dislocation slips,with activation of non-basal<a>and<c+a>slip,but deformation twinning is suppressed.(ii)The compressive deformation shows early-stage tensile twinning,followed by dislocation slips.Twinning induces grain reorientation,leading to significant lattice strain evolution aligned with the texture.The pronounced tension-compression asymmetry is attributed to the favorable shear stress direction formed in the twinning system during compression,which facilitates the activation of tensile twins.During tension,the strain hardening rate(SHR)drops significantly after yielding due to limited activated slip systems.In contrast,the samples under compression exhibit significant increases in SHR after yielding.During compression,dislocation multiplication dominates the initial strain hardening,while twinning progressively contributes more significantly than dislocation slip at higher strains.This study improves our understanding of the tension-compression and strain hardening asymmetries in extruded AM Mg alloys.展开更多
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.Exten...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.展开更多
The detrimental phase transformations of sodium layered transition metal oxides(Na_(x)TMO_(2))during desodiation/sodiation seriously suppress their practical applications for sodium ion batteries(SIBs).Undoubtedly,com...The detrimental phase transformations of sodium layered transition metal oxides(Na_(x)TMO_(2))during desodiation/sodiation seriously suppress their practical applications for sodium ion batteries(SIBs).Undoubtedly,comprehensively investigating of the dynamic crystal structure evolutions of Na_(x)TMO_(2)associating with Na ions extraction/intercalation and then deeply understanding of the relationships between electrochemical performances and phase structures drawing support from advanced characterization techniques are indispensable.In-situ high-energy X-ray diffraction(HEXRD),a powerful technology to distinguish the crystal structure of electrode materials,has been widely used to identify the phase evolutions of Na_(x)TMO_(2)and then profoundly revealed the electrochemical reaction processes.In this review,we begin with the descriptions of synchrotron characterization techniques and then present the advantages of synchrotron X-ray diffraction(XRD)over conventional XRD in detail.The optimizations of structural stability and electrochemical properties for P2-,O3-,and P2/O3-type Na_(x)TMO_(2)cathodes through single/dual-site substitution,high-entropy design,phase composition regulation,and surface engineering are summarized.The dynamic crystal structure evolutions of Na_(x)TMO_(2)polytypes during Na ion extraction/intercalation as well as corresponding structural enhancement mechanisms characterizing by means of HEXRD are concluded.The interior relationships between structure/component of Na_(x)TMO_(2)polytypes and their electrochemical properties are discussed.Finally,we look forward the research directions and issues in the route to improve the electrochemical properties of Na_(x)TMO_(2)cathodes for SIBs in the future and the combined utilizations of multiple characterization techniques.This review will provide significant guidelines for rational designs of high-performance Na_(x)TMO_(2)cathodes.展开更多
The microstructural factors contributing to the high strength of additive-manufactured Al-Si alloys us-ing laser-beam powder bed fusion(PBF-LB)were identified by in-situ synchrotron X-ray diffraction in tensile deform...The microstructural factors contributing to the high strength of additive-manufactured Al-Si alloys us-ing laser-beam powder bed fusion(PBF-LB)were identified by in-situ synchrotron X-ray diffraction in tensile deformation and transmission electron microscopy.PBF-LB and heat treatment were employed to manufacture Al-12%Si binary alloy specimens with different microstructures.At an early stage of de-formation prior to macroscopic yielding,stress was dominantly partitioned into the α-Al matrix,rather than the Si phase in all specimens.Highly concentrated Si solute(~3%)in the α-Al matrix promoted the dynamic precipitation of nanoscale Si phase during loading,thereby increasing the yield strength.After macroscopic yielding,the partitioned stress in the Si phase monotonically increased in the strain-hardening regime with an increase in the dislocation density in the α-Al matrix.At a later stage of strain hardening,the flow curves of the partitioned stress in the Si phase yielded stress relaxation owing to plastic deformation.Therefore,Si-phase particles localized along the cell walls in the cellular-solidified microstructure play a significant role in dislocation obstacles for strain hardening.Compared with the results of the heat-treated specimens with different microstructural factors,the dominant strengthening factors of PBF-LB manufactured Al-Si alloys were discussed.展开更多
