Based on A356 aluminum alloy,aluminum foams were prepared by gas injection foaming process with pure nitrogen,air and some gas mixtures.The oxygen volume fraction of these gas mixtures varied from 0.2%to 8.0%.Optical ...Based on A356 aluminum alloy,aluminum foams were prepared by gas injection foaming process with pure nitrogen,air and some gas mixtures.The oxygen volume fraction of these gas mixtures varied from 0.2%to 8.0%.Optical microscopy,scanning electron microscopy(SEM) and Auger electron spectroscopy(AES) were used to analyze the influence of oxygen content on cell structure,relative density,macro and micro morphology of cell walls,coverage area fraction of oxide film,thickness of oxide film and other aspects.Results indicate that the coverage area fraction of oxide film on bubble surface increases with the increase of oxygen content when the oxygen volume is less than 1.2%.While when the oxygen volume fraction is larger than 1.6%,an oxide film covers the entire bubble surface and aluminum foams with good cell structure can be produced.The thicknesses of oxide films of aluminum foams produced by gas mixtures containing 1.6%-21%oxygen are almost the same.The reasons why the thickness of oxide film nearly does not change with the variation of oxygen content and the amount of oxygen needed to achieve 100%coverage of oxide film are both discussed.In addition,the role of oxide film on bubble surface in foam stability is also analyzed.展开更多
In the range of 620?710 °C, air was blown into A356 aluminum alloy melt to produce aluminum foams. In order to study the influence of temperature on the thickness of oxide film on bubble surface, Auger electron ...In the range of 620?710 °C, air was blown into A356 aluminum alloy melt to produce aluminum foams. In order to study the influence of temperature on the thickness of oxide film on bubble surface, Auger electron spectroscopy (AES) was used. Based on the knowledge of corrosion science and hydrodynamics, two oxidation kinetics models of oxide film on bubble surface were established. The thicknesses of oxide films produced at different temperatures were predicted through those two models. Furthermore, the theoretical values were compared with the experimental values. The results indicate that in the range of 620?710 °C, the theoretical values of the thickness of oxide film predicted by the model including the rising process are higher than the experimental values. While, the theoretical values predicted by the model without the rising process are in good agreement with the experimental values, which shows this model objectively describes the oxidation process of oxide film on bubble surface. This work suggests that the oxidation kinetics of oxide film on bubble surface of aluminum foams produced by gas injection foaming process follows the Arrhenius equation.展开更多
Electrochromic and auto-bleaching processes at the WO2 anodic film in 0. 5 mol/L H2SO4 solution were investigated by cyclic voltammetry, a. c. impedance technique and photocurrent spectrometry. The colouration mechani...Electrochromic and auto-bleaching processes at the WO2 anodic film in 0. 5 mol/L H2SO4 solution were investigated by cyclic voltammetry, a. c. impedance technique and photocurrent spectrometry. The colouration mechanism consists of hydrogen adsorption on the WO2 surface and the transport of H atoms in the WO, lattice. The bleaching process involves at least two steps: transport of interstitial H atoms and hydrogen desorption on the W surface, resulting in interstitial H+ ions; then extration of the H+ ions driven by the external electric field. The auto-bleaching arises from the hydroxylation due to both partial interstitial H atoms and a little of water contained in the film.展开更多
A study was conducted to develop low-friction, wear-resistant surfaces on high temperature alloys for the temperature range from 26℃ to 900℃. The approach investigated consists of modifying the naturally occurring o...A study was conducted to develop low-friction, wear-resistant surfaces on high temperature alloys for the temperature range from 26℃ to 900℃. The approach investigated consists of modifying the naturally occurring oxide film in order to improve its tribological properties. Improvement is needed at low temperatures where the oxide film, previously formed at high temperature, spalls due to stresses induced by sliding. Experiments with Ti, W and Ta additions show a beneficial effect when added to Ni and Ni-base alloys. Low friction can be maintained down to 100℃ from 900℃. For unalloyed Ni friction and surface damage increases at 400℃ to 500℃. Two new alloys were perpared based on the beneficial results of binary alloys and ZrO2 diffusion in Ni.Low friction at temperature above 500℃ and reasonable values (0.32~0.42) at low temperature are obtained.展开更多
Nano cerium oxide films were applied on AA7020-T6 aluminum alloy and the effects of acetic acid concentration on the microstructure and electrochemical properties of the coated samples were investigated by using scann...Nano cerium oxide films were applied on AA7020-T6 aluminum alloy and the effects of acetic acid concentration on the microstructure and electrochemical properties of the coated samples were investigated by using scanning electron microscopy (SEM), X-ray diffraction (XRD), and potentiodynamic polarization methods. It has been found that by increasing the acetic acid/CeCl3·7H2O molar ratio, high uniform and crack-free films with well-developed grains were obtained and grain sizes of the films decreased. Elimination of cracks and decreasing grain size of the nano cerium oxide films caused corrosion resistance to increase.展开更多
