Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs. Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crys...Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs. Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crystal form. Unfortunately, it is usually found in a polymorphic mixture with form B. In this study, pure crystal forms of A and B were prepared and characterized by X-ray powder diffraction （XRPD）, Fourier transform infrared spectroscopy （FT-IR） and thermal analysis. An XRPD-based method for the quantitative determination of the amount of the flupirtine maleate polymorphs form A and form B was also established through a systematic optimization of instrumental parameters. The results of the analytical methodology validation showed that the XPRD method had a broad quantitative range of 0- 100% （w/w）, good linear relationship, with R2= 0.999, excellent repeatability and precision and low limits of detection （LoD） of 0.15% （w/w） and quantification （LoQ） of 0.5% （w/w）. The results also showed that the single-peak method was not as good as the whole pattern in reducing the influence of the preferred orientation, but this can be compensated for by a systematic optimization of instrumental parameters and validating the analytical methodology to reduce errors and obtain a good, repeatable, sensitive, and accurate method. This XRPD method can be used to analyze mixtures of flupirtine maleate polymorphs （forms A and B） quantitatively and control the quality of the bulk drug.展开更多
Employing experimental equipment and techniques,such as electron backscatter diffraction,transmission Kikuchi diffraction,and transmission electron microscopy,the microstructure,phase structure,and orientation relatio...Employing experimental equipment and techniques,such as electron backscatter diffraction,transmission Kikuchi diffraction,and transmission electron microscopy,the microstructure,phase structure,and orientation relationships of 0.6μm electroplated nickel(Ni)steel following annealing at 580-650℃for 15-30 hours were investigated.A comprehensive analysis was conducted to gain insights into the complex changes in the material's properties due to the annealing process.The results reveal that prolonged annealing led to considerable long-range diffusion of surface Ni atoms into the substrate of the 0.6μm Ni-plated steel.This diffusion process resulted in the formation of an alloy diffusion layer,approximately 4μm in thickness,which altered the material's microstructural characteristics.The extent of diffusion and its effect on the microstructure and structure were meticulously quantified.At the annealing temperature,the diffused Ni in the substrate,acting as an austenite-stabilizing element,expanded the austenite phase region.The alloy layer at this temperature predominantly consisted of the face-centered cubic(FCC)-structuredγ(Fe,Ni)solid solution.Upon cooling to room temperature,the alloy diffusion layer evolved into a dual-layer composite structure.The upper layer mainly comprised the FCC-structuredγ(Fe,Ni)solid solution,interspersed with a minor FCC compound superstructure phase.The lower layer underwent a diffusionless phase transformation during cooling,which led to the formation of the body-centered tetragonal/body-centered cubic-structured martensite.This phase,which is known for its high hardness and numerous variants,maintained the classic Kurdjumov-Sachs orientation relationship with the upper FCC parent phase,and it satisfied the close-packed plane{111}γ//{110}α′and close-packed direction<110>γ//<111>α′.A detailed analysis of the different phases within the alloy layer and their phase transitions was presented,offering an in-depth understanding of the material's characteristics.展开更多
The worn scars on Alloy 690 after the fretting corrosion testing in simulated pressurized water reactor(PWR)secondary water have been comprehensively analyzed by scanning transmission electron microscopy(STEM)and tran...The worn scars on Alloy 690 after the fretting corrosion testing in simulated pressurized water reactor(PWR)secondary water have been comprehensively analyzed by scanning transmission electron microscopy(STEM)and transmission Kikuchi diffraction(TKD).The high-quality characterization results experimentally show that the fretting wear accelerates the corrosion of Alloy 690 in two approaches.The first one is to break the integrity of the oxide scale by introducing cavities at the oxide grain boundaries.The second one is to alter the microstructure of the underneath matrix,forming a nano-grained matrix layer.The increased grain boundary density in this layer can accelerate the consumption of Cr in the near-surface matrix.The loss of oxide scale integrity and the accelerated Cr consumption are believed to contribute to the deteriorated corrosion resistance of Alloy 690 during the fretting corrosion process.展开更多
