This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction betwee...This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction between various structural materials and molten salts.The apparatus enables accurate detection of every phase change during hightemperature experiments,including strong reaction processes like corrosion.Molten salts,such as chlorides or fluo⁃rides,together with the structure materials,are inserted into either quartz or boron nitride capillaries,where X-ray diffraction pattern can be continuously collected,as the samples are heated to high temperature.The replacement re⁃action,when molten ZnCl2 are etching Ti3AlC2,can be clearly observed through changes in diffraction peak intensity as well as expansion in c-axis lattice parameter of the hexagonal matrix,due to the larger atomic number and ionic ra⁃dius of Zn2+.Furthermore,we investigated the high-temperature corrosion process when GH3535 alloy is in FLiNaK molten salt,and can help to optimize its stability for potential applications in molten salt reactor.Additionally,this high temperature apparatus is fully compatible with the combined usage of X-ray diffraction and Raman technique,providing both bulk and surface structural information.This high temperature apparatus has been open to users and is extensively used at BL14B1 beamline of the Shanghai Synchrotron Radiation Facility.展开更多
The recovery of nickel from molybdenum leach residue by the process of segregation roasting-sulfuric acid leaching-solvent extraction was investigated. The residue was characterized by microscopic investigations, usin...The recovery of nickel from molybdenum leach residue by the process of segregation roasting-sulfuric acid leaching-solvent extraction was investigated. The residue was characterized by microscopic investigations, using X-ray fluorescence spectrometry （XRF） and X-ray diffractometry （XRD） techniques and the residue after segregation roasting was characterized by chemical phase analysis method. A series of experiments were conducted to examine the mass ratio of activated carbon （AC） to the residue, segregation roasting time and temperature, sulfuric acid concentration, liquid-to-solid ratio, leaching time, leaching temperature, addition amount of 30% H2O2, stirring speed （a constant） on the leaching efficiency of nickel. A maximum nickel leaching efficiency of 90.5% is achieved with the mass ratio of AC to the residue of 1：2.5, segregation roasting time of 2 h, segregation roasting temperature of 850 ℃, sulfuric acid concentration of 4.5 mol/L, liquid-to-solid ratio of 6：1, leaching time of 5 h, leaching temperature of 80 ℃, addition of 30% H202 of 0.6 mL for 1 g dry residue. Under these optimized conditions, the average leaching efficiency of nickel is 89.3%. The nickel extraction efficiency in the examined conditions is about 99.6%, and the nickel stripping efficiency in the examined conditions is about 99.2%.展开更多
To develop an effective process for titanium powders production, a calciothermic reduction process of pigment titanium dioxide （w（TiO2）〉98%）, based on the preform reduction process （PRP）, was investigated by me...To develop an effective process for titanium powders production, a calciothermic reduction process of pigment titanium dioxide （w（TiO2）〉98%）, based on the preform reduction process （PRP）, was investigated by means of XRD, SEM and EDS. In this process, the mixture of TiO2 powder and CaC12 was pressed into pieces as feed preform and was reduced by calcium vapor. Titanium powders was recovered after leaching from the reduced preform with hydrochloric acid and deionized water. The results indicate when the mass ratio of CaC12 to TiO2 is about 1：4 and at a constant temperature of 1 273 K for 6 h in vacuum furnace, titanium powders with 99.55% purity by EDS analysis and irregular shape （8-15 μm in particle size） are obtained.展开更多
A high speed steel composite roll billet was fabricated, which is regular in shape, smooth in surface, slight in trace, compact in internal structure, free of slag inclusion, shrinkage cavity, cracks and other flaws, ...A high speed steel composite roll billet was fabricated, which is regular in shape, smooth in surface, slight in trace, compact in internal structure, free of slag inclusion, shrinkage cavity, cracks and other flaws, and good in macro quality of junction surface using a vertical continuous casting machine. The interface zone microstructure of bimetallic in billet of high speed steel composite roll was analyzed by metallurgical microscope(OM), X-ray diffractmeter(XRD), scanning electron microscopy(SEM) and energy-dispersive X-ray analysis(EDS). The results indicate that the microstructure of roll billet is composed of chilled solidified layer, dendrite zone, interfacial zone of bimetal and core material zone. The microstructure of outer shell material is composed of martensite + bainite + residual austenite + some small labyrinth-shape, small-short lath-shape, or dollop-shape eutectic carbides. The microstructure of core material is slice-shape pearlite and a little ferrite along boundary of cells. The interface region microstructure of bimetallic composite roll consists of diffusion region, chilled solidified layer and columnar grain region.展开更多