As one of the heterostructures,the layered structure has attracted extensive research interest as it achieves superior properties to individual components.The layer interface is considered a critical fac-tor in determ...As one of the heterostructures,the layered structure has attracted extensive research interest as it achieves superior properties to individual components.The layer interface is considered a critical fac-tor in determining the mechanical properties of layered metals,where heterogeneity across the interface results in the strengthening of the soft layer and forming an interfacial stress gradient in the hard layer.However,there is still limited research associated with the formation of interfacial stress gradients in the hard layer,as stress measurement at high spatial resolution remains technically challenging.In the present study,we experimentally quantified the formation of interfacial stress gradients in the Ti layer of Ti/Al layered metal upon tension using in-situ high-energy X-ray diffraction(XRD).The analysis cou-pling in-situ high-energy XRD and in-situ electron back-scattered diffraction(EBSD)suggested that the interfacial stress gradient in the Ti layer rapidly rose as the Al layer was insufficient to accommodate the deformation of Ti.During the later deformation stage,collective effects of dislocation motion and geometrically necessary dislocation(GND)accumulation in the Al layer determined the evolution of in-terfacial stress gradients.The maximum interfacial stress gradient is below 0.4 MPa/μm in Ti layers,with a constant range width of 35μm independent of the macroscopic strain.The present study therefore opens a new window to local stress modification using incompatible component deformation,which is instructive for the design and fabrication of high-performance layered metals.展开更多
Characterizing the microstructure and deformation mechanism associated with the performances and properties of metallic materials is of great importance in understanding the microstructure-property relationship.The pa...Characterizing the microstructure and deformation mechanism associated with the performances and properties of metallic materials is of great importance in understanding the microstructure-property relationship.The past few decades have witnessed the rapid development of characterization techniques from optical microscopy to electron microscopy,although these conventional methods are generally limited to the sample surface because of the intrinsic opaque nature of metallic materials.Advanced synchrotron radiation(SR)facilities can produce X-rays with strong penetrability and high spatiotemporal resolution,and thereby enabling the non-destructive visualization of full-field structural information in three dimensions.Tremendous endeavors were devoted to the 3 rd generation SR over the past three decades,in which X-ray beams have been focused down to 100 nm.In this paper,recent progresses on SR-related characterization technologies were reviewed,with particular emphases on the fundamentals of synchrotron X-ray imaging and synchrotron X-ray diffraction,as well as their applications in the in situ observations of material preparation(e.g.,in situ dendrite growth during solidification)and service under extreme environment(e.g.,in situ mechanics).Future innovations toward next-generation SR and newly emerging SRbased technologies such as dark-field X-ray microscopy and Bragg coherent X-ray diffraction imaging were also advocated.展开更多
The deformation behavior of the as-extruded Mg-Y-Ni alloys with different volume fraction of long period stacking ordered(LPSO)phase during tension and compression was investigated by in-situ synchrotron diffraction.T...The deformation behavior of the as-extruded Mg-Y-Ni alloys with different volume fraction of long period stacking ordered(LPSO)phase during tension and compression was investigated by in-situ synchrotron diffraction.The micro-yielding,macro-yielding,tension-compression asymmetry and strain hardening behavior of the alloys were explored by combining with deformation mechanisms.The micro-yielding is dominated by basal slip of dynamic recrystallized(DRXed)grains in tension,while it is dominated by extension twinning of non-dynamic recrystallized(non-DRXed)grains in compression.At macro-yielding,the non-DRXed grains are still elastic deformed in tension and the basal slip of DRXed grains in compression are activated.Meanwhile,the LPSO phase still retains elastic deformation,but can bear more load,so the higher the volume fraction of hard LPSO phase,the higher the tensile/compressive macro-yield strength of the alloys.Benefiting from the low volume fraction of the non-DRXed grains and the delay effect of LPSO andγphases on extension twinning,the as-extruded alloys exhibit excellent tension-compression symmetry.When the volume fraction of LPSO phase reaches∼50%,tension-compression asymmetry is reversed,which is due to the fact that the LPSO phase is stronger in compression than in tension.The tensile strain hardening behavior is dominated by dislocation slip,while the dominate mechanism for compressive strain hardening changes from twinning in theα-Mg grains to kinking of the LPSO phase with increasing volume fraction of LPSO phase.The activation of kinking leads to the constant compressive strain hardening rate of∼2500 MPa,which is significantly higher than the tensile strain hardening rate.展开更多
Tantalum nitride （TAN） compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature （HPHT） method. The crystal structure and atom occupations of WC-type TaN have been investigated...Tantalum nitride （TAN） compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature （HPHT） method. The crystal structure and atom occupations of WC-type TaN have been investigated by neutron powder diffraction, and the compressibility of WC-type TaN has been investigated by using in-situ high-pressure synchrotron x-ray diffraction. The third-order Birch-Murnaghan equation of state fitted to the x-ray diffraction pressure- volume （P-V） sets of data, collected up to 41 GPa, yields ambient pressure isothermal bulk moduli of B0 = 369（2） GPa with pressure derivatives of B~ = 4 for the WC-type TaN. The bulk modulus of WC-type TaN is not in good agreement with the previous result （Bo = 351 GPa）, which is close to the recent theoretical calculation result （Bo = 378 GPa）. An analysis of the experiment results shows that crystal structure of WC-type TaN can be viewed as alternate stacking of Ta and N layers along the c direction, and the covalent Ta-N bonds between Ta and N layers along the c axis in the crystal structure play an important role in the incompressibility and hardness of WC-type TaN.展开更多
