The microstructure and corrosion resistance of different boric/sulfuric acid anodic（BSAA） films on 7050 aluminum alloy were studied by atomic force microscopy（AFM）,electrochemical impedance spectroscopy（EIS） and...The microstructure and corrosion resistance of different boric/sulfuric acid anodic（BSAA） films on 7050 aluminum alloy were studied by atomic force microscopy（AFM）,electrochemical impedance spectroscopy（EIS） and scanning Kelvin probe（SKP）.The results show that boric acid does not change the structure of barrier layer of anodic film,but will significantly affect the structure of porous layer,consequently affect the corrosion resistance of anodic film.As the content of boric acid in electrolyte increases from 0 to 8 g/L,the resistance of porous layer（Rp） of BSAA film increases,the capacitance of porous layer（CPEp） decreases,the surface potential moves positively,the pore size lessens,and the corrosion resistance improves.However,the Rp,CPEp and surface potential will change towards opposite direction when the content of boric acid is over 8 g/L.展开更多
The special experimental device and sulfuric acid electrolyte were adopted to study the influence of anodic oxidation heat on hard anodic film for 2024 aluminum alloy. Compared with the oxidation heat transferred to t...The special experimental device and sulfuric acid electrolyte were adopted to study the influence of anodic oxidation heat on hard anodic film for 2024 aluminum alloy. Compared with the oxidation heat transferred to the electrolyte through anodic film, the heat transferred to the coolant through aluminum substrate is more beneficial to the growth of anodic film. The film forming speed, film thickness, density and hardness are significantly increased as the degree of undercooling of the coolant increases. The degree of undercooling of the coolant, which is necessary for the growth of anodic film, is related to the degree of undercooling of the electrolyte, thickness of aluminum substrate, thickness of anodic film, natural parameters of bubble covering and current density. The microstructure and performance of the oxidation film could be controlled by the temperature of the coolant.展开更多
Anodization of AZ91D magnesium alloy in the electrolyte solution of 0.5 mol/L of sodium silicate and 1.0 mol/L of potassium fluoride was investigated. The anodic films were characterized using optical microscopy （OM...Anodization of AZ91D magnesium alloy in the electrolyte solution of 0.5 mol/L of sodium silicate and 1.0 mol/L of potassium fluoride was investigated. The anodic films were characterized using optical microscopy （OM）, scanning electron microscopy （SEM）, and X-ray diffraction （XRD）. The corrosion resistance of the various anodized alloys was evaluated by a fast corrosion test using the solution of hydrochloric acid and potassium dichromate. The results showed that the addition of KF resulted in the presence of NaF in the anodic film. The thickness of the anodic film formed under a constant current density of 20 mA/cm^2 for 16 rain at 60℃ exceeded 100 gm. The growth of the anodic film could be divided into three stages based on the anodizing time; the growth rate was much faster during stage Ⅱ than in stages I and Ⅲ. The anodic film exhibited the highest corrosion resistance for the AZ91 alloy, which is attributed to the fact that the anodization was maintained until the end of stage Ⅱ.展开更多
Ni element was introduced to aluminum surface by a simple chemical immersion method, and A1-Ni composite anodic films were obtained by following anodizing. The morphology, structure and composition of the A1-Ni anodic...Ni element was introduced to aluminum surface by a simple chemical immersion method, and A1-Ni composite anodic films were obtained by following anodizing. The morphology, structure and composition of the A1-Ni anodic films were examined by scanning electron microscopy （SEM）, energy disperse spectroscopy （EDS） and atomic force microscopy（AFM）. The electrochemical behaviors of the films were studied by means of polarization measurement and electrochemical impedance spectroscopy （EIS）. The experimental results show that the A1-Ni composite anodic film is more compact with smaller pore diameters than that of the A1 anodic film. The introduction of nickel increases the impedances of both the barrier layer and the porous layer of the anodic films. In NaC1 solutions, the A1-Ni composite anodic films show higher impedance values and better corrosion resistance.展开更多