In order to reduce the oxidizing and volatilizing caused by Mg element in the traditional methods for synthesizing Mg2Sil-xSnx （x=0.2, 0.4, 0.6, 0.8） solid solutions, microwave irradiation techniques were used in pr...In order to reduce the oxidizing and volatilizing caused by Mg element in the traditional methods for synthesizing Mg2Sil-xSnx （x=0.2, 0.4, 0.6, 0.8） solid solutions, microwave irradiation techniques were used in preparing them as thermoelectric materials. Structure and phase composition of the obtained materials were investigated by X-ray diffraction （XRD）. The electrical conductivity, Seebeck coefficient and thermal conductivity were measured as a function of temperature from 300 to 750 K. It is found that Mg2Si1-xSnx solid solutions are well formed with excessive content of 5% （molar fraction） Mg from the stoichiometric MgESil.xSnx under microwave irradiation. A maximum dimensionless figure of merit, ZT, of about 0.26 is obtained for Mg2Si1-xSnx solid solutions at about 500 K for x=0.6.展开更多
Well-crystallized hexagonal hematite （α-Fe2O3） platelets were synthesized by hydrothermal process, using a highly concentrated ferric hydroxide as precursor. The precursor was prepared by adding ammonia to the ferr...Well-crystallized hexagonal hematite （α-Fe2O3） platelets were synthesized by hydrothermal process, using a highly concentrated ferric hydroxide as precursor. The precursor was prepared by adding ammonia to the ferric sulfate solution which was obtained by leaching pyrite cinders with sulfuric acid. Structure and morphology of the synthesized products were investigated by X-ray diffraction, scanning electron microscope, transmission electron microscope and selected area electron diffraction. The results reveal that the reaction temperature has significant effects on the structure, size and shape of the synthesized hematite particles. Typical hexagonal hematite platelets, about 0.4-0.6 μm in diameter and 0.1 μm in thickness, were prepared at 230 ℃ for 0.5 h. Al^3＋, contained in the sulfuric acid leaching solution as an impurity, plays an extremely important role in the formation of hexagonal hematite. In addition, a possible mechanism about the formation of hexagonal hematite platelets was proposed.展开更多
Textile-reinforced concrete(TRC)is suitable to repair and reinforce concrete structures in harsh environments.The performance of the interface between TRC and existing concrete is an important factor in determining th...Textile-reinforced concrete(TRC)is suitable to repair and reinforce concrete structures in harsh environments.The performance of the interface between TRC and existing concrete is an important factor in determining the strengthening effect of TRC.In this paper,a double-sided shear test was performed to investigate the effects of the chloride dry-wet cycles on the average shear strength and slip at the interface between the TRC and existing concrete,also considering the existing concrete strength,bond length,textile layer and short-cut fiber arrangements.In addition,X-ray diffraction(XRD)technology was used to analyze the microscopic matter at the interface in the corrosive environment.The experimental results indicate that the interface performance between TRC and existing concrete would decrease with continued chloride dry-wet cycles.Compared with the specimen with a single layer of textile reinforcement,the specimens with two layers of textile with added PVA or AR-glass short-cut fibers could further improve the properties of the interface between the TRC layer and existing concrete.For the TRC with a single layer of textile,the average shear strength tended to decrease with increasing bond length.In addition,the strength grade of the existing concrete had a minor effect on the interface properties.展开更多
Microarc oxidation （MAO） coatings were prepared on 2024 aluminum alloy in a Na2SiO3-KOH electrolyte with KNinO4 addition varying from 0 to 4 g/L. The microstructure and phases of the coatings were characterized by s...Microarc oxidation （MAO） coatings were prepared on 2024 aluminum alloy in a Na2SiO3-KOH electrolyte with KNinO4 addition varying from 0 to 4 g/L. The microstructure and phases of the coatings were characterized by scanning electron microscopy （SEM） and X-ray diffractometry （XRD）, respectively. The corrosion resistance of MAO coatings was evaluated by electrochemical potentiodynamic polarization in 5% （mass fraction） NaCl solution. The results show that when KMnO4 is added into base electrolyte, the growth speed of oxide coatings is increased obviously. The main phase of oxide coatings is Al2O3, and the contents of MnO2 and MnEA104 phases are increased at the top of oxide coatings with increasing the concentration of KMnO4. The solute elements participate in forming the oxide coatings. When a proper concentration of KMnO4 （2.5 g/L） is added into the base solution, the micropores of the MAO coatings are small and compact, and the corrosion resistance of oxide coatings is increased largely.展开更多
Mesoporous CeO2 was first synthesized by hydrothermal method,and then used to synthesize different contents of CuO)x/CeO2(x:molar ratio of Cu to Ce) by deposition-precipitation method.These materials were characterize...Mesoporous CeO2 was first synthesized by hydrothermal method,and then used to synthesize different contents of CuO)x/CeO2(x:molar ratio of Cu to Ce) by deposition-precipitation method.These materials were characterized by X-ray diffraction(XRD),N2 adsorption and desorption,H2 temperature programmed reduction(H2-TPR) and O2 temperature programmed desorption(O2-TPD) to study the crystal structure,surface area,and the mechanism of CO oxidation.The results show that,on XRD patterns,no evidence of CuO diffraction peaks is present until Cu loading is increased to 20%.The BET surface area decreases noticeably with the increase of Cu content.Compared with other samples,the better reducibility and activity oxygen species of(CuO)10%/CeO2coincide with its better catalytic activity.展开更多