Using high-resolution transmission Kikuchi diffraction(TKD)and transmission electron microscopy(TEM),we examined the hierarchical clusters that form in situ in the heat-affected zone(HAZ),which are com-monly referred ...Using high-resolution transmission Kikuchi diffraction(TKD)and transmission electron microscopy(TEM),we examined the hierarchical clusters that form in situ in the heat-affected zone(HAZ),which are com-monly referred to as“ghost”structures,of bimodal titanium alloy Ti-5Al-2Sn-2Zr-4Mo-4Cr(wt%,TC17).The ghost structures are enriched with Al elements but poor in Mo and Cr compared to the surroundingβmatrix.TKD results show that the ghost structure in middle-HAZ mainly consists ofα_(L)laths with a high-angle grain boundary,which exhibits the classic Burgers orientation relationship(BOR)with the host matrix,while it encircles theα_(P)grains in far-HAZ.And the ghost structure is evidenced to form via in-complete martensitic transformation.TEM results further confirm that the ghost structure is composed ofαL and tinyβ_(L)laths with BOR,with the former being enriched with Al and poor with Cr and Mo,while the latter is the opposite.Interestingly,twoα_(L)variant clusters with a check-mark morphology are fre-quently observed viewed along[0001]_(αL)//[110]_(βL)directions,which are dominated by the crystallographic and geometrical relationships betweenαandβphases.Based on the microstructural characterization,it is hypothesized that the ghost structure is transformed from the initialα_(P)phase,due to the coupling ef-fect of high thermal stress(which induces the formation of a large number of dislocations)and element diffusion caused by sudden temperature increase and plunge cooling in the HAZ during the welding pro-cess.展开更多
Sodium-oxygen batteries(SOBs) have the potential to provide energy densities higher than the state-ofthe-art Li-ion batteries. However, controlling the formation of sodium superoxide(NaO_(2)) as the sole discharge pro...Sodium-oxygen batteries(SOBs) have the potential to provide energy densities higher than the state-ofthe-art Li-ion batteries. However, controlling the formation of sodium superoxide(NaO_(2)) as the sole discharge product on the cathode side is crucial to achieve durable and efficient SOBs. In this work, the discharge efficiency of two graphene-based cathodes was evaluated and compared with that of a commercial gas diffusion layer. The discharge products formed at the surface of these cathodes in a glyme-based electrolyte were carefully studied using a range of characterization techniques. NaO_(2) was detected as the main discharge product regardless of the specific cathode material while small amounts of Na_(2)O_(2).2H_(2)O and carbonate-like side-products were detected by X-ray diffraction as well as by Raman and infrared spectroscopies. This work leverages the use of X-ray diffraction to determine the actual yield of NaO_(2)which is usually overlooked in this type of batteries. Thus, the proper quantification of the superoxide formed on the cathode surface is widely underestimated;even though is crucial for determining the efficiency of the battery while eliminating the parasitic chemistry in SOBs. Here, we develop an ex-situ analysis method to determine the amount of NaO_(2) generated upon discharge in SOBs by transmission X-ray diffraction and quantitative Rietveld analysis. This work unveils that the yield of NaO_(2) depends on the depth of discharge where high capacities lead to very low discharge efficiency, regardless of the used cathode. We anticipate that the methodology developed herein will provide a convenient diagnosis tool in future efforts to optimize the performance of the different cell components in SOBs.展开更多