The good potentiality of the In_2O_3 anodic film as a photoanodic material has been demonstrated.The anodic oxidation of In substrate in alkaline solution for obtaining In_2O_3 film has been developed and their semico...The good potentiality of the In_2O_3 anodic film as a photoanodic material has been demonstrated.The anodic oxidation of In substrate in alkaline solution for obtaining In_2O_3 film has been developed and their semiconducting properties have been investigated through capacitance, photoelectrochemistry and electroreflection measurements.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
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
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
The morphology and structure of the oxide films of Ti in H3PO4 were investigated by galvanos tatic anodization, SEM and XRD. The oxide film grew from some pores in the grooves to layered microdomains as increasing ano...The morphology and structure of the oxide films of Ti in H3PO4 were investigated by galvanos tatic anodization, SEM and XRD. The oxide film grew from some pores in the grooves to layered microdomains as increasing anodizing voltage. The crystallinity of the oxide films decreased with the increase of the concentration of the electrolyte. The model has been proposed for the growth of the oxide films by two steps, i.e. by uniform thickening and by local deposition.展开更多
The effect of fluoride ions on the formation and dissolution behaviour of anodic oxide films on Ti has been investigated in acidic fluoride media (pH=1) using impedance and galvanostatic techniques. A5 the fluoride io...The effect of fluoride ions on the formation and dissolution behaviour of anodic oxide films on Ti has been investigated in acidic fluoride media (pH=1) using impedance and galvanostatic techniques. A5 the fluoride ion concentration and temperature increase the rate of oxide film formation decreases while the dissolution process increases. oxide film formed at high tem-perature and formation voltage was found to contain more defect sites in the film than that formed at a lower one. Activation energies are calculated during the oxide film formation and dissolution and found to be 20.76 and 28.72 kJ/mol, respectively. Formation rate and reciprocal capacitance data are reported as a function of polarizing current density. Values are recorded for the electrolytic parameters A and B. Potentiostatic curves are derived from the galvanostatic results.展开更多
Aluminum capacitor foils with a tunnel etch structure were reacted with boiling water and then anodized at 530 V in boric acid solution or boric acid＋citric acid mixed solution.The microstructure and crystallinity of...Aluminum capacitor foils with a tunnel etch structure were reacted with boiling water and then anodized at 530 V in boric acid solution or boric acid＋citric acid mixed solution.The microstructure and crystallinity of the resulting anodized film were examined by TEM and XRD.The special capacitance,resistance and withstanding voltage of the film were explored with electrochemical impedance spectroscopy（EIS）,LCR meter and small-current charging.The results show that the high voltage anodized oxide film consists of an inner layer with high crystallinity and an outer layer with low crystallinity.However,the crystallinity of the film formed in boric acid＋citric acid mixed solution is higher than that of the film formed in only boric acid solution,leading to an increase in film＇s field strength and special capacitance.Meanwhile,there are more defects from phase transformation in the out layer of the film formed in boric acid＋citric acid mixed solution than in that of film formed in only boric acid solution,leading to a decrease in film＇s resistance and withstanding voltage.展开更多
The anodic films of novel Pb-Ca-Sn-Ce alloy, traditional Pb-Ca-Sn and Pb-Sb alloys formed in sulfuric solution at anodic +0.9 V potential corrosion for 6 h were investigated by means of XPS, XRD methods and AC impedan...The anodic films of novel Pb-Ca-Sn-Ce alloy, traditional Pb-Ca-Sn and Pb-Sb alloys formed in sulfuric solution at anodic +0.9 V potential corrosion for 6 h were investigated by means of XPS, XRD methods and AC impedance measurement. The results show that the growth of Pb(Ⅱ) oxide on the new Pb-Ca-Sn-Ce alloy surface is inhibited. The AC impedance measurement shows that resistance of the corrosion layer of novel Pb-Ca-Sn-Ce alloy decreases. It is found that the novel Pb-Ca-Sn-Ce alloy can encourage the development of PbO2 in the scale, and enhance the conductivity of the anodic scale. Hence the deep recycling properties of the battery can be expected better.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