Carbon-carbon composite （C/C） materials are prone to severe oxidation and volatilization problems. To address these issues, mullite （3Al2O3.2SiO2）/silicon carbide （SIC） coatings were deposited on C/C composite s...Carbon-carbon composite （C/C） materials are prone to severe oxidation and volatilization problems. To address these issues, mullite （3Al2O3.2SiO2）/silicon carbide （SIC） coatings were deposited on C/C composite substrates characterized into high and low densities. The coatings were applied by a two-step approach： pack cementation and silica sol based slurry coating processes. The relationship between the microstructure of 3Al2O3·2SiO2/SiC coatings and C/C substrates during isothermal oxidation cycle at 1 500 ℃ was investigated using X-ray diffractometer （XRD） and scanning electron microscope （SEM） mounted with energy dispersive spectrometer （EDS）. The results indicate that the density of the substrates has a marked effect on the coatings. Dense, thick and well-bonded coatings are obtained in the high density substrate. After 106 h of isothermal oxidation, the high density substrate with 3Al2O3-2SiO2/SiC coating offers effective protection as compared to low density substrate suffering recession.展开更多
Mg-8Sn-1Al-1Zn-xNi(x=0.5%, 1.0%, 1.5%, 2.0%, mass fraction) alloys were designed and prepared. The microstructures and the mechanical properties were studied by using optical microscope, scanning electronic microscope...Mg-8Sn-1Al-1Zn-xNi(x=0.5%, 1.0%, 1.5%, 2.0%, mass fraction) alloys were designed and prepared. The microstructures and the mechanical properties were studied by using optical microscope, scanning electronic microscope, energy dispersive X-ray spectroscope, X-ray diffraction and a standard universal testing machine. The results show that the microstructure of Ni-containing alloys consist of α-Mg, Mg2 Sn, β-Mg-Ni-Al and γ-AlNi phases. No β-Mg-Ni-Al phase was observed in TAZ811-2.0Ni alloy due to its 1:1 atomic ratio of Ni/Al. The addition of Ni refines the α-Mg dendrites and suppresses the formation of coarse Mg2 Sn phase. The tensile properties results show that the TAZ811-0.5Ni alloy presented the best mechanical properties, which is due to the rod-like β-Mg-Ni-Al phase, refined α-Mg dendrites and Mg2 Sn phase, as well as γ-AlNi phase. The tensile fracture mechanism transits from cleavage to quasi-cleavage fracture with the increasing Ni addition.展开更多
Micaceous iron oxide （MIO） with a hexagonal flaky shape was prepared by hydrothermal method. The ferric hydroxide used as precursor was obtained by an acidic leaching solution of pyrite cinders reacting with ammonia...Micaceous iron oxide （MIO） with a hexagonal flaky shape was prepared by hydrothermal method. The ferric hydroxide used as precursor was obtained by an acidic leaching solution of pyrite cinders reacting with ammonia solution. The optimal experimental conditions for preparing micaceous iron oxide were investigated by orthogonal experiments. Micaceous iron oxide can be successfully prepared when optimal parameters of total iron concentration of 2.0 mol/L, pH value of 8, n（Fe2＋）/n（Fe3＋） of 0.1, mass of seed crystal of 1 g, reaction temperature of 260 ℃ and reaction time of 30 min are applied. X-ray diffractometry （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM） and selected area electron diffractometry （SAEM） were adopted to characterize the hydrothermal products prepared under optimal conditions. The results indicate that highly crystallized α-Fe2O3 hexagonal flakes, about 1.0-1.5 μm in diameter and 0.1 μm in thickness, are prepared. Furthermore, the quality of micaceous iron oxide prepared can meet the required characteristics of micaceous iron oxide pigments for paints （ISO 10601--2007）.展开更多
The effects of alkali oxides （Na2O and K2O addition on both the sintering behavior and dielectric properties of Ca-AI-B-Si-O glass/Al2O3 composites were investigated by Fourier transform infrared spectroscopy （FTIR...The effects of alkali oxides （Na2O and K2O addition on both the sintering behavior and dielectric properties of Ca-AI-B-Si-O glass/Al2O3 composites were investigated by Fourier transform infrared spectroscopy （FTIR）, differential scanning calorimeter （DSC）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. The results show that the increasing amount of alkali oxides in the glass causes the decrease of [SiO4], which results in the decrease of the continuity of glass network, and leads to the decrease of the softening temperature Tf of the samples and the increasing trend of crystallization. And that deduces corresponding rise of densification, dielectric constant, dielectric loss of the low temperature co-fired ceramic （LTCC） materials and the decrease of its thermal conductivity. By contrast, the borosilicate glass/A1203 composites with 1.5% （mass fraction） alkali oxides sintered at 875 ℃ for 30 rain exhibit better properties of a bulk density of 2.79 g/cm3, a porosity of 0.48%, a 2 value of 2.28 W/（m.K）, a er value of 7.82 and a tand value of 9.1 × 10-4 （measured at 10 MHz）.展开更多
Sodium fluoride and high specific area silica were synthesized by using sodium hexafluorosilicate(Na2Si F6) and sodium carbonate decahydrate(Na2CO3·10H2O). The influencing factors of react temperature, contact ti...Sodium fluoride and high specific area silica were synthesized by using sodium hexafluorosilicate(Na2Si F6) and sodium carbonate decahydrate(Na2CO3·10H2O). The influencing factors of react temperature, contact time, sodium dodecyl sulfate(SDS) and molar ratio of Na2 Si F6 to Na2CO3·10H2O were investigated. The optimum process involves the reaction of 0.075 mol Na2 Si F6 and 150 m L, 0.225 mol Na2CO3·10H2O(molar ratio of 1:3) at 85 °C for 90 min, and 2.0×10-3 mol sodium dodecyl sulfate(SDS) as additive. The results show that the purities of Si O2 and Na F at extraction yields of 96.5% and 98.0% are 91.0% and 98.6%, respectively. The obtained Si O2 were characterized by X-ray diffraction(XRD), scanning electron microscope(SEM), Fourier transform infrared ray(FTIR), differential scanning calorimetry and thermogravimetric analysis(DSC-TGA), N2 absorption/desorption(BET) and laser particle size analyzer. The result demonstrates that Si O2 particles have a high BET surface area of 103 m2/g, and a mean grain size of 985 nm.展开更多