Synchrotron polychromatic X-ray microdiffraction（micro-XRD） was applied to study in situ deformation twinning of commercially AZ31（Mg-3Al-1Zn） strip subjected to uniaxial tension.The morphology and growth of twins...Synchrotron polychromatic X-ray microdiffraction（micro-XRD） was applied to study in situ deformation twinning of commercially AZ31（Mg-3Al-1Zn） strip subjected to uniaxial tension.The morphology and growth of twins were analyzed in situ under the load level from 64 to 73 MPa.The X-ray microdiffraction data,collected on beamline 12.3.2 at the Advanced Light Source,were then used to map an area of 396μm x 200μm within the region of interest.The experimental set-up and X-ray diffraction microscopy with a depth resolution allow the position and orientation of each illuminated grain to be determined at the submicron size.A list of parent grains sorted by crystallographic orientation were selected to examine their twinning behavior.The results depict twin variant selection,local misorientation fluctuation and mosaic spread for multi-twins within the same parent grain.As load increases,the amplitude of misorientation fluctuation along twin trace keeps increasing.This is attributable to the accumulation of geometrically necessary dislocations.展开更多
The microstructure evolution and micromechanical behaviors of additively manufactured 18Ni_(3)00 marag-ing steel for both as-printed and aged one were investigated using the in situ high-energy X-ray diffrac-tion(HE-X...The microstructure evolution and micromechanical behaviors of additively manufactured 18Ni_(3)00 marag-ing steel for both as-printed and aged one were investigated using the in situ high-energy X-ray diffrac-tion(HE-XRD)technique with uniaxial tensile tests.The investigations revealed that the volume frac-tion of reversed austenite increased as the annealing temperature rose.The maraging steel was strength-ened byη-Ni_(3)Ti precipitates,where the aged maraging steel had a higher UTS value of∼1860 MPa than∼1135 MPa in the as-printed one,but sacrificed more than half of ductility(from∼8.6%to∼4.0%).The austenite in aged steel presents more stability induced by the aging process than that in as-printed counterpart,which has a higher critical martensitic transformation stress of∼1200 MPa than that of∼780 MPa in as-printed steel.The austenite grains orientated with[200]//LD yield before the macro-yielding and preferential martensite transformation occurs.This study provides further insight into the intricated micromechanical responses of additively manufactured 18Ni_(3)00 maraging steel,enlarging the scope of its adaptation and application.展开更多
Nano-scale chemical inhomogeneity in surface oxide films formed on a V-and N-containing martensite stainless steel and tempering heating induced changes are investigated by a combination of synchrotron-based hard X-ra...Nano-scale chemical inhomogeneity in surface oxide films formed on a V-and N-containing martensite stainless steel and tempering heating induced changes are investigated by a combination of synchrotron-based hard X-ray Photoelectron emission spectroscopy(HAXPES)and microscopy(HAXPEEM)as well as microscopic X-ray absorption spectroscopy(μ-XAS)techniques.The results reveal the inhomogeneity in the oxide films on the micron-sized Cr_(2)N-and VN-type particles,while the inhomogeneity on the martensite matrix phase exists due to localised formation of nano-sized tempering nitride particles at 600℃.The oxide film formed on Cr_(2)N-type particles is rich in Cr_(2)O_(3) compared with that on the martensite matrix and VN-type particles.With the increase of tempering temperature,Cr_(2)O_(3) formation is faster for the oxidation of Cr in the martensite matrix than the oxidation of Cr nitride-rich particles.展开更多
基金CAS Photon Science Research Center for Carbon DioxideCAS President’s International Fellowship Initiative(2024PVA0097)+1 种基金National Key Research and Development Program of China(2017YFA0403000,2017YFA0402800)National Natural Science Foundation of China(U1932201,U1732121)。
文摘This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction between various structural materials and molten salts.The apparatus enables accurate detection of every phase change during hightemperature experiments,including strong reaction processes like corrosion.Molten salts,such as chlorides or fluo⁃rides,together with the structure materials,are inserted into either quartz or boron nitride capillaries,where X-ray diffraction pattern can be continuously collected,as the samples are heated to high temperature.The replacement re⁃action,when molten ZnCl2 are etching Ti3AlC2,can be clearly observed through changes in diffraction peak intensity as well as expansion in c-axis lattice parameter of the hexagonal matrix,due to the larger atomic number and ionic ra⁃dius of Zn2+.Furthermore,we investigated the high-temperature corrosion process when GH3535 alloy is in FLiNaK molten salt,and can help to optimize its stability for potential applications in molten salt reactor.Additionally,this high temperature apparatus is fully compatible with the combined usage of X-ray diffraction and Raman technique,providing both bulk and surface structural information.This high temperature apparatus has been open to users and is extensively used at BL14B1 beamline of the Shanghai Synchrotron Radiation Facility.