The change of conductivity, thickness and scanning electron microscopy （SEM） appearance of the anode film of CrWMn in 10% NaNO3 at different anode potential either with or without the magnetic field applied are inve...The change of conductivity, thickness and scanning electron microscopy （SEM） appearance of the anode film of CrWMn in 10% NaNO3 at different anode potential either with or without the magnetic field applied are investigated by testing film resistance, galvanostatic transient and using SEM to design magnetic circuit in magnetic assisted electrochemical machining （MAECM）. The experiments show that the anode film has semi-conducting property. Compared with the situation without magnetic field applied, the resistance of the film formed at 1 .SV （anode potential） increased and decreased at 4.0V while B=0.4T and the magnetic north pole points toward anode. The SEM photo demonstrates that the magnetic field will densify the film in the passivation area and quicken dissolution of the anode metal in over-passivation area. Based on the influence of magnetic field on electrochemical machining（ECM） due to the changes of the anode film conductivity behavior, the magnetic north pole should be designed to point towards the workpiece surface that has been machined. Process experiments agree with the results of test analysis.展开更多
Anodized composite films containing Si C nanoparticles were synthesized on Ti6Al4 V alloy by anodic oxidation procedure in C4O6H4Na2 electrolyte. Scanning electron microscopy(SEM), energy dispersive spectroscopy(EDS) ...Anodized composite films containing Si C nanoparticles were synthesized on Ti6Al4 V alloy by anodic oxidation procedure in C4O6H4Na2 electrolyte. Scanning electron microscopy(SEM), energy dispersive spectroscopy(EDS) and X-ray photoelectron spectroscopy(XPS) were employed to characterize the morphology and composition of the films fabricated in the electrolytes with and without addition of Si C nanoparticles. Results show that Si C particles can be successfully incorporated into the oxide film during the anodizing process and preferentially concentrate within internal cavities and micro-cracks. The ball-on-disk sliding tests indicate that Si C-containing oxide films register much lower wear rate than the oxide films without Si C under dry sliding condition. Si C particles are likely to melt and then are oxidized by frictional heat during sliding tests. Potentiodynamic polarization behavior reveals that the anodized alloy with Si C nanoparticles results in a reduction in passive current density to about 1.54×10-8 A/cm2, which is more than two times lower than that of the Ti O2 film(3.73×10-8 A/cm2). The synthesized composite film has good anti-wear and anti-corrosion properties and the growth mechanism of nanocomposite film is also discussed.展开更多
Different additives were added into the potassium fluorozirconate solution to prepare different nickelfree sealing reagents,with which the anodic oxidation film of aluminum alloy was sealed at room temperature.The pho...Different additives were added into the potassium fluorozirconate solution to prepare different nickelfree sealing reagents,with which the anodic oxidation film of aluminum alloy was sealed at room temperature.The phosphor chromic acid weight loss method was used to evaluate the sealing effects.Using electron scanning microscopy(SEM),the surface and cross-sectional micromorphologies of the anodic oxidation films sealed by different fluorozirconate sealants were observed.The position and state of zirconium element distribution in the film hole were investigated by the further quantitative and distribution analysis of Zr element.This study provides an experimental evidence for the theoretical studies of fluorozirconate-sealed anodic oxidation films.It is shown that the fluorozirconate has good sealing effects and has a wide prospect for sealing the aluminum alloy samples.Its products were highly corrosion resistant,and were filled in the openings of the micropores in the oxide film.展开更多
