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A Novel High Temperature Apparatus for in situ Synchrotron X-ray Diffraction Studies of Molten Salt
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作者 CAO Hui-li GAO Mei +5 位作者 Andebet G.Tamirat ZHAO Hong-bin ZHOU Xing-tai HUANG Yu-ying LEI Qi WEN Wen 《分析测试学报》 CAS CSCD 北大核心 2024年第10期1608-1617,共10页
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
关键词 in-situ x-ray diffraction rotary micro-diffractometer rotary high-temperature apparatus molten salt
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Microstructural origins of high strength of Al-Si alloy manufactured by laser powder bed fusion:In-situ synchrotron radiation X-ray diffraction approach 被引量:1
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作者 Naoki Takata Mulin Liu +4 位作者 Masahiro Hirata Asuka Suzuki Makoto Kobashi Masaki Kato Hiroki Adachi 《Journal of Materials Science & Technology》 SCIE EI CAS CSCD 2024年第11期80-89,共10页
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
关键词 Laser powder bed fusion Aluminum alloys Microstructures x-ray diffraction(xrd) Strain hardening
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Crystallographic Characteristic of Intermetallic Compounds in Al-Si-Mg Casting Alloys Using Electron Backscatter Diffraction 被引量:2
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作者 ZOU Yongzhi XU Zhengbing +1 位作者 HE Juan ZENG Jianmin 《Chinese Journal of Mechanical Engineering》 SCIE EI CAS CSCD 2010年第3期305-311,共7页
The Al-Si-Mg alloy which can be strengthened by heat treatment is widely applied to the key components of aerospace and aeronautics. Iron-rich intermetallic compounds are well known to be strongly influential on mecha... The Al-Si-Mg alloy which can be strengthened by heat treatment is widely applied to the key components of aerospace and aeronautics. Iron-rich intermetallic compounds are well known to be strongly influential on mechanical properties in Al-Si-Mg alloys. But intermetallic compounds in cast Al-Si-Mg alloy intermetallics are often misidentified in previous metallurgical studies. It was described as many different compounds, such as AlFeSi, Al8Fe2Si, Al5(Fe, Mn)3Si2 and so on. For the purpose of solving this problem, the intermetallic compounds in cast Al-Si alloys containing 0.5% Mg were investigated in this study. The iron-rich compounds in Al-Si-Mg casting alloys were characterized by optical microscope(OM), scanning electron microscope(SEM), energy dispersive X-ray spectrometer(EDS), electron backscatter diffraction(EBSD) and X-ray powder diffraction(XRD). The electron backscatter diffraction patterns were used to assess the crystallographic characteristics of intermetallic compounds. The compound which contains Fe/Mg-rich particles with coarse morphologies was Al8FeMg3Si6 in the alloy by using EBSD. The compound belongs to hexagonal system, space group P6_2m, with the lattice parameter a=0.662 nm, c=0.792 nm. The β-phase is indexed as tetragonal Al3FeSi2, space group I4/mcm, a=0.607 nm and c=0.950 nm. The XRD data indicate that Al8FeMg3Si6 and Al3FeSi2 are present in the microstructure of Al-7Si-Mg alloy, which confirms the identification result of EBSD. The present study identified the iron-rich compound in Al-Si-Mg alloy, which provides a reliable method to identify the intermetallic compounds in short time in Al-Si-Mg alloy. Study results are helpful for identification of complex compounds in alloys. 展开更多
关键词 Al-Si-Mg alloys intermetallic compound electron backscatter diffraction(EBSD) x-ray powder diffractionxrd)
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In-situ X-ray computed tomography tensile tests and analysis of damage mechanism and mechanical properties in laser powder b e d fused Invar 36 alloy 被引量:1
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作者 Qidong Yang Shuo Yang +6 位作者 Shiyu Ma Junhan Zhou Ye Zhou Rongzheng Huang Kai Wei Zhaoliang Qu Xujing Yang 《Journal of Materials Science & Technology》 SCIE EI CAS CSCD 2024年第8期29-46,共18页
Laser powder bed fusion(LPBF)is a potential additive manufacturing process to manufacture Invar 36 alloy components with complicated geometry.Whereas it inevitably introduces specific microstructures and pore defects,... Laser powder bed fusion(LPBF)is a potential additive manufacturing process to manufacture Invar 36 alloy components with complicated geometry.Whereas it inevitably introduces specific microstructures and pore defects,which will further influence the mechanical properties.Hence,aiming at exploring the LPBF process-related microstructures and pore defects,and especially their influences on the damage mechanism and mechanical properties,Invar 36 alloy was manufactured by LPBF under designed different laser scanning speeds.The microstructure observations reveal that higher scanning speeds lead to equiaxed and short columnar grains