基金Project supported by the National Natural Science Foundation of China(No.51102181)the National Basic Research Program (973) of China(No.2009CB623104)the Open Fund of Large Apparatus of Tongji University(Nos.0002012004 and 0002012012),China
文摘The pure γ-Ca2SiO4 （]t-C2S） phase was prepared at 1623 K of calcining temperature, 10 h of holding time and furnace cooling. The 13-C2S phase was obtained through γ-C2S conversion with the following calcination system which was adopted at 1473 K of calcining temperature, 1 h of holding time and then water-cooling. The conversion rate of γ-C2S was studied by the Rietveld quantitative laboratory X-ray powder diffraction supported by synchrotron X-ray diffraction images. The refinement results show that the final conversion rate of γ-C2S is higher than 92%. The absolute error of the γ-C2S conversion rate between two Rietveld refinements （sample with or without α-Al2O3） is 3.6%, which shows that the Rietveld quantitative X-ray diffraction analysis is an appropriate and accurate method to quantify the γ-C2S conversion rate.
基金financially supported by the Fundamental Research Funds for the Central Universities (No.2017QNA04)。
文摘The phase transformations during thermomechanical processing can be employed to optimize mechanical properties of β-type Ti alloys.However,such understandings are still lacking for the alloy consisting of dual β+α" phases in solution-treated and quenched state.In this paper,the phase transformations in a Ti38 Nb model alloy subjected to different thermomechanical processing were investigated by using synchrotron X-ray diffraction(SXRD) experiments,and their influence on the Young’s modulus was discussed.The results indicated that highdensity dislocations introduced by cold rolling still existed after annealing at temperatures lower than 573 K,which can decrease the martensitic transformation start temperature to below room temperature.With annealing temperatures increasing,the α"→β,β→ω_(iso),and β→α phase transformations occurred successively.At annealing temperature of 473 K,the specimen consisted of a trace of α"and ω phases as well as dominant β phase which was kept to room temperature by the high density of dislocations,rather than by the chemical stabilization.As a result,an ultralow Young’s modulus of 25.9 GPa was realized.Our investigation not only provides in-depth understandings of the phase transformations during thermomechanical processing of β-type Ti alloys,but also sheds light on designing biomedical Ti alloys with ultralow Young’s modulus.
基金supported by the National Natural Science Foundation of China (No.51971153)the National Key Research and Development Program of China (No.2017YFE0302600)。
文摘The effect of the solute(Mo)on the stress development of nanocrystalline Ni and Ni-Mo films upon heat-ing has been investigated in real time using in situ synchrotron X-ray diffraction.The complex and distinct relationship between the film stress and grain boundaries(GBs)has been examined by the evolution of real-time intrinsic stress in combination with the in situ grain growth and thermal characterizations.The different intrinsic stress evolutions in the Ni and Ni-Mo films during the heating process result from the modification of GBs by Mo alloying,including GB amorphization,GB relaxation,and GB segregation.It has been found that GBs play a vital role in the stress development of nanocrystalline films.The addition of a solute can not only inhibit grain growth but also influence the stress evolution in the film by changing the atomic diffusivity at the GBs.This work provides valuable and unique insights into the effect of solutes on stress development in nanocrystalline films during annealing,permitting control of the film stress through solute addition and heat treatment,which is critical for improving the design,processing,and lifetime of advanced nanocrystalline film devices at high temperatures.
基金Supported by the National Natural Science Foundation and the Ministry of Science and Technology of Chinathe National Natural Science Foundation of China under Grant No U1530402+3 种基金the U.S. Department of Energy of Office of Science under Grant No DE-AC02-06CH11357the DOE-NNSA under Grant No DE-NA0001974the DOE-BES under Grant No DE-FG02-99ER45775the Instrumentation Funding of National Science Foundation
文摘The pressure effect on the crystalline structure of the I-II- V semiconductor Li（Zn,Mn）As ferromagnet is studied using in situ high-pressure x-ray diffraction and diamond anvil cell techniques. A phase transition starting at -11.6GPa is found. The space group of the high-pressure new phase is proposed as Pmca. Fitting with the Birch-Murnaghan equation of state, the bulk modulus B0 and its pressure derivative B0 of the ambient pressure structure with space group of F43m are B0 = 75.4 GPa and B0 = 4.3, respectively.
基金supported by National Natural Science Foundation of China(U2032118 and 42172048)Guizhou Provincial Science and Technology Projects(QKHPTRCYQK[2023]035 and QKHJC-ZK[2021]ZD042)+1 种基金Hundred Talents Program of the Chinese Academy of SciencesGuizhou Provincial 2020 and 2021 Science and Technology Subsidies(Nos.GZ2020SIG and GZ2021SIG)。
文摘The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction.No phase transition was detected over the experimental temperature range.Using(Berman in J Petrol29:445-522,1988.10.1093/petrology/29.2.445)equations to fit the temperature-volume data,the volumetric thermal expansion coefficients at ambient conditions(α_(V0))of MgTiO_(3) and FeTiO_(3) were obtained as follows:2.55(6)×10^(-5)K^(-1)and 2.82(10)×10^(-5)K^(-1),respectively.We infer that the larger effective ionic radius of Fe^(2+)(Ⅵ)(0.78 A)than that of Mg^(2+)(Ⅵ)(0.72?)renders FeTiO_(3)has a larger volumetric thermal expansivity than MgTiO_(3).Simultaneously,the refined axial thermal expansion coefficients under ambient conditions areα_(a0)=0.74(3)×10^(-5)K^(-1)andα_(c0)=1.08(5)×10^(-5)K^(-1)for the aaxis and c-axis of MgTiO_(3),respectively,andα_(a0)=0.95(5)×10^(-5)K^(-1)andα_(c0)=0.92(12)×10^(-5)K^(-1)for the aaxis and c-axis of FeTiO_(3),respectively.The axial thermal expansivity of MgTiO_(3) is anisotropic,but that of FeTiO_(3) is nearly isotropic.We infer that the main reason for the different axial thermal expansivity between MgTiO_(3) and FeTiO_(3) is that the thermal expansion mode of the Mg-O bond in MgTiO_(3) is different from that of the Fe-O bonds in FeTiO_(3).