Ru O2·n H2O film was deposited on tantalum foils by electrodeposition and heat treatment using Ru Cl3·3H2O as precursor.Surface morphology, composition change and cyclic voltammetry from precursor to amorpho...Ru O2·n H2O film was deposited on tantalum foils by electrodeposition and heat treatment using Ru Cl3·3H2O as precursor.Surface morphology, composition change and cyclic voltammetry from precursor to amorphous and crystalline RuO2·n H2O films were studied by X-ray diffractometer, Fourier transformation infrared spectrometer, differential thermal analyzer, scanning electron microscope and electrochemical analyzer, respectively. The results show that the precursor was transformed gradually from amorphous to crystalline phase with temperature. When heat treated at 300 °C for 2h, RuO2·n H2O electrode surface gains mass of2.5 mg/cm2 with specific capacitance of 782 F/g. Besides, it is found that the specific capacitance of the film decreased by roughly20% with voltage scan rate increasing from 5 to 250 m V/s.展开更多
The ingots of Pr0.15TbxDy0.85-xFe2 （x=0.10-0.85） series compounds with a single phase were prepared -by a arc melting method. The X-ray diffraction patterns were measured using a Philips X’pert MPD X-ray diffractom...The ingots of Pr0.15TbxDy0.85-xFe2 （x=0.10-0.85） series compounds with a single phase were prepared -by a arc melting method. The X-ray diffraction patterns were measured using a Philips X’pert MPD X-ray diffractometer with a non-ambient sample stage at different temperatures, the magnetostrictive distortion in (Pr0.15TbxDy0.85-xFe2) polycrystals was investigated by X-ray diffraction patterns and the magnetostriction coefficient λ111 was calculated. The results show -when the temperature is raised above the spin reorientation temperature region, a splitting appears in the reflection （440）; the λ111 increase with the increasing of Tb content for (Pr0.15TbxDy0.85-xFe2) polycrystals and the full width at half maximum （FWHM） of the reflection （440） increases gradually with the increasing of Tb content. Moreover, as the FWHM of the reflection （440） decreases gradually with the increasing of temperature, the λ111 decreases slightly with the increasing of temperature at the temperature region of 223-373K for Pr0.15Tb0.3Dy0.55Fe2 alloy.展开更多
Oxidation behaviors of blank and CeO2 coated T91 steel were investigated at 600 ℃ in water vapor for up to 150 h. Gold marker was used to define the mass transport direction. The oxide scales were studied with X-ray ...Oxidation behaviors of blank and CeO2 coated T91 steel were investigated at 600 ℃ in water vapor for up to 150 h. Gold marker was used to define the mass transport direction. The oxide scales were studied with X-ray diffractometry （XRD）, scanning electron microscopy （SEM） and electron probe microanalyzer （EPMA）. The oxidation resistance of the steel is improved by CeO2 coating, though the improvement is not remarkable. Ce-rich oxide band is located at the interface of the inner equiaxed layer and the outer columnar layer after oxidation, which is not consistent with the original surface. The results show that outward iron transport is blocked by the Ce-rich band. A new oxide nucleating and growing site （reaction front） is induced at the inner surface of the Ce rich band.展开更多
The development of the recrystallization texture of the alloy AA3104 was investigated by analysis of orientation distribution functions determined by X-ray diffraction,supported by EBSD local texture analysis.A typic...The development of the recrystallization texture of the alloy AA3104 was investigated by analysis of orientation distribution functions determined by X-ray diffraction,supported by EBSD local texture analysis.A typical β-fiber with nearly 20%Bs orientation {011}211 was detected in the final hot rolled sheet.At the beginning of annealing at 350 ℃,the cube component{001}100 got a sharp increase.TEM results show that the growth of both number and size of precipitation appears to inhibit the advantage of Cube orientation {001}100 notably after annealing at 350 ℃ for 15 min.Finally,it comes out to be a random distributed orientation by full recry stallization.展开更多
The effect of H_2 gas content on the reduction of Panzhihua titanomagnetite concentrate pellets by carbon monoxide was investigated by isothermal reduction experiment using CO-N_2-H_2 gas mixtures in a vertical electr...The effect of H_2 gas content on the reduction of Panzhihua titanomagnetite concentrate pellets by carbon monoxide was investigated by isothermal reduction experiment using CO-N_2-H_2 gas mixtures in a vertical electric resistance furnace.The morphology and phase transformation of reduced samples obtained were detected by scanning electron microscopy,energy disperse spectroscopy analysis and X-ray diffractometry respectively.The results show that increasing H_2 content will enhance the initial stage of reduction rate apparently.There are two reasons responsible for this effect,one is that H_2 accelerates the chemical reaction,and the other is that the addition of H_2 gas can improve the porosity of pellet intensively.It is noteworthy that this effect is more obvious when the reduction temperature reaches 1473 K with sticking phenomenon happening.There are no crystalline phases which can be found such as ulvospinle,ilmenite,ferrous-pseudobrookite and any titanium oxide except titanomagnetite(TTM).The reduction progress is suggested as follows:1) Fe_2O_3→Fe_3O_4→FeO→Fe;2) Fe_2TiO_5→Fe_2TiO_4+Fe_3O_4→TTM.Element Al migrates and gets enriched in high titanium content iron ores,and eventually Al to Ti molar ratio is 1:3.Al is likely to dissolve in titanium iron oxides to form a kind of composite iron compound,which results in the restrain of reduction.展开更多