with higher dislocation density,while lower scanning speeds result in elongated columnar grains with lower dislocation density.The pore defects analyzed by X-ray computed tomography(XCT)suggest that the high laser scanning speed gives rise to numerous lamellar and large lack-of-fusion(LOF)pores,and the excessively low laser scanning speed produces relatively small keyhole pores with high sphericity.Moreover,the insitu XCT tensile tests were originally performed to evaluate the damage evolution and failure mechanism.Specifically,high laser scanning speed causes brittle fracture due to the rapid growth and coalescence of initial lamellar LOF pores along the scan-ning direction.Low laser scanning speed induces ductile fracture originating from unstable depressions in the surfaces,while metallurgical and keyhole pores have little impact on damage evolution.Eventually,the process-structure-property correlation is established.The presence of high volume fraction of lamel-lar LOF pores,resulting from high scanning speed,leads to inferior yield strength and ductility.Besides,specimens without LOF pores exhibit larger grain sizes and lower dislocation density at decreased scanning speeds,slightly reducing yield strength while slightly enhancing ductility.This understanding lays the foundation for widespread applications of LPBF-processed Invar 36 alloy. 展开更多
关键词 Invar 36 alloy Laser powder bed fusion Microstructure Pore defects Mechanical property x-ray tomography in-situ tensile test
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MAX phase forming mechanism of M-Al-C(M=Ti,V,Cr)coatings:In-situ X-ray diffraction and first-principle calculations 被引量:1
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作者 Jianghuai Yuan Zhenyu Wang +5 位作者 Guanshui Ma Xiaojing Bai Yong Li Xiaoying Cheng Peiling Ke Aiying Wang 《Journal of Materials Science & Technology》 SCIE EI CAS CSCD 2023年第12期140-152,共13页
The interesting hybrid properties of ceramics and metals induced by unique nano-laminated structures make the M_(n+1)AX n(MAX)phase attractive as a potential protective coating for vital structural compo-nents in hars... The interesting hybrid properties of ceramics and metals induced by unique nano-laminated structures make the M_(n+1)AX n(MAX)phase attractive as a potential protective coating for vital structural compo-nents in harsh systems.However,an extremely narrow phase-forming region makes it difficult to prepare MAX phase coatings with high purity,which is required to obtain coatings with high-temperature anti-oxidation capabilities.This work describes the dependence of the phase evolution in deposited M-Al-C(M=Ti,V,Cr)coatings as a function on temperature using in-situ X-ray diffraction analysis.Compared to V_(2)AlC and Cr_(2)AlC MAX phase coatings,the Ti_(2)AlC coating displayed a higher phase-forming tempera-ture accompanied by a lack of any intermediate phases before the appearance of the Ti_(2)AlC MAX phase.The results of the first-principle calculations correlated with the experience in which Ti_(2)AlC exhibited the largest formation energy and density of states.The effect of the phase compositions of these three MAX phase coatings on mechanical properties were also investigated using ex-situ Vickers and nano-indenter tests,demonstrating the improved mechanical properties with good stability at high temperatures.These findings provide a deeper understanding of the phase-forming mechanism of MAX phase coatings to guide the preparation of high-purity MAX phase coatings and the optimization of MAX phase coatings with expected intermediate phases such as Cr_(2)C,V_(2)C etc.,as well as their application as protective coat-ings in temperature-related harsh environments. 展开更多
关键词 MAX phase coating Phase-formation mechanism in-situ x-ray diffraction First-principle calculations Mechanical properties
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Anomalous bond lengthening in compressed magnetic doped semiconductor Ba(Zn_(0.95)Mn_(0.05))_(2)As_(2)
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作者 Fei Sun Yi Peng +3 位作者 Guoqiang Zhao Xiancheng Wang Zheng Deng Changqing Jin 《Journal of Semiconductors》 EI CAS CSCD 2024年第4期36-41,共6页
Applying pressure has been evidenced as an effective method to control the properties of semiconductors,owing to its capability to modify the band configuration around Fermi energy.Correspondingly,structural evolution... Applying pressure has been evidenced as an effective method to control the properties of semiconductors,owing to its capability to modify the band configuration around Fermi energy.Correspondingly,structural evolutions under external pres-sures are required to analyze the mechanisms.Herein high-pressure structure of a magnetic doped semiconductor Ba(Zn_(0.95)Mn_(0.05))_(2)As_(2)is studied with combination of in-situ synchrotron X-ray diffractions and diamond anvil cells.The materials become ferromagnetic with Curie temperature of 105 K after further 20%K doping.The title material undergoes an isostruc-tural phase transition at around 19 GPa.Below the transition pressure,it is remarkable to find lengthening of Zn/Mn-As bond within Zn/MnAs layers,since chemical bonds are generally shortened with applying pressures.Accompanied with the bond stretch,interlayer As-As distances become shorter and the As-As dimers form after the phase transition.With further compres-sion,Zn/Mn-As bond becomes shortened due to the recovery of isotropic compression on the Zn/MnAs layers. 展开更多