基金supported by the National Natural Science Foundation of China(NSFC)(Grant Nos.11805009 and 51921001)the Fundamental Research Funds for the Central Universities(Grant No.06111020)。
文摘The phase evolution and thermal expansion behavior in superalloy during heating play an essential role in controlling the size and distribution of precipitates,as well as optimizing thermomechanical properties.Synchrotron X-ray diffraction is able to go through the interior of sample and can be carried out with in situ environment,and thus,it can obtain more statistics information in real time comparing with traditional methods,such as electron and optical microscopies.In this study,in situ heating synchrotron X-ray diffraction was carried out to study the phase evolution in a typicalγ′phase precipitation strengthened Ni-based superalloy,Waspaloy,from 29 to 1050°C.Theγ′,γ,M_(23)C_(6)and M C phases,including their lattice parameters,misfits,dissolution behavior and thermal expansion coefficients,were mainly investigated.Theγ′phase and M_(23)C_(6)carbides appeared obvious dissolution during heating and re-precipitated when the temperature dropped to room temperature.Combining with the microscopy results,we can indicate that the dissolution of M_(23)C_(6)leads to the growth of grain andγ′phase cannot be completely dissolved for the short holding time above the solution temperature.Besides,the coefficients of thermal expansions of all the phases are calculated and fitted as polynomials.
文摘In situ synchrotron X-ray diffraction experiments of SWCNT （single-walled carbon nanotube） electrode in alkali halide aqueous electrolyte at several applied potentials were performed, and the change in the diffraction pattern of SWCNTs was observed. It was found that the position of the 100 diffraction peak does not change with applied potential while the peak intensity decreases with anion adsorption. It was concluded that the space inside the tube would be the important ion adsorption site for the well-gown SWCNT bundles.
基金supported by the Australian Research Council Linkage Project(No.LP200200717)co sponsored by Newmont Corporation(United States)and Vega Industries(India)+1 种基金the Powder Diffraction Beamline at the Australia’s Nuclear Science and Technology Organisation(No.PDR19870),Australiathe Centre for Microscopy and Microanalysis at the University of Queensland(No.1366),Australia。
文摘Pyrrhotite naturally occurs in various superstructures including magnetic(4C)and non-magnetic(5C,6C)types,each with distinct physicochemical properties and flotation behaviors.Challenges in accurately identifying and quantifying these superstructures hinder the optimization of pyrrhotite depression in flotation processes.To address this critical issue,synchrotron X-ray powder diffraction(S-XRPD)with Rietveld refinement was employed to quantify the distribution of superstructures in the feed and flotation concentrates of a copper–gold ore.To elucidate the mechanisms influencing depression,density functional theory(DFT)calculations were conducted to explore the electronic structures and surface reactivity of the pyrrhotite superstructures toward the adsorption of water,oxygen and hydroxyl ions(OH-)as dominant species present in the flotation process.S-XRPD analysis revealed that flotation recovery rates of pyrrhotite followed the order of 4C<6C<5C.DFT calculations indicated that the Fe 3d and S 3p orbital band centers exhibited a similar trend relative to the Fermi level with 4C being the closest.The Fe3d band center suggested that the 4C structure possessed a more reactive surface toward the oxygen reduction reaction,promoting the formation of hydrophilic Fe-OH sites.The S 3p band center order also implied that xanthate on the non-magnetic 5C and 6C surfaces could oxidize to dixanthogen,increasing hydrophobicity and floatability,while 4C formed less hydrophobic metal-xanthate complexes.Adsorption energy and charge transfer analyses of water,hydroxyl ions and molecular oxygen further supported the high reactivity and hydrophilic nature of 4C pyrrhotite.The strong bonding with hydroxyl ions indicated enhanced surface passivation by hydrophilic Fe–OOH complexes,aligning with the experimentally observed flotation order(4C<6C<5C).These findings provide a compelling correlation between experimental flotation results and electronic structure calculations,delivering crucial insights for optimizing flotation processes and improving pyrrhotite depression.This breakthrough opens up new opportunities to enhance the efficiency of flotation processes in the mining industry.