基金CAS Photon Science Research Center for Carbon DioxideCAS President’s International Fellowship Initiative(2024PVA0097)+1 种基金National Key Research and Development Program of China(2017YFA0403000,2017YFA0402800)National Natural Science Foundation of China(U1932201,U1732121)。
文摘This study demonstrates the design and application of a novel high temperature rotatory apparatus for insitu synchrotron X-ray diffraction studies of molten salts,facilitating investigation into the interaction between various structural materials and molten salts.The apparatus enables accurate detection of every phase change during hightemperature experiments,including strong reaction processes like corrosion.Molten salts,such as chlorides or fluo⁃rides,together with the structure materials,are inserted into either quartz or boron nitride capillaries,where X-ray diffraction pattern can be continuously collected,as the samples are heated to high temperature.The replacement re⁃action,when molten ZnCl2 are etching Ti3AlC2,can be clearly observed through changes in diffraction peak intensity as well as expansion in c-axis lattice parameter of the hexagonal matrix,due to the larger atomic number and ionic ra⁃dius of Zn2+.Furthermore,we investigated the high-temperature corrosion process when GH3535 alloy is in FLiNaK molten salt,and can help to optimize its stability for potential applications in molten salt reactor.Additionally,this high temperature apparatus is fully compatible with the combined usage of X-ray diffraction and Raman technique,providing both bulk and surface structural information.This high temperature apparatus has been open to users and is extensively used at BL14B1 beamline of the Shanghai Synchrotron Radiation Facility.
基金Project(2007CB613604)supported by the National Basic Research Program of China
文摘The recovery of nickel from molybdenum leach residue by the process of segregation roasting-sulfuric acid leaching-solvent extraction was investigated. The residue was characterized by microscopic investigations, using X-ray fluorescence spectrometry （XRF） and X-ray diffractometry （XRD） techniques and the residue after segregation roasting was characterized by chemical phase analysis method. A series of experiments were conducted to examine the mass ratio of activated carbon （AC） to the residue, segregation roasting time and temperature, sulfuric acid concentration, liquid-to-solid ratio, leaching time, leaching temperature, addition amount of 30% H2O2, stirring speed （a constant） on the leaching efficiency of nickel. A maximum nickel leaching efficiency of 90.5% is achieved with the mass ratio of AC to the residue of 1：2.5, segregation roasting time of 2 h, segregation roasting temperature of 850 ℃, sulfuric acid concentration of 4.5 mol/L, liquid-to-solid ratio of 6：1, leaching time of 5 h, leaching temperature of 80 ℃, addition of 30% H202 of 0.6 mL for 1 g dry residue. Under these optimized conditions, the average leaching efficiency of nickel is 89.3%. The nickel extraction efficiency in the examined conditions is about 99.6%, and the nickel stripping efficiency in the examined conditions is about 99.2%.
基金Project(51004058) supported by the National Natural Science Foundation of ChinaProject(2011FB039) supported by the Natural Science Foundation of Yunnan Province,China
文摘To develop an effective process for titanium powders production, a calciothermic reduction process of pigment titanium dioxide （w（TiO2）〉98%）, based on the preform reduction process （PRP）, was investigated by means of XRD, SEM and EDS. In this process, the mixture of TiO2 powder and CaC12 was pressed into pieces as feed preform and was reduced by calcium vapor. Titanium powders was recovered after leaching from the reduced preform with hydrochloric acid and deionized water. The results indicate when the mass ratio of CaC12 to TiO2 is about 1：4 and at a constant temperature of 1 273 K for 6 h in vacuum furnace, titanium powders with 99.55% purity by EDS analysis and irregular shape （8-15 μm in particle size） are obtained.
基金Project(200809123) supported by the National Natural Science Foundation of China
文摘A high speed steel composite roll billet was fabricated, which is regular in shape, smooth in surface, slight in trace, compact in internal structure, free of slag inclusion, shrinkage cavity, cracks and other flaws, and good in macro quality of junction surface using a vertical continuous casting machine. The interface zone microstructure of bimetallic in billet of high speed steel composite roll was analyzed by metallurgical microscope(OM), X-ray diffractmeter(XRD), scanning electron microscopy(SEM) and energy-dispersive X-ray analysis(EDS). The results indicate that the microstructure of roll billet is composed of chilled solidified layer, dendrite zone, interfacial zone of bimetal and core material zone. The microstructure of outer shell material is composed of martensite + bainite + residual austenite + some small labyrinth-shape, small-short lath-shape, or dollop-shape eutectic carbides. The microstructure of core material is slice-shape pearlite and a little ferrite along boundary of cells. The interface region microstructure of bimetallic composite roll consists of diffusion region, chilled solidified layer and columnar grain region.