Superparamagnetic monodisperse Mg0.8Mn0.2Fe2O4 nanoparticles have been successfully synthesized in liquid polyol at elevated temperature of 200 °C. Diethylene glycol（DEG） used here plays dual role in synthesis ...Superparamagnetic monodisperse Mg0.8Mn0.2Fe2O4 nanoparticles have been successfully synthesized in liquid polyol at elevated temperature of 200 °C. Diethylene glycol（DEG） used here plays dual role in synthesis as it acts as reducing agent and alternatively coats the surface of nanoparticles while synthesis and thereby maintaining uniform size and dispersibility. Powder X-ray diffraction（XRD） and magnetic measurements showed that the sample is cubic spinel and superparamagnetic at room temperature. Raman spectra confirmed the formation of the Mg0.8Mn0.2Fe2O4 nanoparticles.The nanoparticles exhibit very good stability in water due to in situ coating with DEG molecules.展开更多
Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ phosphors were synthesized by solid-state reaction technique. The crystalline phase and luminescence performances of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ were observe...Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ phosphors were synthesized by solid-state reaction technique. The crystalline phase and luminescence performances of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ were observed by X-ray powder diffractometer（XRD）, transmission electron microscope（TEM）, photoluminescence spectrometer and brightness meter, respectively. The addition of Ag~＋ can diminish in the crystal particle sizes of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）. Because Ag＋ can reduce the concentration of the undesirable defects in the phosphor, luminescence intensity of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ is 2.3 times as high as that of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）at the same preparation condition. The effect of Ag＋ on the persistent afterglow properties is to deepen the energy storage traps and enhance the energy transfer efficiency from Ca_（0.9）Mg_（0.1）TiO_3 to Pr^（3＋）. The persistent afterglow properties of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ are better than those of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋） at the same preparation condition. In conclusion,Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ phosphor with molar ratio of Ag~＋to Pr^（3＋） 3：1 obtained at 900 ℃ for 4 h exhibits the optimal photoluminescence performances.展开更多
Amorphous structure generated by high-energy ball miller(BM)is often used as a precursor for generating nanocomposites through controlled devitrification.The amorphous forming composition range of ternary Al-Cu-Zr sys...Amorphous structure generated by high-energy ball miller(BM)is often used as a precursor for generating nanocomposites through controlled devitrification.The amorphous forming composition range of ternary Al-Cu-Zr system was calculated using the extended Miedema’s semiempirical model.Eleven compositions of Al-Cu-Zr system showed a wide range of negative enthalpy of mixing(-ΔH^(mix))and amorphization(-ΔH^(amor))among the constituent elements was selected for synthesis by BM.They yielded either nanocomposites of partial amorphous and crystalline structure or no amorphous phase at all in the as-milled condition.The Al_(88)Cu_(6)Zr_(6) alloy with relatively small negativeΔH^(mix)(-0.4 kJ/mol)andΔH^(amor)(-14.8 kJ/mol)became completely amorphous after 120 h of milling.展开更多
The growth mechanisms of high temperature Yttrium- and Bismuth-based-superconductors were investigated at nanoscale. We started with studying the growth relationships among the three phases of Bi-2201, Bi-2212, and Bi...The growth mechanisms of high temperature Yttrium- and Bismuth-based-superconductors were investigated at nanoscale. We started with studying the growth relationships among the three phases of Bi-2201, Bi-2212, and Bi-2233, and then extended to another growth mechanism of Bi-2223 and the growth of yttrium-based high-temperature nanosuperconductors （nano-YBCO）. A time dependence of growth experiment was performed. In this experiment, the Bi-based superconductors grew within different sintering periods, and its three phases were determined by X-ray diffraction. And then, a time dependence of growth model was suggested to explain the experimental facts. With this model, governing equations were derived to quantitatively describe the growth and decomposition mechanisms during sintering period. The results calculated from the derived equations were well in agreement with the experimental data. We also suggested an alternative growth mechanism for the Bi-2223 phase, which was supported by an observation of transmission electron microscopy （TEM）. The nano-YBCO also grew, and their orthorhombic crystal structures were determined by the TEM. The superconducting properties of Bi-2223 were investigated by the measurements of ac magnetic susceptibility. It is expected that the derived equations will fit the alternative experimental growth mechanism of the Bi-2223 phase and the nano-YBCO growth mechanism, too.展开更多