文摘Magnesium(Mg)alloys typically exhibit anisotropic mechanical behaviors due to their hexagonal close-packed(hcp)crystal structures,often leading to tension-compression asymmetries.Understanding of the asymmetrical and related deformation mechanisms is crucial for their structural applications,particularly in the lightweight transportation industries.Nevertheless,the underlying deformation mechanisms(e.g.,slip versus twinning)at each deformation stage during tension and compression have not been fully understood.In this study,we employed tensile and compressive tests on extruded Al and Mn containing Mg alloy,i.e.,an AM alloy Mg-0.6Mn-0.5Al-0.5Zn-0.4Ca,during the synchrotron X-ray diffraction.Our results show that distinct deformation behaviors and mechanisms in tension and compression are associated with the strong texture in the extruded samples:(i)The tensile deformation is dominated by dislocation slips,with activation of non-basal<a>and<c+a>slip,but deformation twinning is suppressed.(ii)The compressive deformation shows early-stage tensile twinning,followed by dislocation slips.Twinning induces grain reorientation,leading to significant lattice strain evolution aligned with the texture.The pronounced tension-compression asymmetry is attributed to the favorable shear stress direction formed in the twinning system during compression,which facilitates the activation of tensile twins.During tension,the strain hardening rate(SHR)drops significantly after yielding due to limited activated slip systems.In contrast,the samples under compression exhibit significant increases in SHR after yielding.During compression,dislocation multiplication dominates the initial strain hardening,while twinning progressively contributes more significantly than dislocation slip at higher strains.This study improves our understanding of the tension-compression and strain hardening asymmetries in extruded AM Mg alloys.
基金supported by the National Natural Science Foundation of China(Nos.52171098 and 51921001)the State Key Laboratory for Advanced Metals and Materials(No.2022Z-02)+1 种基金the National High-level Personnel of Special Support Program(No.ZYZZ2021001)the Fundamental Research Funds for the Central Universities(Nos.FRF-TP-20-03C2 and FRF-BD-20-02B).
文摘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.
基金supported by the State Grid Corporation Science and Technology Project(No.5419-202158503A-0-5-ZN)。
文摘The detrimental phase transformations of sodium layered transition metal oxides(Na_(x)TMO_(2))during desodiation/sodiation seriously suppress their practical applications for sodium ion batteries(SIBs).Undoubtedly,comprehensively investigating of the dynamic crystal structure evolutions of Na_(x)TMO_(2)associating with Na ions extraction/intercalation and then deeply understanding of the relationships between electrochemical performances and phase structures drawing support from advanced characterization techniques are indispensable.In-situ high-energy X-ray diffraction(HEXRD),a powerful technology to distinguish the crystal structure of electrode materials,has been widely used to identify the phase evolutions of Na_(x)TMO_(2)and then profoundly revealed the electrochemical reaction processes.In this review,we begin with the descriptions of synchrotron characterization techniques and then present the advantages of synchrotron X-ray diffraction(XRD)over conventional XRD in detail.The optimizations of structural stability and electrochemical properties for P2-,O3-,and P2/O3-type Na_(x)TMO_(2)cathodes through single/dual-site substitution,high-entropy design,phase composition regulation,and surface engineering are summarized.The dynamic crystal structure evolutions of Na_(x)TMO_(2)polytypes during Na ion extraction/intercalation as well as corresponding structural enhancement mechanisms characterizing by means of HEXRD are concluded.The interior relationships between structure/component of Na_(x)TMO_(2)polytypes and their electrochemical properties are discussed.Finally,we look forward the research directions and issues in the route to improve the electrochemical properties of Na_(x)TMO_(2)cathodes for SIBs in the future and the combined utilizations of multiple characterization techniques.This review will provide significant guidelines for rational designs of high-performance Na_(x)TMO_(2)cathodes.
基金JST PRESTO(grant number JPMJPR22Q4)(Japan)The Light Metal Educational Foundation,Inc.(Japan),and“Knowledge Hub Aichi”Aichi Prefectural Government(Japan)The synchrotron radiation experiments were performed at BL46XUof SPring-8with the approval of the Japan Synchrotron Radiation Research Institute(JASRI)(Proposal No.2021A1663,2022A1001and 2022A1798).
文摘The microstructural factors contributing to the high strength of additive-manufactured Al-Si alloys us-ing laser-beam powder bed fusion(PBF-LB)were identified by in-situ synchrotron X-ray diffraction in tensile deformation and transmission electron microscopy.PBF-LB and heat treatment were employed to manufacture Al-12%Si binary alloy specimens with different microstructures.At an early stage of de-formation prior to macroscopic yielding,stress was dominantly partitioned into the α-Al matrix,rather than the Si phase in all specimens.Highly concentrated Si solute(~3%)in the α-Al matrix promoted the dynamic precipitation of nanoscale Si phase during loading,thereby increasing the yield strength.After macroscopic yielding,the partitioned stress in the Si phase monotonically increased in the strain-hardening regime with an increase in the dislocation density in the α-Al matrix.At a later stage of strain hardening,the flow curves of the partitioned stress in the Si phase yielded stress relaxation owing to plastic deformation.Therefore,Si-phase particles localized along the cell walls in the cellular-solidified microstructure play a significant role in dislocation obstacles for strain hardening.Compared with the results of the heat-treated specimens with different microstructural factors,the dominant strengthening factors of PBF-LB manufactured Al-Si alloys were discussed.
