Influence of supersaturation on the structure of a series of freshly prepared supersaturated sodium aluminate solutions with medium concentration was investigated by solution X-ray diffraction. Experimental results sh...Influence of supersaturation on the structure of a series of freshly prepared supersaturated sodium aluminate solutions with medium concentration was investigated by solution X-ray diffraction. Experimental results show that the basic Al-containing species in all kinds of supersaturated solution is four-coordinated ions. Opposite to Al-O distance contracted in highly concentrated solution, a little expand of the Al-O distance from 1.75 *@ to 1.85 *@ occurs with increasing supersaturation, which is consistent with the occurrence of oligomeric aluminate species. Meanwhile, O-O distance in the first shell of H 2O-H 2O(OH) in supersaturated sodium aluminate solution is obviously longer than in hydroxide sodium solution and becomes longer and longer with increasing supersaturation. Na-O bond length is about 2.4 *@ and changes little with supersaturation. The reason for Al-O bond expanding with supersaturation and its influence on the stability of solution was discussed.展开更多
The epitaxial relationships of lattices and crystalline qualities of LSMO/ZnO/sapphire double-hetero systems were thoroughly analyzed using X-ray diffraction techniques with a modern high resolution XRD system. It was...The epitaxial relationships of lattices and crystalline qualities of LSMO/ZnO/sapphire double-hetero systems were thoroughly analyzed using X-ray diffraction techniques with a modern high resolution XRD system. It was revealed that the epitaxial growth of the LSMO (110) phase was promoted under higher temperature accompanying the suppression of other competitive growth of the LSMO (001) and (111) phases. Supplying the plasma oxygen accelerated the suppression of the LSMO (111) phase. The complex epitaxial orientational relationships in these three growth modes were revealed from the precise analyses with the high resolution out-of-plane XRD and the in-plane XRD measurements, pole figure measurements, and reciprocal space mappings measurements, as [112ˉ](111)LSMO//[11ˉ00](0001)ZnO//[112ˉ0](0001)Sap, [110ˉ](111LSMO)//[11ˉ00](0001)Zno//[112ˉ0](0001)Sap, and [110](001)LSMO//[11ˉ00](0001)Zno//[112ˉ0](0001)Sap. The validity of this model for the epitaxial orientational relationships in LSMO/ZnO/sapphire double heteroepitaxial layers was confirmed identically with the data ana- lyses of the out-of-plane wide-range Reciprocal Space Mapping using the 2-dimensional X-ray detector.展开更多
The effects of solid solution on the deformation behavior of binary Mg-xZn(x=0,1,2 wt%)alloys featuring a designated texture that enables extension twinning under tension parallel to the basal pole in most grains,were...The effects of solid solution on the deformation behavior of binary Mg-xZn(x=0,1,2 wt%)alloys featuring a designated texture that enables extension twinning under tension parallel to the basal pole in most grains,were investigated using in-situ neutron diffraction and the EVPSC-TDT model.Neutron diffraction was used to quantitatively track grain-level lattice strains and diffraction intensity changes(related to mechanical twinning)in differently oriented grains of each alloy during cyclic tensile/compressive loadings.These measurements were accurately captured by the model.The stress-strain curves of Mg-1 wt%Zn and Mg-2 wt%Zn alloys show as-expected solid solution strengthening from the addition of Zn compared to pure Mg.The macroscopic yielding and hardening behaviors are explained by alternating slip and twinning modes as calculated by the model.The solid solution's influence on individual deformation modes,including basal〈a〉slip,prismatic〈a〉slip,and extension twinning,was then quantitatively assessed in terms of activity,yielding behavior,and hardening response by combining neutron diffraction results with crystal plasticity predictions.The Mg-1 wt%Zn alloy displays distinct yielding and hardening behavior due to solid solution softening of prismatic〈a〉slip.Additionally,the dependence of extension twinning,in terms of the twinning volume fraction,on Zn content exhibits opposite trends under tensile and compressive loadings.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
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