Anodic oxide films of the titanium alloy Ti-10V-2Fe-3Al in ammonium tartrate electrolyte without hydrofluoric acid or fluoride were fabricated. The morphology, components, and microstructure of the films were characte...Anodic oxide films of the titanium alloy Ti-10V-2Fe-3Al in ammonium tartrate electrolyte without hydrofluoric acid or fluoride were fabricated. The morphology, components, and microstructure of the films were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results showed that the films were thick, uniform, and nontransparent. Such films exhibited sedimentary morphology, with a thickness of about 3 μm, and the pore diameters of the deposits ranged from several hundred nanometers to 1.5 μm. The films were mainly titanium dioxide. Some coke-like deposits, which may contain or be changed by OH, NH, C-C, C-O, and C=O groups, were doped in the films. The films were mainly amorphous with a small amount of anatase and rutile phase.展开更多
Porous anodic oxide films were fabricated galvanostatically on titanium alloy Ti-10V-2Fe-3Al in ammonium tartrate solution with different anodizing time.Scanning electron microscopy(SEM) and field emission scanning el...Porous anodic oxide films were fabricated galvanostatically on titanium alloy Ti-10V-2Fe-3Al in ammonium tartrate solution with different anodizing time.Scanning electron microscopy(SEM) and field emission scanning electron microscopy(FE-SEM) were used to investigate the morphology evolution of the anodic oxide film.It is shown that above the breakdown voltage,oxygen is generated with the occurrence of drums morphology.These drums grow and extrude,which yields the compression stress.Subsequently,microcracks are generated.With continuous anodizing,porous oxides form at the microcracks.Those oxides grow and connect to each other,finally replace the microcrack morphology.The depth profile of the anodic oxide film formed at 1 800 s was examined by Auger electron spectroscopy(AES).It is found that the film is divided into three layers according to the molar fractions of elements.The outer layer is incorporated by carbon,which may come from electrolyte solution.The thickness of the outer layer is approximately 0.2-0.3 μm.The molar fractions of elements in the intermediate layer are extraordinarily stable,while those in the inner layer vary significantly with sputtering depth.The thicknesses of the intermediate layer and the inner layer are 2 μm and 1.0-1.5 μm,respectively.Moreover,the growth mechanism of porous anodic oxide films in neutral tartrate solution was proposed.展开更多
The oxidation kinetics,surface morphology and phase structure of oxide films grown on 25Cr20Ni alloy in air-H2O and H2-H2O atmospheres at 900 ℃ for 20 h were investigated.The anti-coking performance and resistance to...The oxidation kinetics,surface morphology and phase structure of oxide films grown on 25Cr20Ni alloy in air-H2O and H2-H2O atmospheres at 900 ℃ for 20 h were investigated.The anti-coking performance and resistance to carburization of the two oxide films were compared using 25Cr20Ni alloy tubes with an inner diameter of 10 mm and a length of 850 mm in a bench scale naphtha steam pyrolysis unit.The oxidation kinetics followed a parabolic law in an air-H2O atmosphere and a logarithm law in a H2-H2O atmosphere in the steady-state stage.The oxide film grown in the air-H2O atmosphere had cracks where the elements Fe and Ni were enriched and the un-cracked area was covered with octahedral-shaped MnCr2O4 spinels and Cr1.3Fe0.7O3 oxide clusters,while the oxide film grown in the H2-H2O atmosphere was intact and completely covered with dense standing blade MnCr2O4 spinels.In the pyrolysis tests,the anti-coking performance and resistance to carburization of the oxide film grown in the H2-H2O atmosphere were far better than that in the air-H2O atmosphere.The mass of coke formed in the oxide film grown in the H2-H2O atmosphere was less than 10% of that in the air-H2O atmosphere.The Cr1.3Fe0.7O3 oxide clusters converted into Cr23C6 carbides and the cracks were filled with carbon in the oxide film grown in the air-H2O atmosphere after repeated coking and decoking tests,while the dense standing blade MnCr2O4 spinels remained unchanged in the oxide film grown in the H2-H2O atmosphere.The ethylene,propylene and butadiene yields in the pyrolysis tests were almost the same for the two oxide films.展开更多
The effect of depressurizing speed on mold filling behavior and entrainment of oxide film of A356 alloy was studied. Themold filling behavior and velocity fields were recorded by water simulation with particle image v...The effect of depressurizing speed on mold filling behavior and entrainment of oxide film of A356 alloy was studied. Themold filling behavior and velocity fields were recorded by water simulation with particle image velocimetry. The results show thatthe gate velocity first increased dramatically, then changed with the depressurizing speed: the gate velocity increased slowly atrelatively high depressurizing speed; at reasonable depressurizing speed, the gate velocity kept unchanged; while at lowerdepressurizing speed, the gate velocity decreased firstly and then kept unchanged. High gate velocity results in melt falling backunder gravity at higher speed. The falling velocity is the main factor of oxide film entrainment in vacuum suction casting. The designcriterion of depressurizing rate was deduced, and the A356 alloy castings were poured to test the formula. The four-point bend testand Weibull probability plots were applied to assessing the fracture mechanisms of the as-cast A356 alloy. The results illuminate amethod on designing suitable depressurizing speed for mold filling in vacuum suction casting.展开更多