A thick composite anodic oxide film was fabricated in an environmentally friendly malic acid electrolyte containing Poly Tetra Fluoro Ethylene(PTFE)nanoparticles on Ti-10V-2Fe-3Al alloys.The influence of pulse frequen...A thick composite anodic oxide film was fabricated in an environmentally friendly malic acid electrolyte containing Poly Tetra Fluoro Ethylene(PTFE)nanoparticles on Ti-10V-2Fe-3Al alloys.The influence of pulse frequency on the morphology,microstructure and composition of composite anodic oxide films containing PTFE nanoparticles was investigated using Field Emission Scanning Electron Microscopy(FE-SEM)equipped with Energy Dispersive Spectroscopy(EDS),Atomic Force Microscopy(AFM)and Raman spectroscopy.The tribological properties in terms of the friction coefficient,wear loss and morphology of worn surfaces were measured by ball-ondisc tests.The electrochemical property was evaluated by potentiodynamic polarization.The results indicated that the titanium dioxide of composite anodic oxide films transformed from anatase to rutile with the change of pulse frequency,which could result from the electrochemical dynamic equilibrium.The combination of PTFE nanoparticles and malic acid electrolyte molecules can influence the energy fluctuation of electrochemical equilibrium and formation of composite anodic oxide films.Moreover,composite anodic oxide films fabricated under the condition of 1.0–2.0 Hz exhibited the best wear resistance and corrosion property.The schematic diagram of the film formation and PTFE nanoparticles spreading process under different frequencies was elucidated.展开更多
The effects of samarium on the properties of the anodic Pb(II) oxides films formed on lead at 0 9 V (vs. Hg/Hg 2SO 4) in 4 5 mol/L H 2SO 4 solution were studied using linear sweep voltammetry (LSV), electrochemi...The effects of samarium on the properties of the anodic Pb(II) oxides films formed on lead at 0 9 V (vs. Hg/Hg 2SO 4) in 4 5 mol/L H 2SO 4 solution were studied using linear sweep voltammetry (LSV), electrochemical impedance spectroscopy (EIS) and scanning electron micrographs (SEM). The experimental results show that adding Sm to lead metal can inhibit the growth of the Pb(II) oxides film effectively, and reduce the resistance of the PbO oxides film obviously. The addition of Sm increases the porosity of the anodic film, which may cause the increase of the ionic conductance produced by the interstitial liquid among the PbO particles in the film and lead to the decrease of the resistance of the anodic film.展开更多
In the present study, 2024 aluminum alloy specimen was anodized in acetic acid and oxalic acid e- lectrolytes. Effects of the current density on the microstructure and corrosion resistance of anodic oxide film have be...In the present study, 2024 aluminum alloy specimen was anodized in acetic acid and oxalic acid e- lectrolytes. Effects of the current density on the microstructure and corrosion resistance of anodic oxide film have been investigated. The steady voltage increases from 11 V to 71 V with the current density increase from 0. 5 A/din2 to 2. 5 A/din2. The SEM reveals that there are pits, cavities and irregular pores in the anodic film, and their size and morphologies change with the current density. The corrosion resistance of the film was evalua- ted by potentiodynamic polarization and electrochemical impedance in 0.1 mol/L FeC13 solution at room temper- ature. The results show that corrosion resistance of the anodic oxide film changes with the current density, and the anodic fihn formed at the current density of 1.0 A/dm2 has the best corrosion resistance. These observations indicate that anodic film formed at J -- 1.0 A/dm2can serve as a support material for the Cu micrometallic pat-展开更多
文摘The microstructure and corrosion resistance of different boric/sulfuric acid anodic（BSAA） films on 7050 aluminum alloy were studied by atomic force microscopy（AFM）,electrochemical impedance spectroscopy（EIS） and scanning Kelvin probe（SKP）.The results show that boric acid does not change the structure of barrier layer of anodic film,but will significantly affect the structure of porous layer,consequently affect the corrosion resistance of anodic film.As the content of boric acid in electrolyte increases from 0 to 8 g/L,the resistance of porous layer（Rp） of BSAA film increases,the capacitance of porous layer（CPEp） decreases,the surface potential moves positively,the pore size lessens,and the corrosion resistance improves.However,the Rp,CPEp and surface potential will change towards opposite direction when the content of boric acid is over 8 g/L.