The low-dose X-ray induced long afterglow near infrared(NIR)luminescence from Cr^(3+)doped Zn_(1-x)Cd_(x)Ga_(2)O_(4)spinel solid solutions was investigated.The structure analysis shows the good formation of Zn_(1-x)Cd...The low-dose X-ray induced long afterglow near infrared(NIR)luminescence from Cr^(3+)doped Zn_(1-x)Cd_(x)Ga_(2)O_(4)spinel solid solutions was investigated.The structure analysis shows the good formation of Zn_(1-x)Cd_(x)Ga_(2)O_(4)spinel solid solutions,which possesses a cubic spinel structure with Fd3m space group.The formation of Zn_(1-x)Cd_(x)Ga_(2)O_(4)spinel solid solutions induces the obvious increase of long afterglow near infrared luminescence excited by low-dose X-ray,When the content of doped Cd^(2+)reaches 0.1,the low-dose X-ray induced long afterglow NIR luminescence is the maximum.More importantly,only 5 s Xray irradiation can induce more than 6 h NIR afterglow emission,of which the afterglow luminescent intensity is still 5 times stronger than the background intensity after 6 h.The thermoluminescent results show that under the 5 s exposure of X-ray,the trap density of Zn_(0.9)Cd_(0.1)Ga_(2)O_(4):Cr^(3+)is much higher than that of ZnGa_(2)O_(4):Cr^(3+).The replacement of Cd^(2+)ions with large radius at Zn^(2+)sites causes the increase of de fects and dislocations,which results in the obvious increase of trap co ncentrations.And the addition of high-z number elements Cd^(2+)would enhance the X-ray absorption of the solid solutions,which thus can be easily excited by low-dose X-ray.Zn_(0.9)Cd_(0.1)Ga_(2)O_(4):1%Cr^(3+)solid solution is a potential candidate of lowdose X-ray induced long afterglow luminescent materials.展开更多
A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, ...A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, Zr4＋, Ti4＋and Pb4＋cations are incorporated into the lattice of tetragonal rutile SnO2 to form a solid solution structure. As a consequence, the surface area and thermal stability of the catalysts are improved. Moreover, the oxygen species of the modified catalysts become easier to be reduced. Therefore, the oxidation activity over the catalysts was improved, except for the one modified by Pb oxide. Manganese oxide demonstrates the best promotional effects for SnO2. Using an X‐ray diffraction extrapolation method, the lattice capacity of SnO2 for Mn2O3 was 0.135 g Mn2O3/g SnO2, which indicates that to form stable solid solution, only 21%Sn4＋cations in the lattice can be maximally replaced by Mn3＋. If the amount of Mn3＋cations is over the capacity, Mn2O3 will be formed, which is not favorable for the activity of the catalysts. The Sn rich samples with only Sn‐Mn solid solution phase show higher activity than the ones with excess Mn2O3 species.展开更多
Detailed time-and-space-averaged structure of MgSO4 in the concentrated aqueous solutions was investigated via X-ray diffraction with an X’pert Pro θ-θ diffractometer at 298 K, yielding structural function and radi...Detailed time-and-space-averaged structure of MgSO4 in the concentrated aqueous solutions was investigated via X-ray diffraction with an X’pert Pro θ-θ diffractometer at 298 K, yielding structural function and radial distribution function（RDF）. The developed KURVLR program was employed for the theoretical investigation in consideration of the ionic hydration and ion association. Multi-peaks Gaussian fitting method was applied to deconvolving the overlapping bands of Differential radial distribution function（DRDF）. The calculation of the geometric model shows that octahedrally six-coordinated Mg（H2O）62＋, with an Mg2＋…OW bond length of 0.201 nm dominates in the solutions. There exists contact ion-pair（CIP） in the more concentrated solution（1：18, H2O/salt molar ratio） with a coordination number of 0.8 and a characteristic Mg…S distance of 0.340 nm. The result indicates the hydrated SO42– ion happens in the solution. The S…OW bond distance was determined to be 0.382 nm with a coordination number of 13. The fraction of CIP increases significantly with the increasing concentration. The symmetry of the hydration structure of sulfate ion is lowered by forming complex with magnesium ion.展开更多
In situ x-ray diffraction electrochemical method is used to study the activation of silver electrode in KCl solution and UPD lead on silver electrode surface. We found that the activation makes the silver crystal thic...In situ x-ray diffraction electrochemical method is used to study the activation of silver electrode in KCl solution and UPD lead on silver electrode surface. We found that the activation makes the silver crystal thicker in (111), and the arrangement of water molecules on the silver electrode surface with UPD lead is partially ordered.展开更多
In this paper we propose a new method for measuring the thickness of the GaN epilayer, by using the ratio of the integrated intensity of the GaN epilayer X-ray diffraction peaks to that of the sapphire substrate ones....In this paper we propose a new method for measuring the thickness of the GaN epilayer, by using the ratio of the integrated intensity of the GaN epilayer X-ray diffraction peaks to that of the sapphire substrate ones. This ratio shows a linear dependence on the GaN epilayer thickness up to 2 μm. The new method is more accurate and convenient than those of using the relationship between the integrated intensity of GaN epilayer diffraction peaks and the GaN thickness. Besides, it can eliminate the absorption effect of the GaN epilayer.展开更多