Medium-entropy alloys(MEAs)have garnered significant interest due to their unique mechanical prop-erties,but phase instabilities such as the formation of brittle sigma(σ)phase during annealing pose challenges to thei...Medium-entropy alloys(MEAs)have garnered significant interest due to their unique mechanical prop-erties,but phase instabilities such as the formation of brittle sigma(σ)phase during annealing pose challenges to their practical application.This study investigates the microstructural evolution and me-chanical behavior of an 80%cold-rolled Fe_(45)Co_(35)Cr_(10)V_(10)MEA that was isochronally annealed between 100℃ and 900℃ for 300 s and characterized using hardness indentations,in-situ X-ray diffraction,and thermodynamic calculations,with high-resolution electron microscopy detailing microstructural evo-lution at 625℃,675℃,and 725℃.The results show increases in Vickers hardness between 500℃ and 625℃,attributed to the nucleation of a Cr-and V-rich sigma(σ)phase,primarily at the bcc grain boundaries.Beyond 625℃,the hardness decreased due toσ-phase dissolution,recovery of bcc and fcc phases,bcc→fcc phase reversion,and recrystallization of the reverted fcc phase.Scanning-transmission electron microscopy and transmission Kikuchi diffraction revealed a Kurdjumov-Sachs orientation rela-tionship(OR)at 675℃ and a near Nishiyama-Wassermann OR at 725℃ for bcc-fcc interfaces,whereas bcc-σand fcc-σinterfaces showed no dominant OR.In addition toσphase,two types of bcc phase were identified at 625℃.Type 1 bcc initially retained a near-nominal composition and a disordered crystal structure from deformation-induced bcc martensite but gradually became Fe-enriched and Cr-and V-depleted up to 725℃.In contrast,Type 2 bcc phase was Fe-depleted and Co-enriched at 625℃ but dis-appeared at 675℃,coinciding with the onset of bcc→fcc phase reversion.This phase also exhibited B2-like chemical short-range ordering,with alternating FeCo-rich and CrV-rich domains.This study provides insights into the complex phase transformation occurring between 500℃ and 725℃ in a Fe_(45)Co_(35)Cr_(10)V_(10)MEA,which can be leveraged to design alloys with optimized mechanical properties for practical appli-cations.展开更多
基金supported by the Major Program of Ministry of Science and Technology of China(No:2015ZX09J15104-003002)
文摘Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs. Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crystal form. Unfortunately, it is usually found in a polymorphic mixture with form B. In this study, pure crystal forms of A and B were prepared and characterized by X-ray powder diffraction （XRPD）, Fourier transform infrared spectroscopy （FT-IR） and thermal analysis. An XRPD-based method for the quantitative determination of the amount of the flupirtine maleate polymorphs form A and form B was also established through a systematic optimization of instrumental parameters. The results of the analytical methodology validation showed that the XPRD method had a broad quantitative range of 0- 100% （w/w）, good linear relationship, with R2= 0.999, excellent repeatability and precision and low limits of detection （LoD） of 0.15% （w/w） and quantification （LoQ） of 0.5% （w/w）. The results also showed that the single-peak method was not as good as the whole pattern in reducing the influence of the preferred orientation, but this can be compensated for by a systematic optimization of instrumental parameters and validating the analytical methodology to reduce errors and obtain a good, repeatable, sensitive, and accurate method. This XRPD method can be used to analyze mixtures of flupirtine maleate polymorphs （forms A and B） quantitatively and control the quality of the bulk drug.