The chemical stripping method of titanium alloy oxide films was studied. An environment friendly solution hydrogen peroxide and sodium hydroxide without hydrofluoric acid or fluoride were used to strip the oxide films...The chemical stripping method of titanium alloy oxide films was studied. An environment friendly solution hydrogen peroxide and sodium hydroxide without hydrofluoric acid or fluoride were used to strip the oxide films. The morphologies of the surface and cross-section of the oxide films before and after the films stripping were characterized by using scanning electron microscopy (SEM). The microstructure and chemical compositions of the oxide films before and after the films stripping were investigated by using Raman spectroscopy (Raman) and X-ray photoelectron spectroscopy (XPS). It was shown that the thickness of the oxide film was in the range of 5-6 μm. The oxide films were stripped for 2 to 8 min in the solution. Moreover, the effect of the stripping time on the efficiency of the film stripping was investigated, and the optimum stripping time was between 6-8 min. When the stripping solution completely dissolved the whole film, the α/β microstructure of the titanium alloy Ti-10V-2Fe-3Al was partly revealed. The stripping mechanism was discussed in terms of the dissolution of film delamination. The hydrogen peroxide had a significant effect on the dissolution of the titanium alloy anodic oxide film. The feasibility of the dissolution reaction also was evaluated.展开更多
The evolution of morphology, composition, thickness and corrosion resistance of the oxide film on pure Sn solder substrate submitted to high-temperature aging in 150 °C dry atmosphere was investigated. The result...The evolution of morphology, composition, thickness and corrosion resistance of the oxide film on pure Sn solder substrate submitted to high-temperature aging in 150 °C dry atmosphere was investigated. The results indicate that high-temperature aging accelerates the dehydration of Sn(OH)_(4)in the pre-existing native oxide film to form SnO_(2)and facilitates the oxidation of fresh Sn substrate, resulting in the gradual increase in oxide film thickness and surface roughness with prolonging aging time. However, the corrosion resistance of the film initially is enhanced and then deteriorated with an extending aging time. Besides, the formation and evolution mechanisms of the oxide film with aging time were discussed.展开更多
Al specimens were covered with TiO2 film by sol-gel dip-coating and then anodized in ammonium adipate solution.The structure,composition and capacitance properties of the anodic oxide film were investigated by transmi...Al specimens were covered with TiO2 film by sol-gel dip-coating and then anodized in ammonium adipate solution.The structure,composition and capacitance properties of the anodic oxide film were investigated by transmission electron microscopy (TEM),Auger electron spectroscopy (AES),X-ray diffractometry (XRD) and electrochemical impedance spectroscopy (EIS).It was found that an anodic oxide film with a dual-layer structure formed between TiO2 coating and Al substrate.The film consisted of an inner Al2O3 layer and an outer Ti-Al composite oxide layer.The thickness of layers varied with the number of times of sol-gel dip-coating.The capacitance of anodic oxide films formed on coated specimens was at most 80% higher than that without TiO2.In film formation mechanism,it was claimed that the formation of composite oxide film was mainly affected by the structure of micro-pores network in TiO2 coating which had an influence on Al3+ and O2? ions transport during the anodizing.展开更多
Oxide films formed on the surfaces of Fe-based bulk metallic glasses in the temperature range between 373 K and 573 K were characterized and their effects on the corrosion behaviors were investigated by microstructura...Oxide films formed on the surfaces of Fe-based bulk metallic glasses in the temperature range between 373 K and 573 K were characterized and their effects on the corrosion behaviors were investigated by microstructural and electrochemical analysis. The oxide film formed at 573 K is iron-rich oxide and it exhibits an n-type semiconductor at a higher potential than 0.35 V and a p-type semiconductor at a lower potential than 0.35 V. Capacitance measurements show that the donor density decreases with the increase in oxidation temperature, while the thickness of the space charge layer increases with the oxidation temperature rising. The result of immersion tests shows that the mass loss rate increases with the oxidation temperature rising. Therefore, the correlation between microstructure and corrosion resistance needs to be proposed because the corrosion resistance is deteriorated with the development of the oxide films.展开更多
Anodic oxide films grown on titanium alloy Ti-10V-2Fe-3Al in the solution of sodium tartrate, then sealed in boiling deionised water and calcium acetate solution were observed by using field emission scanning electron...Anodic oxide films grown on titanium alloy Ti-10V-2Fe-3Al in the solution of sodium tartrate, then sealed in boiling deionised water and calcium acetate solution were observed by using field emission scanning electron microscopy (FE-SEM), and were chemically analysed by using energy dispersive spectroscopy (EDS). Corrosion behaviour was investigated in a 3.5% sodium chloride solution, using electrochemical impedance spectroscopy (EIS). The morphology of the anodic oxide films was dependent on the sealing processes. The surface sealed in calcium acetate solution presented a more homogeneous and smooth structure compared with that sealed in boiling deionised water. The corrosion resistance of the oxide films sealed in calcium acetate solution was better than that sealed in boiling deionised water.展开更多