关键词 magnetic semiconductor high-pressure in-situ x-ray diffraction phase transition
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Novel high-voltage cathode for aqueous zinc ion batteries:Porous K_(0.5)VOPO_(4)·1.5H_(2)O with reversible solid-solution intercalation and conversion storage mechanism
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作者 Liyu Wang Mingliang Zhao +9 位作者 Xiaoyu Zhang Menghua Wu Yu Zong Yu Chen Xinliang Huang Mingjie Xing Xin Ning Wen Wen Daming Zhu Xiaochuan Ren 《Journal of Energy Chemistry》 SCIE EI CAS CSCD 2024年第6期71-78,I0003,共9页
Cathode materials that possess high output voltage,as well as those that can be mass-produced using facile techniques,are crucial for the advancement of aqueous zinc-ion battery(ZIBs)applications,Herein,we present for... Cathode materials that possess high output voltage,as well as those that can be mass-produced using facile techniques,are crucial for the advancement of aqueous zinc-ion battery(ZIBs)applications,Herein,we present for the first time a new porous K_(0.5)VOPO_(4)·1.5H_(2)O polyanionic cathode(P-KIVP)with high output voltage(above 1.2 V)that can be manufactured at room temperature using straightforward coprecipitation and etching techniques.The P-KVP cathode experiences anisotropic crystal plane expansion via a sequential solid-solution intercalation and phase co nversion pathway throughout the Zn^(2+)storage process,as confirmed by in-situ synchrotron X-ray diffraction and ex-situ X-ray photoelectron spectroscopy.Similar to other layered vanadium-based polyanionic materials,the P-KVP cathode experiences a progressive decline in voltage during the cycle,which is demonstrated to be caused by the irreversible conversion into amorphous VO_(x).By introducing a new electrolyte containing Zn(OTF)_(2) to a mixed triethyl phosphate and water solution,it is possible to impede this irreversible conversion and obtain a high output voltage and longer cycle life by forming a P-rich cathode electrolyte interface layer.As a proof-of-concept,the flexible fiber-shaped ZIBs based on modified electrolyte woven into a fabric watch band can power an electronic watch,highlighting the application potential of P-KVP cathode. 展开更多
关键词 Aqueous zinc ion battery CATHODE Porous material High voltage platform in-situ synchrotron x-ray diffraction
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Preparation, Characterization of Superacid SO_4^(2-)/ZrO_2-SiO_2 and Its Activity on Catalytic Synthesis of Methyl p-Nitrobenzoate 被引量:2
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作者 王刚 TAO Liya +5 位作者 HOU Xin CAO Hi DONG Cheng NIE Wo XU Jun 张立庆 《Journal of Wuhan University of Technology(Materials Science)》 SCIE EI CAS 2014年第5期895-899,共5页
Solid superacid SO42-/ZrO2-SiO2 was prepared by dip-impregnation method, and its catalytic activity was tested with esterification of p-nitrobenzoic acid and methanol. The optimum conditions were also found, that is, ... Solid superacid SO42-/ZrO2-SiO2 was prepared by dip-impregnation method, and its catalytic activity was tested with esterification of p-nitrobenzoic acid and methanol. The optimum conditions were also found, that is, the molar ratio between silica and zirconia was 10:1, the calcination temperature was 550 ℃ and the soaked consistency of H2SO4 was 1.0 mol.L-1. Under the conditions that the ratio of methanol to aeid(mL/ g) was 12:1, the amount of catalyst was 0.5 g, the reaction time was 5 h and the stirring speed was 800 r.min-1, the yield of methyl p-nitrobenzoate could reach up to 90.5%. Then the characterizations of cataslyst, including the acidity and types of acidic centers, specific surface area and surface structure was respectively examined by Hammer indicator, in-situ pyridine IR, BET method, FT-IR(KBr), transmission electron microscope (TEM), and X-ray diffraction (XRD). The results showed that the catalyst SO42-/ZrO2-SiO2 was superacid with high specific surface area due to Ho〈-12.70. It contained acidic sites of Lewis and BrФnsted, and its surface structure changed after esterification. The zirconia crystal was mainly tetragonal and silica crystal was not found. 展开更多
关键词 solid superacid methyl p-nitrobenzoate in-situ pyridine IR x-ray diffraction