文摘Employing experimental equipment and techniques,such as electron backscatter diffraction,transmission Kikuchi diffraction,and transmission electron microscopy,the microstructure,phase structure,and orientation relationships of 0.6μm electroplated nickel(Ni)steel following annealing at 580-650℃for 15-30 hours were investigated.A comprehensive analysis was conducted to gain insights into the complex changes in the material's properties due to the annealing process.The results reveal that prolonged annealing led to considerable long-range diffusion of surface Ni atoms into the substrate of the 0.6μm Ni-plated steel.This diffusion process resulted in the formation of an alloy diffusion layer,approximately 4μm in thickness,which altered the material's microstructural characteristics.The extent of diffusion and its effect on the microstructure and structure were meticulously quantified.At the annealing temperature,the diffused Ni in the substrate,acting as an austenite-stabilizing element,expanded the austenite phase region.The alloy layer at this temperature predominantly consisted of the face-centered cubic(FCC)-structuredγ(Fe,Ni)solid solution.Upon cooling to room temperature,the alloy diffusion layer evolved into a dual-layer composite structure.The upper layer mainly comprised the FCC-structuredγ(Fe,Ni)solid solution,interspersed with a minor FCC compound superstructure phase.The lower layer underwent a diffusionless phase transformation during cooling,which led to the formation of the body-centered tetragonal/body-centered cubic-structured martensite.This phase,which is known for its high hardness and numerous variants,maintained the classic Kurdjumov-Sachs orientation relationship with the upper FCC parent phase,and it satisfied the close-packed plane{111}γ//{110}α′and close-packed direction<110>γ//<111>α′.A detailed analysis of the different phases within the alloy layer and their phase transitions was presented,offering an in-depth understanding of the material's characteristics.
基金Shanghai Pujiang Program(No.21PJ1406400)is acknowledged for funding this research.
文摘The worn scars on Alloy 690 after the fretting corrosion testing in simulated pressurized water reactor(PWR)secondary water have been comprehensively analyzed by scanning transmission electron microscopy(STEM)and transmission Kikuchi diffraction(TKD).The high-quality characterization results experimentally show that the fretting wear accelerates the corrosion of Alloy 690 in two approaches.The first one is to break the integrity of the oxide scale by introducing cavities at the oxide grain boundaries.The second one is to alter the microstructure of the underneath matrix,forming a nano-grained matrix layer.The increased grain boundary density in this layer can accelerate the consumption of Cr in the near-surface matrix.The loss of oxide scale integrity and the accelerated Cr consumption are believed to contribute to the deteriorated corrosion resistance of Alloy 690 during the fretting corrosion process.
基金supported by the National Natural Science Foun-dation of China(Grant Nos.51871222 and 52171021)Japan Soci-ety for the Promotion of Science(No.P20737)Natural Science Foundation of Liaoning Province(No.2023-MS-018).
文摘Using high-resolution transmission Kikuchi diffraction(TKD)and transmission electron microscopy(TEM),we examined the hierarchical clusters that form in situ in the heat-affected zone(HAZ),which are com-monly referred to as“ghost”structures,of bimodal titanium alloy Ti-5Al-2Sn-2Zr-4Mo-4Cr(wt%,TC17).The ghost structures are enriched with Al elements but poor in Mo and Cr compared to the surroundingβmatrix.TKD results show that the ghost structure in middle-HAZ mainly consists ofα_(L)laths with a high-angle grain boundary,which exhibits the classic Burgers orientation relationship(BOR)with the host matrix,while it encircles theα_(P)grains in far-HAZ.And the ghost structure is evidenced to form via in-complete martensitic transformation.TEM results further confirm that the ghost structure is composed ofαL and tinyβ_(L)laths with BOR,with the former being enriched with Al and poor with Cr and Mo,while the latter is the opposite.Interestingly,twoα_(L)variant clusters with a check-mark morphology are fre-quently observed viewed along[0001]_(αL)//[110]_(βL)directions,which are dominated by the crystallographic and geometrical relationships betweenαandβphases.Based on the microstructural characterization,it is hypothesized that the ghost structure is transformed from the initialα_(P)phase,due to the coupling ef-fect of high thermal stress(which induces the formation of a large number of dislocations)and element diffusion caused by sudden temperature increase and plunge cooling in the HAZ during the welding pro-cess.