The evolution of the surface oxide film along the depth direction of typical aluminum alloy under mediumtemperature brazing was investigated by means of X-ray photoelectron spectroscopy(XPS). For the alloy with Mg con...The evolution of the surface oxide film along the depth direction of typical aluminum alloy under mediumtemperature brazing was investigated by means of X-ray photoelectron spectroscopy(XPS). For the alloy with Mg content below 2.0wt%, whether under cold rolling condition or during medium-temperature brazing process, the enrichment of Mg element on the surface was not detected and the oxide film was pure Al2O3. However, the oxide film grew obviously during medium-temperature brazing process, and the thickness was about 80 nm. For the alloy with Mg content above 2.0wt%, under cold rolling condition, the original surface oxide film was pure Al2O3. However, the Mg element was significantly enriched on the outermost surface during medium-temperature brazing process, and MgO-based oxide film mixed with small amount of MgAl2O4 was formed with a thickness of about 130 nm. The alloying elements of Mn and Si were not enriched on the surface neither under cold rolling condition nor during mediumtemperature brazing process for all the selected aluminum alloy, and the surface oxide film was similar to that of pure aluminum, which was almost entire Al2O3.展开更多
The so-called“Oxide/Metal/Oxide sandwich”method is one of the technique used to investigate the dynamic oxidation of metals which happens during the casting process.In this study,characteristics of the oxide films f...The so-called“Oxide/Metal/Oxide sandwich”method is one of the technique used to investigate the dynamic oxidation of metals which happens during the casting process.In this study,characteristics of the oxide films formed on the molten magnesium in dynamic conditions have been investigated using the aforementioned method.The air bubbles were released into the cast sample at the pressure of 0.2 atm through a quartz tube of 1 mm internal diameter.The interface of two adjacent entrapped bubbles is considered as the Oxide/Metal/Oxide(OMO)sandwich.The sandwiches were characterized by the aid of the optical and scanning electron microscopy and also X-Ray diffraction analyses.Two different approaches,including measuring the width of the folds formed on the oxide films and the edge of the sandwiches,were used to estimate the thickness of the films.The thicknesses were estimated to be in the range of 200 to 800 nm.The features such as fold,wrinkle,and crack were observed on the OMO sandwiches.On the microscopic scale,the oxide films were rough and porous.This is attributed to the non-protective behavior of oxide films.The XRD patterns indicated that the oxide films formed on the pure molten magnesium in dynamic conditions are crystallized MgO.展开更多
The interaction of oxide film with molten flux during aluminum brazing has been studied by means of X-ray powder diffraction. The following conclusions have been deduced: The swell- ing of aluminum oxide film is cause...The interaction of oxide film with molten flux during aluminum brazing has been studied by means of X-ray powder diffraction. The following conclusions have been deduced: The swell- ing of aluminum oxide film is caused by Li^+ inserting into the vacancies of octahedral or tetrahedral structure of 0 atom skeleton in у-Al_2O_3 . The strength of oxide film decreases as the crytallinity increases by the treating of flux containing LiF.展开更多
In this paper, the brazing mechanism of LY12 aluminum alloy at middle range temperature was presented. The CsF-AlF_3 non-corrosive flux was utilized to remove the complex oxide film on the surface of LY12 aluminum all...In this paper, the brazing mechanism of LY12 aluminum alloy at middle range temperature was presented. The CsF-AlF_3 non-corrosive flux was utilized to remove the complex oxide film on the surface of LY12 aluminum alloy. The results revealed that the oxide film was removed by the improved CsF-AlF_3 flux accompanied with the occurrence of reaction as well as dissolution and the compounds CsF played an important role to remove the oxide film. Actually, the high activity of flux, say, the ability to remove the oxide film, was due to the presence of the compounds, such as NH_4F,NH_4AlF_4 and composite molten salt. The production of HF was the key issue to accelerate the reaction and enhance to eliminate the oxide film by dissolution. It was found that the rare earth element La at small percentage was not enriched at the interface. Moreover, the rare earth fluoride enhanced the dissolution behavior.展开更多
Tin oxide(SnO2) and fluorine doped tin oxide(FTO) films were prepared on glass substrates by sol-gel spin-coating using SnCl4 and NH4F precursors.Fluorine doping concentration was fixed at 4 at%and 20 at%by contro...Tin oxide(SnO2) and fluorine doped tin oxide(FTO) films were prepared on glass substrates by sol-gel spin-coating using SnCl4 and NH4F precursors.Fluorine doping concentration was fixed at 4 at%and 20 at%by controlling precursor sol composition.Films exhibited the tetragonal rutile-type crystal structure regardless of fluorine concentration.Uniform and highly transparent FTO films,with more than 85%of optical transmittance,were obtained by annealing at 600℃.Florine doping of films was verified by analyzing the valence band region obtained by XPS.It was found that the fluorine doping affects the shape of valence band of SnO2 films.In addition,it was observed that the band gap of SnO2 is reduced as well as the Fermi level is upward shifted by the effect of fluorine doping.展开更多