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Plasma assisted synthesis of LiNi_(0.6)Co_(0.2)Mn_(0.2)O_(2) cathode materials with good cyclic stability at subzero temperatures 被引量:2
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作者 Fanbo Meng Renzong Hu +3 位作者 Zhiwei Chen Liang Tan Xuexia Lan Bin Yuan 《Journal of Energy Chemistry》 SCIE EI CAS CSCD 2021年第5期46-55,共10页
Layered Ni-rich cathode materials,LiNi_(0.6)Co_(0.2)Mn_(0.2)O_(2)(NCM622),are synthesized via solid reaction assisted with a plasma milling pretreatment,which is resulted in lowering sintering temperatures for solid p... Layered Ni-rich cathode materials,LiNi_(0.6)Co_(0.2)Mn_(0.2)O_(2)(NCM622),are synthesized via solid reaction assisted with a plasma milling pretreatment,which is resulted in lowering sintering temperatures for solid precursors.The plasma milling pretreated NCM622 cathode material sintered at 780℃(named as PM-780)demonstrates good cycling stability at both room and subzero temperatures.Specifically,the PM-780 cathode delivers an initial discharge capacity of 171.2 mAh g^(-1) and a high capacity retention of 99.7%after 300 cycles with current rate of 90 mA g^(-1) at 30℃,while stable capacities of 120.3 and 94.0 m Ah g^(-1) can be remained at-10℃and-20℃in propylene carbonate contained electrolyte,respectively.In-situ XRD together with XPS and SEM reveal that the NCM622 cycled at-10℃presented better structural stability and more intact interface than that of cathodes cycled at 30℃.It is also found that subzero temperatures only limit the discharge potential of NCM622 without destroying its structure during cycling since it still exhibits high discharge capacity at 30℃after cycled at subzero temperatures.This work may expand the knowledge about the low-temperature characteristics of layered cathode materials for Li-ion batteries and lay the foundation for its further applications. 展开更多
关键词 Ni-rich cathode materials Solid reaction Plasma milling Subzero temperature in-situ x-ray diffraction
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Modulation of lattice oxygen boosts the electrochemical activity and stability of Co-free Li-rich cathodes 被引量:1
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作者 Gui-Jing Xu Wang Ke +5 位作者 Fu-Da Yu Jie Feng Yun-Shan Jiang Lan-Fang Que Lei Zhao Zhen-Bo Wang 《Journal of Energy Chemistry》 SCIE EI CAS CSCD 2022年第12期117-126,I0004,共11页
Co-free Li-rich layered oxide cathodes have drawn much attention owing to their low cost and high energy density.Nevertheless,anion oxidation of oxygen leads to oxygen peroxidation during the first charging process,wh... Co-free Li-rich layered oxide cathodes have drawn much attention owing to their low cost and high energy density.Nevertheless,anion oxidation of oxygen leads to oxygen peroxidation during the first charging process,which leads to co-migration of transition metal ions and oxygen vacancies,causing structural instability.In this work,we propose a pre-activation strategy driven by chemical impregnation to modulate the chemical state of surface lattice oxygen,thus regulating the structural and electrochemical properties of the cathodes.In-situ X-ray diffraction confirms that materials based on activated oxygen configuration have higher structural stability.More importantly,this novel efficient strategy endows the cathodes having a lower surface charge transfer barrier and higher Li+transfer kinetics characteristic and ameliorates its inherent issues.The optimized cathode exhibits excellent electrochemical performance:after 300 cycles,high capacity(from 238 m Ah g^(-1)to 193 m Ah g^(-1)at 1 C)and low voltage attenuation(168 mV)are obtained.Overall,this modulated surface lattice oxygen strategy improves the electrochemical activity and structural stability,providing an innovative idea to obtain high-capacity Co-free Li-rich cathodes for next-generation Li-ion batteries. 展开更多
关键词 PRE-ACTIVATION Modulation of lattice oxygen in-situ x-ray diffraction Structure stability Co-free Li-rich cathodes
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Revealing structure behavior behind the piezoelectric performance of prototype lead-free Bi_(0.5)Na_(0.5)TiO_(3)-BaTiO_(3) under in-situ electric field 被引量:1
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作者 Huajie Luo Shiyu Tang +7 位作者 Hui Liu Zheng Sun Baitao Gao Yang Ren He Qi Shiqing Deng Houbing Huang Jun Chen 《Journal of Materiomics》 SCIE 2022年第6期1104-1112,共9页