基金Project(2009BB4228) supported by the Natural Science Foundation of Chongqing City,ChinaProject(CK2010Z09) supported by the Research Foundation of Chongqing University of Science and Technology,China
文摘In order to reduce the oxidizing and volatilizing caused by Mg element in the traditional methods for synthesizing Mg2Sil-xSnx （x=0.2, 0.4, 0.6, 0.8） solid solutions, microwave irradiation techniques were used in preparing them as thermoelectric materials. Structure and phase composition of the obtained materials were investigated by X-ray diffraction （XRD）. The electrical conductivity, Seebeck coefficient and thermal conductivity were measured as a function of temperature from 300 to 750 K. It is found that Mg2Si1-xSnx solid solutions are well formed with excessive content of 5% （molar fraction） Mg from the stoichiometric MgESil.xSnx under microwave irradiation. A maximum dimensionless figure of merit, ZT, of about 0.26 is obtained for Mg2Si1-xSnx solid solutions at about 500 K for x=0.6.
基金Project(2008A090300016) supported by the Key Science and Technology Item of Guangdong Province,ChinaProject(ZKJ2010022) supported by the Precious Apparatus Opening Center Foundation of Central South University,China
文摘Well-crystallized hexagonal hematite （α-Fe2O3） platelets were synthesized by hydrothermal process, using a highly concentrated ferric hydroxide as precursor. The precursor was prepared by adding ammonia to the ferric sulfate solution which was obtained by leaching pyrite cinders with sulfuric acid. Structure and morphology of the synthesized products were investigated by X-ray diffraction, scanning electron microscope, transmission electron microscope and selected area electron diffraction. The results reveal that the reaction temperature has significant effects on the structure, size and shape of the synthesized hematite particles. Typical hexagonal hematite platelets, about 0.4-0.6 μm in diameter and 0.1 μm in thickness, were prepared at 230 ℃ for 0.5 h. Al^3＋, contained in the sulfuric acid leaching solution as an impurity, plays an extremely important role in the formation of hexagonal hematite. In addition, a possible mechanism about the formation of hexagonal hematite platelets was proposed.
基金Project(2017XKZD09)supported by the Fundamental Research Funds for the Central Universities,China。
文摘Textile-reinforced concrete(TRC)is suitable to repair and reinforce concrete structures in harsh environments.The performance of the interface between TRC and existing concrete is an important factor in determining the strengthening effect of TRC.In this paper,a double-sided shear test was performed to investigate the effects of the chloride dry-wet cycles on the average shear strength and slip at the interface between the TRC and existing concrete,also considering the existing concrete strength,bond length,textile layer and short-cut fiber arrangements.In addition,X-ray diffraction(XRD)technology was used to analyze the microscopic matter at the interface in the corrosive environment.The experimental results indicate that the interface performance between TRC and existing concrete would decrease with continued chloride dry-wet cycles.Compared with the specimen with a single layer of textile reinforcement,the specimens with two layers of textile with added PVA or AR-glass short-cut fibers could further improve the properties of the interface between the TRC layer and existing concrete.For the TRC with a single layer of textile,the average shear strength tended to decrease with increasing bond length.In addition,the strength grade of the existing concrete had a minor effect on the interface properties.
基金Project(2008BAE63B00) supported by the National Key Technologies Research and Development Program of China
文摘Microarc oxidation （MAO） coatings were prepared on 2024 aluminum alloy in a Na2SiO3-KOH electrolyte with KNinO4 addition varying from 0 to 4 g/L. The microstructure and phases of the coatings were characterized by scanning electron microscopy （SEM） and X-ray diffractometry （XRD）, respectively. The corrosion resistance of MAO coatings was evaluated by electrochemical potentiodynamic polarization in 5% （mass fraction） NaCl solution. The results show that when KMnO4 is added into base electrolyte, the growth speed of oxide coatings is increased obviously. The main phase of oxide coatings is Al2O3, and the contents of MnO2 and MnEA104 phases are increased at the top of oxide coatings with increasing the concentration of KMnO4. The solute elements participate in forming the oxide coatings. When a proper concentration of KMnO4 （2.5 g/L） is added into the base solution, the micropores of the MAO coatings are small and compact, and the corrosion resistance of oxide coatings is increased largely.
基金Project(2011FZ030)supported by the Natural Science Foundation of Yunnan Province,ChinaProjects(2011144,2011221)supported by Analysis and Test Foundation of Kunming University of Science and Technology,China
文摘Mesoporous CeO2 was first synthesized by hydrothermal method,and then used to synthesize different contents of CuO)x/CeO2(x:molar ratio of Cu to Ce) by deposition-precipitation method.These materials were characterized by X-ray diffraction(XRD),N2 adsorption and desorption,H2 temperature programmed reduction(H2-TPR) and O2 temperature programmed desorption(O2-TPD) to study the crystal structure,surface area,and the mechanism of CO oxidation.The results show that,on XRD patterns,no evidence of CuO diffraction peaks is present until Cu loading is increased to 20%.The BET surface area decreases noticeably with the increase of Cu content.Compared with other samples,the better reducibility and activity oxygen species of(CuO)10%/CeO2coincide with its better catalytic activity.
基金Project(2011CB605805) supported by the National Basic Research Program of ChinaProject(51021063) supported by the Creative Research Group of National Natural Science Foundation of China
文摘Carbon-carbon composite （C/C） materials are prone to severe oxidation and volatilization problems. To address these issues, mullite （3Al2O3.2SiO2）/silicon carbide （SIC） coatings were deposited on C/C composite substrates characterized into high and low densities. The coatings were applied by a two-step approach： pack cementation and silica sol based slurry coating processes. The relationship between the microstructure of 3Al2O3·2SiO2/SiC coatings and C/C substrates during isothermal oxidation cycle at 1 500 ℃ was investigated using X-ray diffractometer （XRD） and scanning electron microscope （SEM） mounted with energy dispersive spectrometer （EDS）. The results indicate that the density of the substrates has a marked effect on the coatings. Dense, thick and well-bonded coatings are obtained in the high density substrate. After 106 h of isothermal oxidation, the high density substrate with 3Al2O3-2SiO2/SiC coating offers effective protection as compared to low density substrate suffering recession.