Nucleation of Fe-rich intermetallic phases on α-Al2O3 oxide films was analyzed in five experimental Al-Fe-Mn-Si alloys. In an attempt to verify the role of α-Al2O3 films in nucleating Fe-rich intermetallics, experim...Nucleation of Fe-rich intermetallic phases on α-Al2O3 oxide films was analyzed in five experimental Al-Fe-Mn-Si alloys. In an attempt to verify the role of α-Al2O3 films in nucleating Fe-rich intermetallics, experiments have been conducted under conditions where formed in situ oxide films were present. Some Fe-rich intermetallics are observed to be related with the oxide films in the microstructure, the present results are in accordance with some research that suggest that the Fe-rich intermetallic phases nucleate upon the oxide films. The intermetallic phases and α-Al2O3 films were unambiguously identified with the help of complementary techniques such as thermal analysis, SEM/EDS and X-ray diffraction.展开更多
基金Project(51371104)supported by the National Natural Science Foundation of China
文摘Based on A356 aluminum alloy,aluminum foams were prepared by gas injection foaming process with pure nitrogen,air and some gas mixtures.The oxygen volume fraction of these gas mixtures varied from 0.2%to 8.0%.Optical microscopy,scanning electron microscopy(SEM) and Auger electron spectroscopy(AES) were used to analyze the influence of oxygen content on cell structure,relative density,macro and micro morphology of cell walls,coverage area fraction of oxide film,thickness of oxide film and other aspects.Results indicate that the coverage area fraction of oxide film on bubble surface increases with the increase of oxygen content when the oxygen volume is less than 1.2%.While when the oxygen volume fraction is larger than 1.6%,an oxide film covers the entire bubble surface and aluminum foams with good cell structure can be produced.The thicknesses of oxide films of aluminum foams produced by gas mixtures containing 1.6%-21%oxygen are almost the same.The reasons why the thickness of oxide film nearly does not change with the variation of oxygen content and the amount of oxygen needed to achieve 100%coverage of oxide film are both discussed.In addition,the role of oxide film on bubble surface in foam stability is also analyzed.
基金Project(51371104)supported by the National Nature Science Foundation of China
文摘In the range of 620?710 °C, air was blown into A356 aluminum alloy melt to produce aluminum foams. In order to study the influence of temperature on the thickness of oxide film on bubble surface, Auger electron spectroscopy (AES) was used. Based on the knowledge of corrosion science and hydrodynamics, two oxidation kinetics models of oxide film on bubble surface were established. The thicknesses of oxide films produced at different temperatures were predicted through those two models. Furthermore, the theoretical values were compared with the experimental values. The results indicate that in the range of 620?710 °C, the theoretical values of the thickness of oxide film predicted by the model including the rising process are higher than the experimental values. While, the theoretical values predicted by the model without the rising process are in good agreement with the experimental values, which shows this model objectively describes the oxidation process of oxide film on bubble surface. This work suggests that the oxidation kinetics of oxide film on bubble surface of aluminum foams produced by gas injection foaming process follows the Arrhenius equation.
基金The project Supported by National Natural Science Foundation of China.
文摘Electrochromic and auto-bleaching processes at the WO2 anodic film in 0. 5 mol/L H2SO4 solution were investigated by cyclic voltammetry, a. c. impedance technique and photocurrent spectrometry. The colouration mechanism consists of hydrogen adsorption on the WO2 surface and the transport of H atoms in the WO, lattice. The bleaching process involves at least two steps: transport of interstitial H atoms and hydrogen desorption on the W surface, resulting in interstitial H+ ions; then extration of the H+ ions driven by the external electric field. The auto-bleaching arises from the hydroxylation due to both partial interstitial H atoms and a little of water contained in the film.
文摘A study was conducted to develop low-friction, wear-resistant surfaces on high temperature alloys for the temperature range from 26℃ to 900℃. The approach investigated consists of modifying the naturally occurring oxide film in order to improve its tribological properties. Improvement is needed at low temperatures where the oxide film, previously formed at high temperature, spalls due to stresses induced by sliding. Experiments with Ti, W and Ta additions show a beneficial effect when added to Ni and Ni-base alloys. Low friction can be maintained down to 100℃ from 900℃. For unalloyed Ni friction and surface damage increases at 400℃ to 500℃. Two new alloys were perpared based on the beneficial results of binary alloys and ZrO2 diffusion in Ni.Low friction at temperature above 500℃ and reasonable values (0.32~0.42) at low temperature are obtained.