SrTiO3 thin films are epitaxially grown on DyScO3, LaAlO3 substrates with/without buffer layers of DyScO3 and SrRuO3 using laser-MBE. X-ray diffraction methods, such as high resolution X-ray diffraction, grazing incid...SrTiO3 thin films are epitaxially grown on DyScO3, LaAlO3 substrates with/without buffer layers of DyScO3 and SrRuO3 using laser-MBE. X-ray diffraction methods, such as high resolution X-ray diffraction, grazing incident X-ray diffraction, and reciprocal space mapping are used to investigate the lattice structure, dislocation density, in-plane lattice strain distribution along film thickness. From the measurement results, the effects of substrate on film lattice quality and microstructure are discussed.展开更多
A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus.The criterion of standardless X-ray diffraction analysis was suggested,so as ...A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus.The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.展开更多
A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus,The criterion of standardless X-ray diffraction analysis was suggested,so as ...A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus,The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.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 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
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
Beam splitting is one of the main approaches to achieving x-ray ghost imaging, and the intensity correlation between diffraction beam and transmission beam will directly affect the imaging quality. In this paper, we i...Beam splitting is one of the main approaches to achieving x-ray ghost imaging, and the intensity correlation between diffraction beam and transmission beam will directly affect the imaging quality. In this paper, we investigate the intensity correlation between the split x-ray beams by Laue diffraction of stress-free crystal. The analysis based on the dynamical theory of x-ray diffraction indicates that the spatial resolution of diffraction image and transmission image are reduced due to the position shift of the exit beam. In the experimental setup, a stress-free crystal with a thickness of hundredmicrometers-level is used for beam splitting. The crystal is in a non-dispersive configuration equipped with a double-crystal monochromator to ensure that the dimension of the diffraction beam and transmission beam are consistent. A correlation coefficient of 0.92 is achieved experimentally and the high signal-to-noise ratio of the x-ray ghost imaging is anticipated.Results of this paper demonstrate that the developed beam splitter of Laue crystal has the potential in the efficient data acquisition of x-ray ghost imaging.展开更多
Phase transition of polycrystalline iron compressed along the Hugoniot is studied by combining laser-driven shock with in situ x-ray diffraction technique.It is suggested that polycrystalline iron changes from an init...Phase transition of polycrystalline iron compressed along the Hugoniot is studied by combining laser-driven shock with in situ x-ray diffraction technique.It is suggested that polycrystalline iron changes from an initial body-centered cubic structure to a hexagonal close-packed structure with increasing pressure(i.e.,a phase transition fromαtoε).The relationship between density and pressure for polycrystalline iron obtained from the present experiments is found to be in good agreement with the gas-gun Hugoniot data.Our results show that experiments with samples at lower temperatures under static loading,such as in a diamond anvil cell,lead to higher densities measured than those found under dynamic loading.This means that extrapolating results of static experiments may not predict the dynamic responses of materials accurately.In addition,neither the face-centered cubic structure seen in previous molecular-dynamics simulations or twophase coexistence are found within our experimental pressure range.展开更多
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
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
文摘Influence of supersaturation on the structure of a series of freshly prepared supersaturated sodium aluminate solutions with medium concentration was investigated by solution X-ray diffraction. Experimental results show that the basic Al-containing species in all kinds of supersaturated solution is four-coordinated ions. Opposite to Al-O distance contracted in highly concentrated solution, a little expand of the Al-O distance from 1.75 *@ to 1.85 *@ occurs with increasing supersaturation, which is consistent with the occurrence of oligomeric aluminate species. Meanwhile, O-O distance in the first shell of H 2O-H 2O(OH) in supersaturated sodium aluminate solution is obviously longer than in hydroxide sodium solution and becomes longer and longer with increasing supersaturation. Na-O bond length is about 2.4 *@ and changes little with supersaturation. The reason for Al-O bond expanding with supersaturation and its influence on the stability of solution was discussed.