基金Projects supported by the Shanxi Selective Funds for Returned Scholars,ChinaProject(2013021013-4)supported by the Shanxi Province Science Foundation for Youths China+1 种基金Projects(2012L053,2012L003)supported by the Taiyuan University of Technology Funds for Young Scientists,ChinaProject(2014021017-2)supported by the Natural Science Foundation for Young Scientists for Shanxi Province,China
文摘Mg-8Sn-1Al-1Zn-xNi(x=0.5%, 1.0%, 1.5%, 2.0%, mass fraction) alloys were designed and prepared. The microstructures and the mechanical properties were studied by using optical microscope, scanning electronic microscope, energy dispersive X-ray spectroscope, X-ray diffraction and a standard universal testing machine. The results show that the microstructure of Ni-containing alloys consist of α-Mg, Mg2 Sn, β-Mg-Ni-Al and γ-AlNi phases. No β-Mg-Ni-Al phase was observed in TAZ811-2.0Ni alloy due to its 1:1 atomic ratio of Ni/Al. The addition of Ni refines the α-Mg dendrites and suppresses the formation of coarse Mg2 Sn phase. The tensile properties results show that the TAZ811-0.5Ni alloy presented the best mechanical properties, which is due to the rod-like β-Mg-Ni-Al phase, refined α-Mg dendrites and Mg2 Sn phase, as well as γ-AlNi phase. The tensile fracture mechanism transits from cleavage to quasi-cleavage fracture with the increasing Ni addition.
基金Project(2008A090300016) supported by Major Science & Technology Special Program of Guangdong Province,China
文摘Micaceous iron oxide （MIO） with a hexagonal flaky shape was prepared by hydrothermal method. The ferric hydroxide used as precursor was obtained by an acidic leaching solution of pyrite cinders reacting with ammonia solution. The optimal experimental conditions for preparing micaceous iron oxide were investigated by orthogonal experiments. Micaceous iron oxide can be successfully prepared when optimal parameters of total iron concentration of 2.0 mol/L, pH value of 8, n（Fe2＋）/n（Fe3＋） of 0.1, mass of seed crystal of 1 g, reaction temperature of 260 ℃ and reaction time of 30 min are applied. X-ray diffractometry （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM） and selected area electron diffractometry （SAEM） were adopted to characterize the hydrothermal products prepared under optimal conditions. The results indicate that highly crystallized α-Fe2O3 hexagonal flakes, about 1.0-1.5 μm in diameter and 0.1 μm in thickness, are prepared. Furthermore, the quality of micaceous iron oxide prepared can meet the required characteristics of micaceous iron oxide pigments for paints （ISO 10601--2007）.
基金Project(2007AA03Z0455) supported by the National High Technology Research and Development Program ("863" Program) of ChinaProject(BE2010194) supported by Science & Technology Pillar Program of Jiangsu in China+3 种基金Project(BE2009168) supported by Science & Technology Pillar Program of Jiangsu in ChinaProject supported by the Priority Academic Program Development (PAPD) of Jiangsu Higher Education InstitutionsProject(KF201103) supported by State Key Laboratory of New Ceramic and Fine Processing Tsinghua UniversityProject(CXZZ12_0415) supported by Innovation Foundation for Graduate Students of Jiangsu Province,China
文摘The effects of alkali oxides （Na2O and K2O addition on both the sintering behavior and dielectric properties of Ca-AI-B-Si-O glass/Al2O3 composites were investigated by Fourier transform infrared spectroscopy （FTIR）, differential scanning calorimeter （DSC）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. The results show that the increasing amount of alkali oxides in the glass causes the decrease of [SiO4], which results in the decrease of the continuity of glass network, and leads to the decrease of the softening temperature Tf of the samples and the increasing trend of crystallization. And that deduces corresponding rise of densification, dielectric constant, dielectric loss of the low temperature co-fired ceramic （LTCC） materials and the decrease of its thermal conductivity. By contrast, the borosilicate glass/A1203 composites with 1.5% （mass fraction） alkali oxides sintered at 875 ℃ for 30 rain exhibit better properties of a bulk density of 2.79 g/cm3, a porosity of 0.48%, a 2 value of 2.28 W/（m.K）, a er value of 7.82 and a tand value of 9.1 × 10-4 （measured at 10 MHz）.
文摘Sodium fluoride and high specific area silica were synthesized by using sodium hexafluorosilicate(Na2Si F6) and sodium carbonate decahydrate(Na2CO3·10H2O). The influencing factors of react temperature, contact time, sodium dodecyl sulfate(SDS) and molar ratio of Na2 Si F6 to Na2CO3·10H2O were investigated. The optimum process involves the reaction of 0.075 mol Na2 Si F6 and 150 m L, 0.225 mol Na2CO3·10H2O(molar ratio of 1:3) at 85 °C for 90 min, and 2.0×10-3 mol sodium dodecyl sulfate(SDS) as additive. The results show that the purities of Si O2 and Na F at extraction yields of 96.5% and 98.0% are 91.0% and 98.6%, respectively. The obtained Si O2 were characterized by X-ray diffraction(XRD), scanning electron microscope(SEM), Fourier transform infrared ray(FTIR), differential scanning calorimetry and thermogravimetric analysis(DSC-TGA), N2 absorption/desorption(BET) and laser particle size analyzer. The result demonstrates that Si O2 particles have a high BET surface area of 103 m2/g, and a mean grain size of 985 nm.