基金Project (SBZDPY-11-17) supported by the Fund on Key Laboratory Project for Hydrodynamic Force, Ministry of Education, China Project (SZD0502-09-0) supported by Key Disciplines of Materials Processing Engineering of Sichuan Province, China
文摘The special experimental device and sulfuric acid electrolyte were adopted to study the influence of anodic oxidation heat on hard anodic film for 2024 aluminum alloy. Compared with the oxidation heat transferred to the electrolyte through anodic film, the heat transferred to the coolant through aluminum substrate is more beneficial to the growth of anodic film. The film forming speed, film thickness, density and hardness are significantly increased as the degree of undercooling of the coolant increases. The degree of undercooling of the coolant, which is necessary for the growth of anodic film, is related to the degree of undercooling of the electrolyte, thickness of aluminum substrate, thickness of anodic film, natural parameters of bubble covering and current density. The microstructure and performance of the oxidation film could be controlled by the temperature of the coolant.
基金The work was financially supported by the National Natural Science Foundation of China (No.50541003) and the Aeronautic ScienceFoundation of China (No.04H51002).
文摘Anodization of AZ91D magnesium alloy in the electrolyte solution of 0.5 mol/L of sodium silicate and 1.0 mol/L of potassium fluoride was investigated. The anodic films were characterized using optical microscopy （OM）, scanning electron microscopy （SEM）, and X-ray diffraction （XRD）. The corrosion resistance of the various anodized alloys was evaluated by a fast corrosion test using the solution of hydrochloric acid and potassium dichromate. The results showed that the addition of KF resulted in the presence of NaF in the anodic film. The thickness of the anodic film formed under a constant current density of 20 mA/cm^2 for 16 rain at 60℃ exceeded 100 gm. The growth of the anodic film could be divided into three stages based on the anodizing time; the growth rate was much faster during stage Ⅱ than in stages I and Ⅲ. The anodic film exhibited the highest corrosion resistance for the AZ91 alloy, which is attributed to the fact that the anodization was maintained until the end of stage Ⅱ.
基金Funded by the National Natural Science Foundation of China (No.50571006)the Key Project of Science and Technology of Ministry of Education of China (No.108129)
文摘Ni element was introduced to aluminum surface by a simple chemical immersion method, and A1-Ni composite anodic films were obtained by following anodizing. The morphology, structure and composition of the A1-Ni anodic films were examined by scanning electron microscopy （SEM）, energy disperse spectroscopy （EDS） and atomic force microscopy（AFM）. The electrochemical behaviors of the films were studied by means of polarization measurement and electrochemical impedance spectroscopy （EIS）. The experimental results show that the A1-Ni composite anodic film is more compact with smaller pore diameters than that of the A1 anodic film. The introduction of nickel increases the impedances of both the barrier layer and the porous layer of the anodic films. In NaC1 solutions, the A1-Ni composite anodic films show higher impedance values and better corrosion resistance.
文摘The good potentiality of the In_2O_3 anodic film as a photoanodic material has been demonstrated.The anodic oxidation of In substrate in alkaline solution for obtaining In_2O_3 film has been developed and their semiconducting properties have been investigated through capacitance, photoelectrochemistry and electroreflection measurements.
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.
基金This work was supported by. tile grant uf Post-Doc.Program, Kylingpook National tjllivcrsity (if)IN)
文摘The morphology and structure of the oxide films of Ti in H3PO4 were investigated by galvanos tatic anodization, SEM and XRD. The oxide film grew from some pores in the grooves to layered microdomains as increasing anodizing voltage. The crystallinity of the oxide films decreased with the increase of the concentration of the electrolyte. The model has been proposed for the growth of the oxide films by two steps, i.e. by uniform thickening and by local deposition.
文摘The effect of fluoride ions on the formation and dissolution behaviour of anodic oxide films on Ti has been investigated in acidic fluoride media (pH=1) using impedance and galvanostatic techniques. A5 the fluoride ion concentration and temperature increase the rate of oxide film formation decreases while the dissolution process increases. oxide film formed at high tem-perature and formation voltage was found to contain more defect sites in the film than that formed at a lower one. Activation energies are calculated during the oxide film formation and dissolution and found to be 20.76 and 28.72 kJ/mol, respectively. Formation rate and reciprocal capacitance data are reported as a function of polarizing current density. Values are recorded for the electrolytic parameters A and B. Potentiostatic curves are derived from the galvanostatic results.