基金supported by the National Key Re-search&Development Plan(No.2022YFE0110600)the National Natural Science Foundation of China(Nos.52201122,92263201,52171117,and 52371113)+1 种基金the Jiangsu Funding Program for Excel-lent Postdoctoral Talent(No.2022ZB366)the China Postdoc-toral Science Foundation Funded Project(No.2023M731636).
文摘As one of the heterostructures,the layered structure has attracted extensive research interest as it achieves superior properties to individual components.The layer interface is considered a critical fac-tor in determining the mechanical properties of layered metals,where heterogeneity across the interface results in the strengthening of the soft layer and forming an interfacial stress gradient in the hard layer.However,there is still limited research associated with the formation of interfacial stress gradients in the hard layer,as stress measurement at high spatial resolution remains technically challenging.In the present study,we experimentally quantified the formation of interfacial stress gradients in the Ti layer of Ti/Al layered metal upon tension using in-situ high-energy X-ray diffraction(XRD).The analysis cou-pling in-situ high-energy XRD and in-situ electron back-scattered diffraction(EBSD)suggested that the interfacial stress gradient in the Ti layer rapidly rose as the Al layer was insufficient to accommodate the deformation of Ti.During the later deformation stage,collective effects of dislocation motion and geometrically necessary dislocation(GND)accumulation in the Al layer determined the evolution of in-terfacial stress gradients.The maximum interfacial stress gradient is below 0.4 MPa/μm in Ti layers,with a constant range width of 35μm independent of the macroscopic strain.The present study therefore opens a new window to local stress modification using incompatible component deformation,which is instructive for the design and fabrication of high-performance layered metals.
基金financially supported by the National Key Research and Development Plan(Grant Nos.2020YFA0405900,2017YFA0403803)the National Natural Science Foundation of China(Grant No.51927801)the Natural Science Foundation of Jiangsu Province(Grant No.BK20202010)。
文摘Characterizing the microstructure and deformation mechanism associated with the performances and properties of metallic materials is of great importance in understanding the microstructure-property relationship.The past few decades have witnessed the rapid development of characterization techniques from optical microscopy to electron microscopy,although these conventional methods are generally limited to the sample surface because of the intrinsic opaque nature of metallic materials.Advanced synchrotron radiation(SR)facilities can produce X-rays with strong penetrability and high spatiotemporal resolution,and thereby enabling the non-destructive visualization of full-field structural information in three dimensions.Tremendous endeavors were devoted to the 3 rd generation SR over the past three decades,in which X-ray beams have been focused down to 100 nm.In this paper,recent progresses on SR-related characterization technologies were reviewed,with particular emphases on the fundamentals of synchrotron X-ray imaging and synchrotron X-ray diffraction,as well as their applications in the in situ observations of material preparation(e.g.,in situ dendrite growth during solidification)and service under extreme environment(e.g.,in situ mechanics).Future innovations toward next-generation SR and newly emerging SRbased technologies such as dark-field X-ray microscopy and Bragg coherent X-ray diffraction imaging were also advocated.
基金supported by National Natural Science Foundation of China(no.U21A2047,no.51971076 and no.52001069).
文摘The deformation behavior of the as-extruded Mg-Y-Ni alloys with different volume fraction of long period stacking ordered(LPSO)phase during tension and compression was investigated by in-situ synchrotron diffraction.The micro-yielding,macro-yielding,tension-compression asymmetry and strain hardening behavior of the alloys were explored by combining with deformation mechanisms.The micro-yielding is dominated by basal slip of dynamic recrystallized(DRXed)grains in tension,while it is dominated by extension twinning of non-dynamic recrystallized(non-DRXed)grains in compression.At macro-yielding,the non-DRXed grains are still elastic deformed in tension and the basal slip of DRXed grains in compression are activated.Meanwhile,the LPSO phase still retains elastic deformation,but can bear more load,so the higher the volume fraction of hard LPSO phase,the higher the tensile/compressive macro-yield strength of the alloys.Benefiting from the low volume fraction of the non-DRXed grains and the delay effect of LPSO andγphases on extension twinning,the as-extruded alloys exhibit excellent tension-compression symmetry.When the volume fraction of LPSO phase reaches∼50%,tension-compression asymmetry is reversed,which is due to the fact that the LPSO phase is stronger in compression than in tension.The tensile strain hardening behavior is dominated by dislocation slip,while the dominate mechanism for compressive strain hardening changes from twinning in theα-Mg grains to kinking of the LPSO phase with increasing volume fraction of LPSO phase.The activation of kinking leads to the constant compressive strain hardening rate of∼2500 MPa,which is significantly higher than the tensile strain hardening rate.