文摘Nano cerium oxide films were applied on AA7020-T6 aluminum alloy and the effects of acetic acid concentration on the microstructure and electrochemical properties of the coated samples were investigated by using scanning electron microscopy (SEM), X-ray diffraction (XRD), and potentiodynamic polarization methods. It has been found that by increasing the acetic acid/CeCl3·7H2O molar ratio, high uniform and crack-free films with well-developed grains were obtained and grain sizes of the films decreased. Elimination of cracks and decreasing grain size of the nano cerium oxide films caused corrosion resistance to increase.
文摘Anodic oxide films of the titanium alloy Ti-10V-2Fe-3Al in ammonium tartrate electrolyte without hydrofluoric acid or fluoride were fabricated. The morphology, components, and microstructure of the films were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results showed that the films were thick, uniform, and nontransparent. Such films exhibited sedimentary morphology, with a thickness of about 3 μm, and the pore diameters of the deposits ranged from several hundred nanometers to 1.5 μm. The films were mainly titanium dioxide. Some coke-like deposits, which may contain or be changed by OH, NH, C-C, C-O, and C=O groups, were doped in the films. The films were mainly amorphous with a small amount of anatase and rutile phase.
基金Project(50571003) supported by the National Natural Science Foundation of China
文摘Porous anodic oxide films were fabricated galvanostatically on titanium alloy Ti-10V-2Fe-3Al in ammonium tartrate solution with different anodizing time.Scanning electron microscopy(SEM) and field emission scanning electron microscopy(FE-SEM) were used to investigate the morphology evolution of the anodic oxide film.It is shown that above the breakdown voltage,oxygen is generated with the occurrence of drums morphology.These drums grow and extrude,which yields the compression stress.Subsequently,microcracks are generated.With continuous anodizing,porous oxides form at the microcracks.Those oxides grow and connect to each other,finally replace the microcrack morphology.The depth profile of the anodic oxide film formed at 1 800 s was examined by Auger electron spectroscopy(AES).It is found that the film is divided into three layers according to the molar fractions of elements.The outer layer is incorporated by carbon,which may come from electrolyte solution.The thickness of the outer layer is approximately 0.2-0.3 μm.The molar fractions of elements in the intermediate layer are extraordinarily stable,while those in the inner layer vary significantly with sputtering depth.The thicknesses of the intermediate layer and the inner layer are 2 μm and 1.0-1.5 μm,respectively.Moreover,the growth mechanism of porous anodic oxide films in neutral tartrate solution was proposed.
基金financially supported by the scientific research project of China Petroleum and Chemical Corporation(No.409075)
文摘The oxidation kinetics,surface morphology and phase structure of oxide films grown on 25Cr20Ni alloy in air-H2O and H2-H2O atmospheres at 900 ℃ for 20 h were investigated.The anti-coking performance and resistance to carburization of the two oxide films were compared using 25Cr20Ni alloy tubes with an inner diameter of 10 mm and a length of 850 mm in a bench scale naphtha steam pyrolysis unit.The oxidation kinetics followed a parabolic law in an air-H2O atmosphere and a logarithm law in a H2-H2O atmosphere in the steady-state stage.The oxide film grown in the air-H2O atmosphere had cracks where the elements Fe and Ni were enriched and the un-cracked area was covered with octahedral-shaped MnCr2O4 spinels and Cr1.3Fe0.7O3 oxide clusters,while the oxide film grown in the H2-H2O atmosphere was intact and completely covered with dense standing blade MnCr2O4 spinels.In the pyrolysis tests,the anti-coking performance and resistance to carburization of the oxide film grown in the H2-H2O atmosphere were far better than that in the air-H2O atmosphere.The mass of coke formed in the oxide film grown in the H2-H2O atmosphere was less than 10% of that in the air-H2O atmosphere.The Cr1.3Fe0.7O3 oxide clusters converted into Cr23C6 carbides and the cracks were filled with carbon in the oxide film grown in the air-H2O atmosphere after repeated coking and decoking tests,while the dense standing blade MnCr2O4 spinels remained unchanged in the oxide film grown in the H2-H2O atmosphere.The ethylene,propylene and butadiene yields in the pyrolysis tests were almost the same for the two oxide films.
基金Project(51375110)supported by the National Natural Science Foundation of Chain
文摘The effect of depressurizing speed on mold filling behavior and entrainment of oxide film of A356 alloy was studied. Themold filling behavior and velocity fields were recorded by water simulation with particle image velocimetry. The results show thatthe gate velocity first increased dramatically, then changed with the depressurizing speed: the gate velocity increased slowly atrelatively high depressurizing speed; at reasonable depressurizing speed, the gate velocity kept unchanged; while at lowerdepressurizing speed, the gate velocity decreased firstly and then kept unchanged. High gate velocity results in melt falling backunder gravity at higher speed. The falling velocity is the main factor of oxide film entrainment in vacuum suction casting. The designcriterion of depressurizing rate was deduced, and the A356 alloy castings were poured to test the formula. The four-point bend testand Weibull probability plots were applied to assessing the fracture mechanisms of the as-cast A356 alloy. The results illuminate amethod on designing suitable depressurizing speed for mold filling in vacuum suction casting.