基金Project(S2013040015492)supported by the Natural Science Foundation of Guangdong Province,ChinaProject(2007AA03Z240)supported by Hi-tech Research and Development Program of China
文摘Ru O2·n H2O film was deposited on tantalum foils by electrodeposition and heat treatment using Ru Cl3·3H2O as precursor.Surface morphology, composition change and cyclic voltammetry from precursor to amorphous and crystalline RuO2·n H2O films were studied by X-ray diffractometer, Fourier transformation infrared spectrometer, differential thermal analyzer, scanning electron microscope and electrochemical analyzer, respectively. The results show that the precursor was transformed gradually from amorphous to crystalline phase with temperature. When heat treated at 300 °C for 2h, RuO2·n H2O electrode surface gains mass of2.5 mg/cm2 with specific capacitance of 782 F/g. Besides, it is found that the specific capacitance of the film decreased by roughly20% with voltage scan rate increasing from 5 to 250 m V/s.
基金Project(50271023) supported by the National Natural Science Foundation of China
文摘The ingots of Pr0.15TbxDy0.85-xFe2 （x=0.10-0.85） series compounds with a single phase were prepared -by a arc melting method. The X-ray diffraction patterns were measured using a Philips X’pert MPD X-ray diffractometer with a non-ambient sample stage at different temperatures, the magnetostrictive distortion in (Pr0.15TbxDy0.85-xFe2) polycrystals was investigated by X-ray diffraction patterns and the magnetostriction coefficient λ111 was calculated. The results show -when the temperature is raised above the spin reorientation temperature region, a splitting appears in the reflection （440）; the λ111 increase with the increasing of Tb content for (Pr0.15TbxDy0.85-xFe2) polycrystals and the full width at half maximum （FWHM） of the reflection （440） increases gradually with the increasing of Tb content. Moreover, as the FWHM of the reflection （440） decreases gradually with the increasing of temperature, the λ111 decreases slightly with the increasing of temperature at the temperature region of 223-373K for Pr0.15Tb0.3Dy0.55Fe2 alloy.
基金Project(2007A-47) supported by Shandong Electric Power Corporation,China
文摘Oxidation behaviors of blank and CeO2 coated T91 steel were investigated at 600 ℃ in water vapor for up to 150 h. Gold marker was used to define the mass transport direction. The oxide scales were studied with X-ray diffractometry （XRD）, scanning electron microscopy （SEM） and electron probe microanalyzer （EPMA）. The oxidation resistance of the steel is improved by CeO2 coating, though the improvement is not remarkable. Ce-rich oxide band is located at the interface of the inner equiaxed layer and the outer columnar layer after oxidation, which is not consistent with the original surface. The results show that outward iron transport is blocked by the Ce-rich band. A new oxide nucleating and growing site （reaction front） is induced at the inner surface of the Ce rich band.
文摘The development of the recrystallization texture of the alloy AA3104 was investigated by analysis of orientation distribution functions determined by X-ray diffraction,supported by EBSD local texture analysis.A typical β-fiber with nearly 20%Bs orientation {011}211 was detected in the final hot rolled sheet.At the beginning of annealing at 350 ℃,the cube component{001}100 got a sharp increase.TEM results show that the growth of both number and size of precipitation appears to inhibit the advantage of Cube orientation {001}100 notably after annealing at 350 ℃ for 15 min.Finally,it comes out to be a random distributed orientation by full recry stallization.
基金Project (51134008) supported by the National Natural Science Foundation of ChinaProject (2012CB720401) supported by the National Basic Research Program of China
文摘The effect of H_2 gas content on the reduction of Panzhihua titanomagnetite concentrate pellets by carbon monoxide was investigated by isothermal reduction experiment using CO-N_2-H_2 gas mixtures in a vertical electric resistance furnace.The morphology and phase transformation of reduced samples obtained were detected by scanning electron microscopy,energy disperse spectroscopy analysis and X-ray diffractometry respectively.The results show that increasing H_2 content will enhance the initial stage of reduction rate apparently.There are two reasons responsible for this effect,one is that H_2 accelerates the chemical reaction,and the other is that the addition of H_2 gas can improve the porosity of pellet intensively.It is noteworthy that this effect is more obvious when the reduction temperature reaches 1473 K with sticking phenomenon happening.There are no crystalline phases which can be found such as ulvospinle,ilmenite,ferrous-pseudobrookite and any titanium oxide except titanomagnetite(TTM).The reduction progress is suggested as follows:1) Fe_2O_3→Fe_3O_4→FeO→Fe;2) Fe_2TiO_5→Fe_2TiO_4+Fe_3O_4→TTM.Element Al migrates and gets enriched in high titanium content iron ores,and eventually Al to Ti molar ratio is 1:3.Al is likely to dissolve in titanium iron oxides to form a kind of composite iron compound,which results in the restrain of reduction.