Bi_(0.5)Na_(0.5)TiO_(3)-BaTiO_(3)(BNT-100xBT)ceramics are promising candidates for piezoelectric applications.The correlation between their structure and piezoelectric properties has attracted considerable interest.He... Bi_(0.5)Na_(0.5)TiO_(3)-BaTiO_(3)(BNT-100xBT)ceramics are promising candidates for piezoelectric applications.The correlation between their structure and piezoelectric properties has attracted considerable interest.Herein,the structures of 6BT and 7BT with distinct piezoelectricity are investigated via in-situ synchrotron X-ray diffraction and transmission electron microscopy.It is found that although both compositions present morphotropic phase boundary(MPB)features with coexisting R3c and P4bm phases,their refined structures are significantly different.6BT is composed of the R3c phase with a small P4bm fraction after electrical poling,while 7BT presents comparable fractions of the two phases.Less pronounced structure distortion and oxygen octahedral tilting occur in 7BT,which favor the phase transformation,resulting in an enhanced piezoelectricity.This enhancement driven by structural flexibility is elucidated by phenomenological analysis.These results demonstrate that the design of high piezoelectricity at MPBs should consider not only the phase-coexisting states but also the refined crystal structure. 展开更多
关键词 in-situ synchrotron x-ray diffraction Piezoelectric properties Crystal structure
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Thermal and Structural Analyses of PMMA/TiO<sub>2</sub>Nanoparticles Composites 被引量:2
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作者 Nabawia A. El-Zaher Mohamed S. Melegy Osiris W. Guirguis 《Natural Science》 2014年第11期859-870,共12页
In the present work, composites of poly (methyl methacrylate)/titanium oxide nanoparticles (100/0, 97.5/2.5, 95/5, 92.5/7.5, 90/10 and 0/100 wt/wt%)were prepared to be used as bioequivalent materials according to thei... In the present work, composites of poly (methyl methacrylate)/titanium oxide nanoparticles (100/0, 97.5/2.5, 95/5, 92.5/7.5, 90/10 and 0/100 wt/wt%)were prepared to be used as bioequivalent materials according to their importance broad practical and medical applications. Thermal properties as well as X-ray diffraction analyses were employed to characterize the structure properties of such composite. The obtained results showed variations in the glass transition temperature (Tg), the melting temperature (Tm), shape and area of thermal peaks which were attributed to the different degrees of crystallinity and the existence of interactions between PMMA and TiO2 nanoparticle molecules. The XRD patterns showed sharpening of peaks at different concentrations of nano-TiO2 powder with PMMA. This indicated changes in the crystallinity/amorphosity ratio, and also suggested that the miscibility between the amorphous components of homo- polymers PMMA and nano-TiO2 powder is possible.The results showed that nano-TiO2 powder mix with PMMA can improve the thermal stability of the homo-polymer under investigation, lead- ing to interesting technological applications. 展开更多
关键词 Poly(methyl methacrylate) Nano-Titanium Dioxide powder PMMA/TiO2 Nanoparticle COMPOSITES Differential Scanning Calorimetry (DSC) THERMOGRAVIMETRIC Analysis (TGA) x-ray diffraction (xrd)
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Impact of Annealing Treatment on the Behaviour of Titanium Dioxide Nanotube Layers 被引量:1
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作者 Marie Siampiringue Christophe Massard +3 位作者 Eric Caudron Yves Sibaud Mohammed Sarakha Komla Oscar Awitor 《Journal of Biomaterials and Nanobiotechnology》 2016年第3期142-153,共13页
In this work, we study the influence of the annealing treatment on the behaviour of titanium dioxide nanotube layers. The heat treatment protocol is actually the key parameter to induce stable oxide layers and needs t... In this work, we study the influence of the annealing treatment on the behaviour of titanium dioxide nanotube layers. The heat treatment protocol is actually the key parameter to induce stable oxide layers and needs to be better understood. Nanotube layers were prepared by electrochemical anodization of Ti foil in 0.4 wt% hydrofluoric acid solution during 20 minutes and then annealed in air atmosphere. In-situ X-ray diffraction analysis, coupled with thermogravimetry, gives us an inside on the oxidation behaviour of titanium dioxide nanotube layers compared to bulk reference samples. Structural studies were performed at 700°C for 12 h in order to follow the time consequences on the oxidation of the material, in sufficient stability conditions. In-situ XRD brought to light that the amorphous oxide layer induced by anodization is responsible for the simultaneous growths of anatase and rutile phase during the first 30 minutes of annealing while the bulk sample oxidation leads to the nucleation of a small amount of anatase TiO<sub>2</sub>. The initial amorphous oxide layer created by anodization is also responsible for the delay in crystallization compared to the bulk sample. Thermogravimetric analysis exhibits parabolic shape of the mass gain for both anodized and bulk sample;this kinetics is caused by the formation of a rutile external protective layer, as