基金Funded by the National Natural Science Foundation of China(No. 51171011)
文摘The chemical stripping method of titanium alloy oxide films was studied. An environment friendly solution hydrogen peroxide and sodium hydroxide without hydrofluoric acid or fluoride were used to strip the oxide films. The morphologies of the surface and cross-section of the oxide films before and after the films stripping were characterized by using scanning electron microscopy (SEM). The microstructure and chemical compositions of the oxide films before and after the films stripping were investigated by using Raman spectroscopy (Raman) and X-ray photoelectron spectroscopy (XPS). It was shown that the thickness of the oxide film was in the range of 5-6 μm. The oxide films were stripped for 2 to 8 min in the solution. Moreover, the effect of the stripping time on the efficiency of the film stripping was investigated, and the optimum stripping time was between 6-8 min. When the stripping solution completely dissolved the whole film, the α/β microstructure of the titanium alloy Ti-10V-2Fe-3Al was partly revealed. The stripping mechanism was discussed in terms of the dissolution of film delamination. The hydrogen peroxide had a significant effect on the dissolution of the titanium alloy anodic oxide film. The feasibility of the dissolution reaction also was evaluated.
基金financial support from CAS Key Laboratory of Nuclear Materials and Safety Assessment, Institute of Metal Research, Chinese Academy of Sciences。
文摘The evolution of morphology, composition, thickness and corrosion resistance of the oxide film on pure Sn solder substrate submitted to high-temperature aging in 150 °C dry atmosphere was investigated. The results indicate that high-temperature aging accelerates the dehydration of Sn(OH)_(4)in the pre-existing native oxide film to form SnO_(2)and facilitates the oxidation of fresh Sn substrate, resulting in the gradual increase in oxide film thickness and surface roughness with prolonging aging time. However, the corrosion resistance of the film initially is enhanced and then deteriorated with an extending aging time. Besides, the formation and evolution mechanisms of the oxide film with aging time were discussed.
文摘Al specimens were covered with TiO2 film by sol-gel dip-coating and then anodized in ammonium adipate solution.The structure,composition and capacitance properties of the anodic oxide film were investigated by transmission electron microscopy (TEM),Auger electron spectroscopy (AES),X-ray diffractometry (XRD) and electrochemical impedance spectroscopy (EIS).It was found that an anodic oxide film with a dual-layer structure formed between TiO2 coating and Al substrate.The film consisted of an inner Al2O3 layer and an outer Ti-Al composite oxide layer.The thickness of layers varied with the number of times of sol-gel dip-coating.The capacitance of anodic oxide films formed on coated specimens was at most 80% higher than that without TiO2.In film formation mechanism,it was claimed that the formation of composite oxide film was mainly affected by the structure of micro-pores network in TiO2 coating which had an influence on Al3+ and O2? ions transport during the anodizing.
基金supported by the National Natural Science Foundation of China (No.51165038)the Doctoral Startup Fund of Nanchang Hangkong University (No.EA201103238)the Korean Ministry of Commerce, Industry and Energy through the project entitled as "The Development of Structural Metallic Materials and Parts with Super Strength and High Performance"
文摘Oxide films formed on the surfaces of Fe-based bulk metallic glasses in the temperature range between 373 K and 573 K were characterized and their effects on the corrosion behaviors were investigated by microstructural and electrochemical analysis. The oxide film formed at 573 K is iron-rich oxide and it exhibits an n-type semiconductor at a higher potential than 0.35 V and a p-type semiconductor at a lower potential than 0.35 V. Capacitance measurements show that the donor density decreases with the increase in oxidation temperature, while the thickness of the space charge layer increases with the oxidation temperature rising. The result of immersion tests shows that the mass loss rate increases with the oxidation temperature rising. Therefore, the correlation between microstructure and corrosion resistance needs to be proposed because the corrosion resistance is deteriorated with the development of the oxide films.
基金Supported by the National Natural Science Foundation of China(No.51271012)
文摘Anodic oxide films grown on titanium alloy Ti-10V-2Fe-3Al in the solution of sodium tartrate, then sealed in boiling deionised water and calcium acetate solution were observed by using field emission scanning electron microscopy (FE-SEM), and were chemically analysed by using energy dispersive spectroscopy (EDS). Corrosion behaviour was investigated in a 3.5% sodium chloride solution, using electrochemical impedance spectroscopy (EIS). The morphology of the anodic oxide films was dependent on the sealing processes. The surface sealed in calcium acetate solution presented a more homogeneous and smooth structure compared with that sealed in boiling deionised water. The corrosion resistance of the oxide films sealed in calcium acetate solution was better than that sealed in boiling deionised water.