文摘The epitaxial relationships of lattices and crystalline qualities of LSMO/ZnO/sapphire double-hetero systems were thoroughly analyzed using X-ray diffraction techniques with a modern high resolution XRD system. It was revealed that the epitaxial growth of the LSMO (110) phase was promoted under higher temperature accompanying the suppression of other competitive growth of the LSMO (001) and (111) phases. Supplying the plasma oxygen accelerated the suppression of the LSMO (111) phase. The complex epitaxial orientational relationships in these three growth modes were revealed from the precise analyses with the high resolution out-of-plane XRD and the in-plane XRD measurements, pole figure measurements, and reciprocal space mappings measurements, as [112ˉ](111)LSMO//[11ˉ00](0001)ZnO//[112ˉ0](0001)Sap, [110ˉ](111LSMO)//[11ˉ00](0001)Zno//[112ˉ0](0001)Sap, and [110](001)LSMO//[11ˉ00](0001)Zno//[112ˉ0](0001)Sap. The validity of this model for the epitaxial orientational relationships in LSMO/ZnO/sapphire double heteroepitaxial layers was confirmed identically with the data ana- lyses of the out-of-plane wide-range Reciprocal Space Mapping using the 2-dimensional X-ray detector.
基金supported by the National Research Foundation grant funded by the Korean government(No,2023R1A2C2007190,RS-2024-00398068)partially funded by the Natural Science Foundation of Shandong Province,China(No.ZR2022QE206).
文摘The effects of solid solution on the deformation behavior of binary Mg-xZn(x=0,1,2 wt%)alloys featuring a designated texture that enables extension twinning under tension parallel to the basal pole in most grains,were investigated using in-situ neutron diffraction and the EVPSC-TDT model.Neutron diffraction was used to quantitatively track grain-level lattice strains and diffraction intensity changes(related to mechanical twinning)in differently oriented grains of each alloy during cyclic tensile/compressive loadings.These measurements were accurately captured by the model.The stress-strain curves of Mg-1 wt%Zn and Mg-2 wt%Zn alloys show as-expected solid solution strengthening from the addition of Zn compared to pure Mg.The macroscopic yielding and hardening behaviors are explained by alternating slip and twinning modes as calculated by the model.The solid solution's influence on individual deformation modes,including basal〈a〉slip,prismatic〈a〉slip,and extension twinning,was then quantitatively assessed in terms of activity,yielding behavior,and hardening response by combining neutron diffraction results with crystal plasticity predictions.The Mg-1 wt%Zn alloy displays distinct yielding and hardening behavior due to solid solution softening of prismatic〈a〉slip.Additionally,the dependence of extension twinning,in terms of the twinning volume fraction,on Zn content exhibits opposite trends under tensile and compressive loadings.
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.