depicted by the associated in-situ XRD diffractograms. We recorded that titanium dioxide nanotube layers exhibit a lower mean mass gain than the bulk, because of the presence of an initial amorphous oxide layer on anodized samples. In-situ XRD results also provide accurate information concerning the sub-layers behavior during the annealing treatment for the bulk and nanostructured layer. Anatase crystallites are mainly localized at the interface oxide layer-metal and the rutile is at the external interface. Sample surface topography was characterized using scanning electron microscopy (SEM). As a probe of the photoactivity of the annealed TiO<sub>2</sub> nanotube layers, degradation of an acid orange 7 (AO7) dye solution and 4-chlorophenol under UV irradiation (at 365 nm) were performed. Such titanium dioxide nanotube layers show an efficient photocatalytic activity and the analytical results confirm the degradation mechanism of the 4-chlorophenol reported elsewhere. 展开更多
关键词 Titanium Dioxide Nanotubes in-situ x-ray diffraction Annealing Treatment PHOTO-DEGRADATION
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The highly selective catalytic hydrogenation of CO_(2)to CO over transition metal nitrides
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作者 Yichao Wu Zhiwei Xie +6 位作者 Xiaofeng Gao Xian Zhou Yangzhi Xu Shurui Fan Siyu Yao Xiaonian Li Lili Lin 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2022年第3期248-254,共7页
Three transition metal-like facet centered cubic structured transition metal nitrides,γ-Mo_(2)N,β-W_(2)N andδ-NbN,are synthesized and applied in the reaction of CO_(2)hydrogenation to CO.Among the three nitride cat... Three transition metal-like facet centered cubic structured transition metal nitrides,γ-Mo_(2)N,β-W_(2)N andδ-NbN,are synthesized and applied in the reaction of CO_(2)hydrogenation to CO.Among the three nitride catalysts,theγ-Mo_(2)N exhibits superior activity to target product CO,which is 4.6 and 76 times higher than the other two counterparts ofβ-W_(2)N andδ-NbN at 600℃,respectively.Additionally,γ-Mo_(2)N exhibits excellent stability on both cyclic heating-cooling and high space velocity steady state operation.The deactivation degree of cyclic heating-cooling evaluation after 5 cycles and long-term stability performance at 773 and 873 K in 50 h are all less than 10%.In-situ XRD and kinetic studies suggest that theγ-Mo_(2)N itself is able to activate both of the reactants CO_(2)and H_(2).Below 400℃,the reaction mainly occurs at the surface ofγ-Mo_(2)N catalyst.CO_(2)and H_(2)competitively adsorbe on the surface of catalyst and CO_(2)is the relatively stronger surface adsorbate.At a higher temperature,the interstitial vacancies of theγ-Mo_(2)N can be reversibly filled with the oxygen from CO_(2)dissociation.Both of the surface and bulk phase sites ofγ-Mo_(2)N participate in the high temperature CO_(2)hydrogenation pathway. 展开更多
关键词 Carbon dioxide Chemical reaction CATALYSIS Reverse water gas shift(RWGS)reaction Transition metal nitride in-situ x-ray diffraction characterization
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Evaluation of Characteristics of Interfacial Phases Produced in Al/Ni<sub>3</sub>Al Composite during Manufacturing
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作者 Seyed Abdolkarim Sajjadi Maryam Abbasi Mazyar Azadbeh 《Materials Sciences and Applications》 2011年第9期1340-1348,共9页
Metal matrix composites (MMCs) are currently being investigated because of their superior properties. The properties are mainly attributed to the efficiency of the load transfer from the matrix to the reinforcements t... Metal matrix composites (MMCs) are currently being investigated because of their superior properties. The properties are mainly attributed to the efficiency of the load transfer from the matrix to the reinforcements through the matrix-reinforcement interface. The aim of this study is to investigate the effect of manufacturing parameters on the microstructure and morphology of the interface and the aluminide phases formed at the matrix-reinforcement interfaces. The parameters are: milling time to fabricate Ni3Al, method of mixing of Ni3Al and Al powders, compaction pressure and sintering temperature. The composite studied in this research was Al/5 Vol% Ni3Al made from two different types of Ni3Al powders. The results showed that compacting and sintering at higher levels lead to the transformation of Ni3Al particles to thin layers of Al3Ni. It was also shown that the prolonged milling time to produceNi3Alreinforcements and the prolonged ball milling procedure for mixing the powders, both, promote the diffusion process at reinforcement/matrix interface. 展开更多
关键词 Metal-Matrix Composites (MMCs) Interface x-ray diffraction (xrd) powder Processing