基金the European Union (Graphene Flagship-Core 3, Grant number 881603) for the financial support of this workfunding by the Spanish Ministerio de Ciencia,Innovación y Universidades (MICINN),Agencia Estatal de Investigación (AEI) and the European Regional Development Fund (ERDF) through project RTI2018-100832-B-I00financial support from Stand Up for Energy and the Swedish Energy Agency。
文摘Sodium-oxygen batteries(SOBs) have the potential to provide energy densities higher than the state-ofthe-art Li-ion batteries. However, controlling the formation of sodium superoxide(NaO_(2)) as the sole discharge product on the cathode side is crucial to achieve durable and efficient SOBs. In this work, the discharge efficiency of two graphene-based cathodes was evaluated and compared with that of a commercial gas diffusion layer. The discharge products formed at the surface of these cathodes in a glyme-based electrolyte were carefully studied using a range of characterization techniques. NaO_(2) was detected as the main discharge product regardless of the specific cathode material while small amounts of Na_(2)O_(2).2H_(2)O and carbonate-like side-products were detected by X-ray diffraction as well as by Raman and infrared spectroscopies. This work leverages the use of X-ray diffraction to determine the actual yield of NaO_(2)which is usually overlooked in this type of batteries. Thus, the proper quantification of the superoxide formed on the cathode surface is widely underestimated;even though is crucial for determining the efficiency of the battery while eliminating the parasitic chemistry in SOBs. Here, we develop an ex-situ analysis method to determine the amount of NaO_(2) generated upon discharge in SOBs by transmission X-ray diffraction and quantitative Rietveld analysis. This work unveils that the yield of NaO_(2) depends on the depth of discharge where high capacities lead to very low discharge efficiency, regardless of the used cathode. We anticipate that the methodology developed herein will provide a convenient diagnosis tool in future efforts to optimize the performance of the different cell components in SOBs.
基金the Council of Scientific and Industrial Research, India for the award of senior research fellowship (File. 09/1077/(0001)/ 2012/EMR-1)
文摘Superparamagnetic monodisperse Mg0.8Mn0.2Fe2O4 nanoparticles have been successfully synthesized in liquid polyol at elevated temperature of 200 °C. Diethylene glycol（DEG） used here plays dual role in synthesis as it acts as reducing agent and alternatively coats the surface of nanoparticles while synthesis and thereby maintaining uniform size and dispersibility. Powder X-ray diffraction（XRD） and magnetic measurements showed that the sample is cubic spinel and superparamagnetic at room temperature. Raman spectra confirmed the formation of the Mg0.8Mn0.2Fe2O4 nanoparticles.The nanoparticles exhibit very good stability in water due to in situ coating with DEG molecules.
基金Project supported by the Education Department of Yunnan,China(Grant No.2015Y103)
文摘Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ phosphors were synthesized by solid-state reaction technique. The crystalline phase and luminescence performances of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ were observed by X-ray powder diffractometer（XRD）, transmission electron microscope（TEM）, photoluminescence spectrometer and brightness meter, respectively. The addition of Ag~＋ can diminish in the crystal particle sizes of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）. Because Ag＋ can reduce the concentration of the undesirable defects in the phosphor, luminescence intensity of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ is 2.3 times as high as that of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）at the same preparation condition. The effect of Ag＋ on the persistent afterglow properties is to deepen the energy storage traps and enhance the energy transfer efficiency from Ca_（0.9）Mg_（0.1）TiO_3 to Pr^（3＋）. The persistent afterglow properties of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ are better than those of Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋） at the same preparation condition. In conclusion,Ca_（0.9）Mg_（0.1）TiO_3：Pr^（3＋）,Ag~＋ phosphor with molar ratio of Ag~＋to Pr^（3＋） 3：1 obtained at 900 ℃ for 4 h exhibits the optimal photoluminescence performances.
文摘Amorphous structure generated by high-energy ball miller(BM)is often used as a precursor for generating nanocomposites through controlled devitrification.The amorphous forming composition range of ternary Al-Cu-Zr system was calculated using the extended Miedema’s semiempirical model.Eleven compositions of Al-Cu-Zr system showed a wide range of negative enthalpy of mixing(-ΔH^(mix))and amorphization(-ΔH^(amor))among the constituent elements was selected for synthesis by BM.They yielded either nanocomposites of partial amorphous and crystalline structure or no amorphous phase at all in the as-milled condition.The Al_(88)Cu_(6)Zr_(6) alloy with relatively small negativeΔH^(mix)(-0.4 kJ/mol)andΔH^(amor)(-14.8 kJ/mol)became completely amorphous after 120 h of milling.