基金Supported by National Natural Science Foundation of China(No.51005163 and No.51275351)Scientific Research Foundation for the Returned Overseas Chinese Scholars,Ministry of Education of China
文摘The evolution of the surface oxide film along the depth direction of typical aluminum alloy under mediumtemperature brazing was investigated by means of X-ray photoelectron spectroscopy(XPS). For the alloy with Mg content below 2.0wt%, whether under cold rolling condition or during medium-temperature brazing process, the enrichment of Mg element on the surface was not detected and the oxide film was pure Al2O3. However, the oxide film grew obviously during medium-temperature brazing process, and the thickness was about 80 nm. For the alloy with Mg content above 2.0wt%, under cold rolling condition, the original surface oxide film was pure Al2O3. However, the Mg element was significantly enriched on the outermost surface during medium-temperature brazing process, and MgO-based oxide film mixed with small amount of MgAl2O4 was formed with a thickness of about 130 nm. The alloying elements of Mn and Si were not enriched on the surface neither under cold rolling condition nor during mediumtemperature brazing process for all the selected aluminum alloy, and the surface oxide film was similar to that of pure aluminum, which was almost entire Al2O3.
文摘The so-called“Oxide/Metal/Oxide sandwich”method is one of the technique used to investigate the dynamic oxidation of metals which happens during the casting process.In this study,characteristics of the oxide films formed on the molten magnesium in dynamic conditions have been investigated using the aforementioned method.The air bubbles were released into the cast sample at the pressure of 0.2 atm through a quartz tube of 1 mm internal diameter.The interface of two adjacent entrapped bubbles is considered as the Oxide/Metal/Oxide(OMO)sandwich.The sandwiches were characterized by the aid of the optical and scanning electron microscopy and also X-Ray diffraction analyses.Two different approaches,including measuring the width of the folds formed on the oxide films and the edge of the sandwiches,were used to estimate the thickness of the films.The thicknesses were estimated to be in the range of 200 to 800 nm.The features such as fold,wrinkle,and crack were observed on the OMO sandwiches.On the microscopic scale,the oxide films were rough and porous.This is attributed to the non-protective behavior of oxide films.The XRD patterns indicated that the oxide films formed on the pure molten magnesium in dynamic conditions are crystallized MgO.
文摘The interaction of oxide film with molten flux during aluminum brazing has been studied by means of X-ray powder diffraction. The following conclusions have been deduced: The swell- ing of aluminum oxide film is caused by Li^+ inserting into the vacancies of octahedral or tetrahedral structure of 0 atom skeleton in у-Al_2O_3 . The strength of oxide film decreases as the crytallinity increases by the treating of flux containing LiF.
文摘In this paper, the brazing mechanism of LY12 aluminum alloy at middle range temperature was presented. The CsF-AlF_3 non-corrosive flux was utilized to remove the complex oxide film on the surface of LY12 aluminum alloy. The results revealed that the oxide film was removed by the improved CsF-AlF_3 flux accompanied with the occurrence of reaction as well as dissolution and the compounds CsF played an important role to remove the oxide film. Actually, the high activity of flux, say, the ability to remove the oxide film, was due to the presence of the compounds, such as NH_4F,NH_4AlF_4 and composite molten salt. The production of HF was the key issue to accelerate the reaction and enhance to eliminate the oxide film by dissolution. It was found that the rare earth element La at small percentage was not enriched at the interface. Moreover, the rare earth fluoride enhanced the dissolution behavior.
文摘Tin oxide(SnO2) and fluorine doped tin oxide(FTO) films were prepared on glass substrates by sol-gel spin-coating using SnCl4 and NH4F precursors.Fluorine doping concentration was fixed at 4 at%and 20 at%by controlling precursor sol composition.Films exhibited the tetragonal rutile-type crystal structure regardless of fluorine concentration.Uniform and highly transparent FTO films,with more than 85%of optical transmittance,were obtained by annealing at 600℃.Florine doping of films was verified by analyzing the valence band region obtained by XPS.It was found that the fluorine doping affects the shape of valence band of SnO2 films.In addition,it was observed that the band gap of SnO2 is reduced as well as the Fermi level is upward shifted by the effect of fluorine doping.
基金the National Council for Science and Technology of Mexico(Conacyt)for the financial support provided to carry out this work(Project No.149030).
文摘Nucleation of Fe-rich intermetallic phases on α-Al2O3 oxide films was analyzed in five experimental Al-Fe-Mn-Si alloys. In an attempt to verify the role of α-Al2O3 films in nucleating Fe-rich intermetallics, experiments have been conducted under conditions where formed in situ oxide films were present. Some Fe-rich intermetallics are observed to be related with the oxide films in the microstructure, the present results are in accordance with some research that suggest that the Fe-rich intermetallic phases nucleate upon the oxide films. The intermetallic phases and α-Al2O3 films were unambiguously identified with the help of complementary techniques such as thermal analysis, SEM/EDS and X-ray diffraction.