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Formulation and Solid-State Characterisation of a Novel Benzanilide Co-crystal of the Anti-HIV Drug Efavirenz
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作者 Maryam Amra Jordaan Michael Shapi 《Journal of Pharmacy and Pharmacology》 2018年第3期274-285,共12页
HIV/AIDS has had a crippling socio-economic effect on developing countries in Africa. EFV (Efavirenz) is generally used to treat this pathology. However, its clinical efficacy is reduced by its limited water solubil... HIV/AIDS has had a crippling socio-economic effect on developing countries in Africa. EFV (Efavirenz) is generally used to treat this pathology. However, its clinical efficacy is reduced by its limited water solubility. Our recent efforts were to discover new multicomponent molecular crystals of EFV to further enhance the solubility of EFV, which has led to the formulation of a novel BZA (benzanilide) CC (co-crystal). The molecular complex was characterized by X-ray Powder Diffraction (XRD) and FTIR (Fourier transform infrared) spectroscopy. FTIR data showed a shift in the N-H stretch of the amide group of EFV from 3,312.39 cm^-1 to 3,299.71 cm^-1 and the C = O frequency from 1,749.70 cml to 1,739.87 cm^-1 suggesting that the N-H and C = O functionalities of EFV are participating in hydrogen bonding with the N-H and C = O moieties of BZA in the EFV-BZA complex, indicative of improved water solubility. Both the XRD patterns of BZA and EFV show characteristic peaks, however, in the XRD pattern of EFV-BZA CC, one unique peak appeared which is absent in both EFV and BZA at 30.8005° (100% intensity) suggesting the formation of a new solid phase. The results from this study are significant in understanding the complexity of these scarce EFV based CCs and can be used to advance the development of new solid-state structures with improved physicochemical properties. 展开更多
关键词 CCS EFV BZA x-ray powder diffraction xrd) FTIR.
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Design of advanced porous silver powder with high-sintering activity to improve silicon solar cells
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作者 Yongsheng Li Ziwei Chen +11 位作者 Rui Zhou Wenguang Zhao Mu Li Jun Chen Zhongyuan Huang Jian Liu Yuhang Li Maolin Yang Minghan Yu Dong Zhou Yuan Lin Feng Pan 《Nano Research》 SCIE EI CSCD 2024年第4期3189-3197,共9页
Silver(Ag)paste is widely used in semiconductor metallization,especially in silicon solar cells.Ag powder is the material with the highest proportion in Ag paste.The morphology and structure of Ag powder are crucial w... Silver(Ag)paste is widely used in semiconductor metallization,especially in silicon solar cells.Ag powder is the material with the highest proportion in Ag paste.The morphology and structure of Ag powder are crucial which determine its characteristics,especially for the sintering activity.In this work,a simple method was developed to synthesize a type of microcrystalline spherical Ag particles(SP-A)with internal pores and the structural changes and sintering behavior were thoroughly studied by combining ultra-small-angle X-ray scattering(USAXS),small-angle X-ray scattering(SAXS),in-situ heating X-ray diffraction(XRD),focused ion beam(FIB),and thermal analysis measurement.Due to the unique internal pores,the grain size of SP-A is smaller,and the coefficient of thermal expansion(CTE)is higher than that of traditional solid Ag particles.As a result,the sintering activity of SP-A is excellent,which can form a denser sintered body and form silver nanoparticles at the Ag–Si interface to improve silver silicon contact.Polycrystalline silicon solar cell built with SP-A obtained a low series resistance(Rs)and a high photoelectric conversion efficiency(PCE)of 19.26%.These fill a gap in Ag particle structure research,which is significant for the development of high-performance electronic Ag particles and efficient semiconductor devices. 展开更多
关键词 silver particles small angle x-ray scattering(SAXS) pore size distribution in-situ heating x-ray diffraction(xrd) SINTERING silicon solar cells
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Acceptor doping and actuation mechanisms in Sr-doped BiFeO_(3)-BaTiO_(3)ceramics 被引量:1
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作者 Ziqi Yang Yizhe Li +3 位作者 Bing Wang Juncheng Pan Annette K.Kleppe David A.Hall 《Journal of Materiomics》 SCIE CSCD 2024年第1期57-69,共13页