文摘The growth mechanisms of high temperature Yttrium- and Bismuth-based-superconductors were investigated at nanoscale. We started with studying the growth relationships among the three phases of Bi-2201, Bi-2212, and Bi-2233, and then extended to another growth mechanism of Bi-2223 and the growth of yttrium-based high-temperature nanosuperconductors （nano-YBCO）. A time dependence of growth experiment was performed. In this experiment, the Bi-based superconductors grew within different sintering periods, and its three phases were determined by X-ray diffraction. And then, a time dependence of growth model was suggested to explain the experimental facts. With this model, governing equations were derived to quantitatively describe the growth and decomposition mechanisms during sintering period. The results calculated from the derived equations were well in agreement with the experimental data. We also suggested an alternative growth mechanism for the Bi-2223 phase, which was supported by an observation of transmission electron microscopy （TEM）. The nano-YBCO also grew, and their orthorhombic crystal structures were determined by the TEM. The superconducting properties of Bi-2223 were investigated by the measurements of ac magnetic susceptibility. It is expected that the derived equations will fit the alternative experimental growth mechanism of the Bi-2223 phase and the nano-YBCO growth mechanism, too.
基金provided by the Nano and Material Technology Development Program(RS-2023-00281246)via the National Research Foundation of Korea,Ministry of Science and ICT,KoreaThe JEOL JSM-7001F,JEOL ARM 200F,and FEI Helios G3 CX FIB-SEM were funded by the Australian Research Council-Linkage,Infrastructure,Equipment and Facilities GrantsNos.LE0882613,LE120100104 andLE160100063,respectivelyThe Oxford Instruments 80 mm2 X-Max EDS detector and the JEOL JEM F200 were funded via the 2012 UOW Major Equipment Grant and 2019 UOW Equipment Replacement Grant schemes,respectively.
文摘Medium-entropy alloys(MEAs)have garnered significant interest due to their unique mechanical prop-erties,but phase instabilities such as the formation of brittle sigma(σ)phase during annealing pose challenges to their practical application.This study investigates the microstructural evolution and me-chanical behavior of an 80%cold-rolled Fe_(45)Co_(35)Cr_(10)V_(10)MEA that was isochronally annealed between 100℃ and 900℃ for 300 s and characterized using hardness indentations,in-situ X-ray diffraction,and thermodynamic calculations,with high-resolution electron microscopy detailing microstructural evo-lution at 625℃,675℃,and 725℃.The results show increases in Vickers hardness between 500℃ and 625℃,attributed to the nucleation of a Cr-and V-rich sigma(σ)phase,primarily at the bcc grain boundaries.Beyond 625℃,the hardness decreased due toσ-phase dissolution,recovery of bcc and fcc phases,bcc→fcc phase reversion,and recrystallization of the reverted fcc phase.Scanning-transmission electron microscopy and transmission Kikuchi diffraction revealed a Kurdjumov-Sachs orientation rela-tionship(OR)at 675℃ and a near Nishiyama-Wassermann OR at 725℃ for bcc-fcc interfaces,whereas bcc-σand fcc-σinterfaces showed no dominant OR.In addition toσphase,two types of bcc phase were identified at 625℃.Type 1 bcc initially retained a near-nominal composition and a disordered crystal structure from deformation-induced bcc martensite but gradually became Fe-enriched and Cr-and V-depleted up to 725℃.In contrast,Type 2 bcc phase was Fe-depleted and Co-enriched at 625℃ but dis-appeared at 675℃,coinciding with the onset of bcc→fcc phase reversion.This phase also exhibited B2-like chemical short-range ordering,with alternating FeCo-rich and CrV-rich domains.This study provides insights into the complex phase transformation occurring between 500℃ and 725℃ in a Fe_(45)Co_(35)Cr_(10)V_(10)MEA,which can be leveraged to design alloys with optimized mechanical properties for practical appli-cations.