基金Project supported by the State Key Research Project of Shandong Natural Science Foundation(ZR2020KB019)the fund of"Two-Hundred Talent"Plan of Yantai City+1 种基金the National Natural Science Foundation of China(11974013)the Natural Science Foundation of Fujian Province(2022J011270)。
文摘The low-dose X-ray induced long afterglow near infrared(NIR)luminescence from Cr^(3+)doped Zn_(1-x)Cd_(x)Ga_(2)O_(4)spinel solid solutions was investigated.The structure analysis shows the good formation of Zn_(1-x)Cd_(x)Ga_(2)O_(4)spinel solid solutions,which possesses a cubic spinel structure with Fd3m space group.The formation of Zn_(1-x)Cd_(x)Ga_(2)O_(4)spinel solid solutions induces the obvious increase of long afterglow near infrared luminescence excited by low-dose X-ray,When the content of doped Cd^(2+)reaches 0.1,the low-dose X-ray induced long afterglow NIR luminescence is the maximum.More importantly,only 5 s Xray irradiation can induce more than 6 h NIR afterglow emission,of which the afterglow luminescent intensity is still 5 times stronger than the background intensity after 6 h.The thermoluminescent results show that under the 5 s exposure of X-ray,the trap density of Zn_(0.9)Cd_(0.1)Ga_(2)O_(4):Cr^(3+)is much higher than that of ZnGa_(2)O_(4):Cr^(3+).The replacement of Cd^(2+)ions with large radius at Zn^(2+)sites causes the increase of de fects and dislocations,which results in the obvious increase of trap co ncentrations.And the addition of high-z number elements Cd^(2+)would enhance the X-ray absorption of the solid solutions,which thus can be easily excited by low-dose X-ray.Zn_(0.9)Cd_(0.1)Ga_(2)O_(4):1%Cr^(3+)solid solution is a potential candidate of lowdose X-ray induced long afterglow luminescent materials.
基金supported by the National Natural Science Foundation of China (21263015,21567016 and 21503106)the Education Department Foundation of Jiangxi Province (KJLD14005 and GJJ150016)the Natural Science Foundation of Jiangxi Province (20142BAB213013 and 20151BBE50006),which are greatly acknowledged by the authors~~
文摘A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, Zr4＋, Ti4＋and Pb4＋cations are incorporated into the lattice of tetragonal rutile SnO2 to form a solid solution structure. As a consequence, the surface area and thermal stability of the catalysts are improved. Moreover, the oxygen species of the modified catalysts become easier to be reduced. Therefore, the oxidation activity over the catalysts was improved, except for the one modified by Pb oxide. Manganese oxide demonstrates the best promotional effects for SnO2. Using an X‐ray diffraction extrapolation method, the lattice capacity of SnO2 for Mn2O3 was 0.135 g Mn2O3/g SnO2, which indicates that to form stable solid solution, only 21%Sn4＋cations in the lattice can be maximally replaced by Mn3＋. If the amount of Mn3＋cations is over the capacity, Mn2O3 will be formed, which is not favorable for the activity of the catalysts. The Sn rich samples with only Sn‐Mn solid solution phase show higher activity than the ones with excess Mn2O3 species.
基金Supported by the Key Program of the National Natural Science Foundation of China(Nos.20836009 and 20873172)
文摘Detailed time-and-space-averaged structure of MgSO4 in the concentrated aqueous solutions was investigated via X-ray diffraction with an X’pert Pro θ-θ diffractometer at 298 K, yielding structural function and radial distribution function（RDF）. The developed KURVLR program was employed for the theoretical investigation in consideration of the ionic hydration and ion association. Multi-peaks Gaussian fitting method was applied to deconvolving the overlapping bands of Differential radial distribution function（DRDF）. The calculation of the geometric model shows that octahedrally six-coordinated Mg（H2O）62＋, with an Mg2＋…OW bond length of 0.201 nm dominates in the solutions. There exists contact ion-pair（CIP） in the more concentrated solution（1：18, H2O/salt molar ratio） with a coordination number of 0.8 and a characteristic Mg…S distance of 0.340 nm. The result indicates the hydrated SO42– ion happens in the solution. The S…OW bond distance was determined to be 0.382 nm with a coordination number of 13. The fraction of CIP increases significantly with the increasing concentration. The symmetry of the hydration structure of sulfate ion is lowered by forming complex with magnesium ion.