BiFeO_(3)-BaTiO_(3)(BF-BT)ceramics are important multiferroic materials,which are attracting significant attention for potential applications in high temperature lead-free piezoelectric transducers.In the present stud... BiFeO_(3)-BaTiO_(3)(BF-BT)ceramics are important multiferroic materials,which are attracting significant attention for potential applications in high temperature lead-free piezoelectric transducers.In the present study,the effects of Sr^(2+)as an acceptor dopant for Bi^(3+),in the range from 0 to 1.0%(in mole),on the structure and ferroelectric/piezoelectric properties of 0.7BiFeO_(3)-0.3BaTiO_(3)ceramics were evaluated.The use of a post-sintering Ar annealing process was found to be an effective approach to reduce electrical conductivity induced by the presence of electron holes associated with reoxidation during cooling.A low Sr dopant concentration(0.3%,in mole)yielded enhanced ferroelectric(P_(max)∼0.37 C/m^(2),P_(r)∼0.30 C/m^(2))and piezoelectric(d_(33)∼178 pC/N,k_(p)∼0.27)properties,whereas higher levels led to chemically heterogeneous core-shell structures and secondary phases with an associated decline in performance.The electric field-induced strain of the Sr-doped BF-BT ceramics was investigated using a combination of digital image correlation macroscopic strain measurements and in-situ synchrotron X-ray diffraction.Quantification of the intrinsic(lattice strain)and extrinsic(domain switching)contributions to the electric field induced strain indicated that the intrinsic contribution dominated during the poling process. 展开更多
关键词 Bismuth ferrite-barium titanate Acceptor doping ELECTROCERAMICS PIEZOELECTRICITY in-situ x-ray diffraction
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Rational synthesis of chitin-derived nitrogen-doped porous carbon nanofibers for efficient polysulfide confinement 被引量:2
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作者 Shanfeng Yang Shuiping Luo +3 位作者 Xinji Dong Li Tian Pei Kang Shen Jinliang Zhu 《Nano Research》 SCIE EI CSCD 2023年第6期8478-8487,共10页
Principles of inexpensive biotechnology are being increasingly used to address the problems posed by the use of lithium-sulfur batteries.We used chitin,a low-cost marine biowaste product,as a precursor for the in-situ... Principles of inexpensive biotechnology are being increasingly used to address the problems posed by the use of lithium-sulfur batteries.We used chitin,a low-cost marine biowaste product,as a precursor for the in-situ preparation of chitin-derived nitrogendoped hierarchical porous carbon fibers(CNHPCFs)containing abundant pores.These materials are characterized by varying morphologies and high specific surface areas and present a hierarchical porous structure.CNHPCFs adsorb polysulfides,exhibit good ionic conductivity,and can be potentially used to generate green energy.These properties help address the problems of volume expansion and slow transport.The CNHPCF-1@S cathode exhibits excellent cycling performance and high capacity(1368.80 mAh·g^(−1)at 0.2 C;decay rate:0.011%per turn at 5 C).The high electrochemical reversibility recorded for CNHPCF-1@S and the stepwise reaction mechanism followed were studied using the in-situ X-ray diffraction and in-situ Raman spectroscopy techniques.The results reported herein can potentially help develop new ideas for the recycling and treatment of marine biofertilizers.The results can also provide a platform to improve the application prospects of lithium-sulfur batteries. 展开更多
关键词 CHITIN carbon fiber Li-S battery in-situ Raman in-situ x-ray diffraction
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Liquid metal assisted regulation of macro-/micro-structures and mechanical properties of nanoporous copper 被引量:2
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作者 ZHANG Ying BAI QingGuo +1 位作者 YANG WanFeng ZHANG ZhongHua 《Science China(Technological Sciences)》 SCIE EI CAS CSCD 2021年第10期2229-2236,共8页
Nanoporous metals have received significant attention as a new class of structural and functional materials.However,the macroscopic brittle fracture under the tensile test is an impediment to their practical applicati... Nanoporous metals have received significant attention as a new class of structural and functional materials.However,the macroscopic brittle fracture under the tensile test is an impediment to their practical applications.Thus,it is of central importance to develop nanoporous materials with low cost and high tensile ductility.Herein,a nanoporous Cu film supported on a pure Cu substrate(NPC@Cu)was fabricated by utilizing a liquid Ga assisted alloying-dealloying strategy,and the thickness of NPC film can be precisely regulated by changing the mass loading of liquid Ga.In-situ X-ray diffraction was performed to further explore the alloying/dealloying mechanisms.The NPC@Cu films show good tensile mechanical properties with a minimum elongation of 13.5%,which can be attributed to the good interface bonding and certain modulus matching between the nanoporous Cu layer and the Cu substrate.Our findings demonstrate that the design of film-substrate structure provides a feasible strategy for enhancing the mechanical properties of nanoporous metals. 展开更多
关键词 nanoporous metals DEALLOYING mechanical properties in-situ x-ray diffraction structural regulation
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