基金Project supported by University New Materials Disciplines Construction Program of Beijing Region
文摘Aluminum capacitor foils with a tunnel etch structure were reacted with boiling water and then anodized at 530 V in boric acid solution or boric acid＋citric acid mixed solution.The microstructure and crystallinity of the resulting anodized film were examined by TEM and XRD.The special capacitance,resistance and withstanding voltage of the film were explored with electrochemical impedance spectroscopy（EIS）,LCR meter and small-current charging.The results show that the high voltage anodized oxide film consists of an inner layer with high crystallinity and an outer layer with low crystallinity.However,the crystallinity of the film formed in boric acid＋citric acid mixed solution is higher than that of the film formed in only boric acid solution,leading to an increase in film＇s field strength and special capacitance.Meanwhile,there are more defects from phase transformation in the out layer of the film formed in boric acid＋citric acid mixed solution than in that of film formed in only boric acid solution,leading to a decrease in film＇s resistance and withstanding voltage.
文摘The anodic films of novel Pb-Ca-Sn-Ce alloy, traditional Pb-Ca-Sn and Pb-Sb alloys formed in sulfuric solution at anodic +0.9 V potential corrosion for 6 h were investigated by means of XPS, XRD methods and AC impedance measurement. The results show that the growth of Pb(Ⅱ) oxide on the new Pb-Ca-Sn-Ce alloy surface is inhibited. The AC impedance measurement shows that resistance of the corrosion layer of novel Pb-Ca-Sn-Ce alloy decreases. It is found that the novel Pb-Ca-Sn-Ce alloy can encourage the development of PbO2 in the scale, and enhance the conductivity of the anodic scale. Hence the deep recycling properties of the battery can be expected better.
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National Defense Foundation of China (No.51318030401).
文摘The change of conductivity, thickness and scanning electron microscopy （SEM） appearance of the anode film of CrWMn in 10% NaNO3 at different anode potential either with or without the magnetic field applied are investigated by testing film resistance, galvanostatic transient and using SEM to design magnetic circuit in magnetic assisted electrochemical machining （MAECM）. The experiments show that the anode film has semi-conducting property. Compared with the situation without magnetic field applied, the resistance of the film formed at 1 .SV （anode potential） increased and decreased at 4.0V while B=0.4T and the magnetic north pole points toward anode. The SEM photo demonstrates that the magnetic field will densify the film in the passivation area and quicken dissolution of the anode metal in over-passivation area. Based on the influence of magnetic field on electrochemical machining（ECM） due to the changes of the anode film conductivity behavior, the magnetic north pole should be designed to point towards the workpiece surface that has been machined. Process experiments agree with the results of test analysis.
基金Project(51271012)supported by the National Natural Science Foundation of China
文摘Anodized composite films containing Si C nanoparticles were synthesized on Ti6Al4 V alloy by anodic oxidation procedure in C4O6H4Na2 electrolyte. Scanning electron microscopy(SEM), energy dispersive spectroscopy(EDS) and X-ray photoelectron spectroscopy(XPS) were employed to characterize the morphology and composition of the films fabricated in the electrolytes with and without addition of Si C nanoparticles. Results show that Si C particles can be successfully incorporated into the oxide film during the anodizing process and preferentially concentrate within internal cavities and micro-cracks. The ball-on-disk sliding tests indicate that Si C-containing oxide films register much lower wear rate than the oxide films without Si C under dry sliding condition. Si C particles are likely to melt and then are oxidized by frictional heat during sliding tests. Potentiodynamic polarization behavior reveals that the anodized alloy with Si C nanoparticles results in a reduction in passive current density to about 1.54×10-8 A/cm2, which is more than two times lower than that of the Ti O2 film(3.73×10-8 A/cm2). The synthesized composite film has good anti-wear and anti-corrosion properties and the growth mechanism of nanocomposite film is also discussed.