基金Project supported by the Research Foundation of Key Laboratory of Neutron Physics(Grant No.2015BB03)the National Natural Science Foundation of China(Grant Nos.11774247)+2 种基金the Science Foundation for Excellent Youth Scholars of Sichuan University(Grant No.2015SCU04A04)the Joint Usage/Research Center PRIUS(Ehime University,Japan)Chinese Academy of Sciences(Grant No.2017-BEPC-PT-000568)
文摘Tantalum nitride （TAN） compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature （HPHT） method. The crystal structure and atom occupations of WC-type TaN have been investigated by neutron powder diffraction, and the compressibility of WC-type TaN has been investigated by using in-situ high-pressure synchrotron x-ray diffraction. The third-order Birch-Murnaghan equation of state fitted to the x-ray diffraction pressure- volume （P-V） sets of data, collected up to 41 GPa, yields ambient pressure isothermal bulk moduli of B0 = 369（2） GPa with pressure derivatives of B~ = 4 for the WC-type TaN. The bulk modulus of WC-type TaN is not in good agreement with the previous result （Bo = 351 GPa）, which is close to the recent theoretical calculation result （Bo = 378 GPa）. An analysis of the experiment results shows that crystal structure of WC-type TaN can be viewed as alternate stacking of Ta and N layers along the c direction, and the covalent Ta-N bonds between Ta and N layers along the c axis in the crystal structure play an important role in the incompressibility and hardness of WC-type TaN.
基金Project(DP140102355)supported by the Australian Research Council(ARC)Project supported by the China Scholarship Council(CSC)
文摘Synchrotron polychromatic X-ray microdiffraction（micro-XRD） was applied to study in situ deformation twinning of commercially AZ31（Mg-3Al-1Zn） strip subjected to uniaxial tension.The morphology and growth of twins were analyzed in situ under the load level from 64 to 73 MPa.The X-ray microdiffraction data,collected on beamline 12.3.2 at the Advanced Light Source,were then used to map an area of 396μm x 200μm within the region of interest.The experimental set-up and X-ray diffraction microscopy with a depth resolution allow the position and orientation of each illuminated grain to be determined at the submicron size.A list of parent grains sorted by crystallographic orientation were selected to examine their twinning behavior.The results depict twin variant selection,local misorientation fluctuation and mosaic spread for multi-twins within the same parent grain.As load increases,the amplitude of misorientation fluctuation along twin trace keeps increasing.This is attributable to the accumulation of geometrically necessary dislocations.
基金supported by the National Key Research and De-velopment Program of China(No.2023YFB3711901)the National Natural Science Foundation of China(NSFC)(Nos.52171098 and 51921001)+2 种基金the State Key Laboratory for Advanced Metals and Ma-terials(Grant No.2022Z-02)the Fundamental Research Funds for the Central Universities(No.FRF-TP-20-03C2)supported by the U.S.Department of En-ergy,Office of Science,Office of Basic Energy Sciences,under Con-tract No.DE-AC02-06CH11357.
文摘The microstructure evolution and micromechanical behaviors of additively manufactured 18Ni_(3)00 marag-ing steel for both as-printed and aged one were investigated using the in situ high-energy X-ray diffrac-tion(HE-XRD)technique with uniaxial tensile tests.The investigations revealed that the volume frac-tion of reversed austenite increased as the annealing temperature rose.The maraging steel was strength-ened byη-Ni_(3)Ti precipitates,where the aged maraging steel had a higher UTS value of∼1860 MPa than∼1135 MPa in the as-printed one,but sacrificed more than half of ductility(from∼8.6%to∼4.0%).The austenite in aged steel presents more stability induced by the aging process than that in as-printed counterpart,which has a higher critical martensitic transformation stress of∼1200 MPa than that of∼780 MPa in as-printed steel.The austenite grains orientated with[200]//LD yield before the macro-yielding and preferential martensite transformation occurs.This study provides further insight into the intricated micromechanical responses of additively manufactured 18Ni_(3)00 maraging steel,enlarging the scope of its adaptation and application.
基金supported by the Vinnova(project number 2020-03778)supported by the Swedish Research Council(Vetenskapsradet,project number 2021-04157).
文摘Nano-scale chemical inhomogeneity in surface oxide films formed on a V-and N-containing martensite stainless steel and tempering heating induced changes are investigated by a combination of synchrotron-based hard X-ray Photoelectron emission spectroscopy(HAXPES)and microscopy(HAXPEEM)as well as microscopic X-ray absorption spectroscopy(μ-XAS)techniques.The results reveal the inhomogeneity in the oxide films on the micron-sized Cr_(2)N-and VN-type particles,while the inhomogeneity on the martensite matrix phase exists due to localised formation of nano-sized tempering nitride particles at 600℃.The oxide film formed on Cr_(2)N-type particles is rich in Cr_(2)O_(3) compared with that on the martensite matrix and VN-type particles.With the increase of tempering temperature,Cr_(2)O_(3) formation is faster for the oxidation of Cr in the martensite matrix than the oxidation of Cr nitride-rich particles.