基金This paper was suported by the National Natural Science Foundation of China.
文摘In situ x-ray diffraction electrochemical method is used to study the activation of silver electrode in KCl solution and UPD lead on silver electrode surface. We found that the activation makes the silver crystal thicker in (111), and the arrangement of water molecules on the silver electrode surface with UPD lead is partially ordered.
基金the National Natural Science Foundation of China(Grant No.69825107,NSFC-RGC Joint program:NSFC5001161953 and N_HKU028/00)
文摘In this paper we propose a new method for measuring the thickness of the GaN epilayer, by using the ratio of the integrated intensity of the GaN epilayer X-ray diffraction peaks to that of the sapphire substrate ones. This ratio shows a linear dependence on the GaN epilayer thickness up to 2 μm. The new method is more accurate and convenient than those of using the relationship between the integrated intensity of GaN epilayer diffraction peaks and the GaN thickness. Besides, it can eliminate the absorption effect of the GaN epilayer.
基金Supported by National Natural Science Foundation of China (10774065)Science Foundation for Excellent Youth Scholars of Huaiyin Normal University (08QNZCK 005)
文摘SrTiO3 thin films are epitaxially grown on DyScO3, LaAlO3 substrates with/without buffer layers of DyScO3 and SrRuO3 using laser-MBE. X-ray diffraction methods, such as high resolution X-ray diffraction, grazing incident X-ray diffraction, and reciprocal space mapping are used to investigate the lattice structure, dislocation density, in-plane lattice strain distribution along film thickness. From the measurement results, the effects of substrate on film lattice quality and microstructure are discussed.
文摘A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus.The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.
文摘A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus,The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.
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 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Project supported by the National Key Research and Development Program of China (Grant Nos.2022YFF0709103,2022YFA1603601,2021YFF0601203,and 2021YFA1600703)the National Natural Science Foundation of China (Grant No.81430087)the Shanghai Pilot Program for Basic Research-Chinese Academy of Sciences,Shanghai Branch (Grant No.JCYJ-SHFY-2021-010)。
文摘Beam splitting is one of the main approaches to achieving x-ray ghost imaging, and the intensity correlation between diffraction beam and transmission beam will directly affect the imaging quality. In this paper, we investigate the intensity correlation between the split x-ray beams by Laue diffraction of stress-free crystal. The analysis based on the dynamical theory of x-ray diffraction indicates that the spatial resolution of diffraction image and transmission image are reduced due to the position shift of the exit beam. In the experimental setup, a stress-free crystal with a thickness of hundredmicrometers-level is used for beam splitting. The crystal is in a non-dispersive configuration equipped with a double-crystal monochromator to ensure that the dimension of the diffraction beam and transmission beam are consistent. A correlation coefficient of 0.92 is achieved experimentally and the high signal-to-noise ratio of the x-ray ghost imaging is anticipated.Results of this paper demonstrate that the developed beam splitter of Laue crystal has the potential in the efficient data acquisition of x-ray ghost imaging.
基金supported by the National Natural Science Foundation of China(Grant Nos.12304033,12072328,and 11991073).
文摘Phase transition of polycrystalline iron compressed along the Hugoniot is studied by combining laser-driven shock with in situ x-ray diffraction technique.It is suggested that polycrystalline iron changes from an initial body-centered cubic structure to a hexagonal close-packed structure with increasing pressure(i.e.,a phase transition fromαtoε).The relationship between density and pressure for polycrystalline iron obtained from the present experiments is found to be in good agreement with the gas-gun Hugoniot data.Our results show that experiments with samples at lower temperatures under static loading,such as in a diamond anvil cell,lead to higher densities measured than those found under dynamic loading.This means that extrapolating results of static experiments may not predict the dynamic responses of materials accurately.In addition,neither the face-centered cubic structure seen in previous molecular-dynamics simulations or twophase coexistence are found within our experimental pressure range.
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.