基金financially supported by the National New Material Testing and Evaluation Platform Main Center Project(No.TC170A5SU-1)。
文摘Different additives were added into the potassium fluorozirconate solution to prepare different nickelfree sealing reagents,with which the anodic oxidation film of aluminum alloy was sealed at room temperature.The phosphor chromic acid weight loss method was used to evaluate the sealing effects.Using electron scanning microscopy(SEM),the surface and cross-sectional micromorphologies of the anodic oxidation films sealed by different fluorozirconate sealants were observed.The position and state of zirconium element distribution in the film hole were investigated by the further quantitative and distribution analysis of Zr element.This study provides an experimental evidence for the theoretical studies of fluorozirconate-sealed anodic oxidation films.It is shown that the fluorozirconate has good sealing effects and has a wide prospect for sealing the aluminum alloy samples.Its products were highly corrosion resistant,and were filled in the openings of the micropores in the oxide film.
基金co-supported by the National Natural Science Foundation of China(Nos.51971040 and 51971044)the Fundamental Research Funds for the Central Universities,China(2020CDJQY-A007)+1 种基金China Postdoctoral Science Foundation Funded Project(Nos.2017M620410 and 2018T110942)the Chongqing Postdoctoral Scientific Research Foundation(No.Xm2017010)。
文摘A thick composite anodic oxide film was fabricated in an environmentally friendly malic acid electrolyte containing Poly Tetra Fluoro Ethylene(PTFE)nanoparticles on Ti-10V-2Fe-3Al alloys.The influence of pulse frequency on the morphology,microstructure and composition of composite anodic oxide films containing PTFE nanoparticles was investigated using Field Emission Scanning Electron Microscopy(FE-SEM)equipped with Energy Dispersive Spectroscopy(EDS),Atomic Force Microscopy(AFM)and Raman spectroscopy.The tribological properties in terms of the friction coefficient,wear loss and morphology of worn surfaces were measured by ball-ondisc tests.The electrochemical property was evaluated by potentiodynamic polarization.The results indicated that the titanium dioxide of composite anodic oxide films transformed from anatase to rutile with the change of pulse frequency,which could result from the electrochemical dynamic equilibrium.The combination of PTFE nanoparticles and malic acid electrolyte molecules can influence the energy fluctuation of electrochemical equilibrium and formation of composite anodic oxide films.Moreover,composite anodic oxide films fabricated under the condition of 1.0–2.0 Hz exhibited the best wear resistance and corrosion property.The schematic diagram of the film formation and PTFE nanoparticles spreading process under different frequencies was elucidated.
文摘The effects of samarium on the properties of the anodic Pb(II) oxides films formed on lead at 0 9 V (vs. Hg/Hg 2SO 4) in 4 5 mol/L H 2SO 4 solution were studied using linear sweep voltammetry (LSV), electrochemical impedance spectroscopy (EIS) and scanning electron micrographs (SEM). The experimental results show that adding Sm to lead metal can inhibit the growth of the Pb(II) oxides film effectively, and reduce the resistance of the PbO oxides film obviously. The addition of Sm increases the porosity of the anodic film, which may cause the increase of the ionic conductance produced by the interstitial liquid among the PbO particles in the film and lead to the decrease of the resistance of the anodic film.
基金Sponsored by the National Natural Science Foundation of China (Grant No. 60971020)
文摘In the present study, 2024 aluminum alloy specimen was anodized in acetic acid and oxalic acid e- lectrolytes. Effects of the current density on the microstructure and corrosion resistance of anodic oxide film have been investigated. The steady voltage increases from 11 V to 71 V with the current density increase from 0. 5 A/din2 to 2. 5 A/din2. The SEM reveals that there are pits, cavities and irregular pores in the anodic film, and their size and morphologies change with the current density. The corrosion resistance of the film was evalua- ted by potentiodynamic polarization and electrochemical impedance in 0.1 mol/L FeC13 solution at room temper- ature. The results show that corrosion resistance of the anodic oxide film changes with the current density, and the anodic fihn formed at the current density of 1.0 A/dm2 has the best corrosion resistance. These observations indicate that anodic film formed at J -- 1.0 A/dm2can serve as a support material for the Cu micrometallic pat-
