Fabrication and characterization of anodic oxide films on a Ti-10V-2Fe-3Al titanium alloy

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.

Morphology and growth of porous anodic oxide films on Ti-10V-2Fe-3Al in neutral tartrate solution

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.

EIS Characterization of Sealed Anodic Oxide Films on Titanium Alloy Ti-10V-2Fe-3Al

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.

WO_3 Anodic Oxide Film——I.Electrochromism and Auto-bleaching mechanism

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.

Formation and Morphology of Anodic Oxide Films of Ti

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.

Macroscopic Studies on the Properties of the Anodic Oxide Films on Titanium

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.

Effects of acetic acid on microstructure and electrochemical properties of nano cerium oxide films coated on AA7020-T6 aluminum alloy

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.

INTERACTION OF OXIDE FILM WITH MOLTEN FLUX DURING ALUMINUM BRAZING

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.

Formation and capacitance properties of Ti-Al composite oxide film on aluminum

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.

Effects of the Annealing Heating Rate on Sputtered Aluminum Oxide Films

AlxOy films by DC reactive magnetron sputtering were annealed in air ambient at 500 ℃for 1 h with different heating rates of 5,15,and 25 ℃/min.Then heat treatments at 900 ℃ were carried out on these 500 ℃-annealed films to simulate the high-temperature application environment.Effects of the annealing heating rate on structure and properties of both 500 ℃-annealed and 900 ℃-heated films were investigated systematically.It was found that distinct γ-Al2O3 crystallization was observed in the 900 ℃-heated films only when the annealing heating rates are 15 and 25 ℃/min.The 500 ℃-annealed film possessed the most compact surface morphology in the case of 25 ℃/min.The highest microhardness of both 500 ℃-annealed and 900℃-heated films were obtained when the annealing heating rate was 15 ℃/min.

Oxidation kinetics of oxide film on bubble surface of aluminum foams produced by gas injection foaming process

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.

Evolution of Surface Oxide Film of Typical Aluminum Alloy During Medium-Temperature Brazing Process

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.

Reaction behavior between the oxide film of LY12 aluminum alloy and the flux

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.

Influence of Surface Oxide Films on Elastic Behaviors of Straight Screw Dislocations Parallel to the Surface of Pure Aluminum

The image stress of straight screw dislocations parallel to the medium surface covered by thin heterogeneous films was analyzed and deduced, in order to calculate the image shear stress. The relationship between image stress and distance from the screw dislocation to the interface of pure aluminum and its oxide covering was calculated based on the analysis. It was shown quantitatively that a sign conversion of the image stress appears in the case of thin oxide covering, while dislocation would pile up near the interface because of the possible slips of the screw dislocations induced by the image stress, which might break down the very thin oxide covering. Further investigation on edge dislocations or other dislocation configurations need to be done.

Effect of depressurizing speed on mold filling behavior and entrainment of oxide film in vacuum suction casting of A356 alloy

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.

Reaction mechanism between oxide film on surface of Al-Li alloy and CsF-AlF_3 flux

The composition of the oxide film on the surface of Al-Li alloy was measured after accelerated oxidation at 500 and 540 ℃,and the reaction mechanism between CsF-AlF3 flux and the oxide film on the surface of Al-Li alloy was also discussed.The results show that the oxide film on the surface of Al-Li alloy is mostly composed of Li2CO3 and amorphous Al2O3.The brazing technology for Al-Li alloy is accomplished using the improved CsF-AlF3 flux.The improved flux CsF-AlF3 can effectively remove the oxide film by the way of reacting and/or dissolving the oxide film,of which CsF compound plays an important role in the course of removing the oxide film.The key step is the generation of HF,which induces and accelerates the reaction of removing oxide film.The generation of H2O also accelerates the reaction.

Nucleation of Fe-Rich Intermetallic Phases on α-Al_(2)O_(3) Oxide Films in Al-Si Alloys

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.

Influence of additive element on surface oxide film of A356 alloy

The influences of RE-modification and Sr-modification on the hydrogen content and surface oxide film of A356 aluminum alloy melt were investigated. The hydrogen content of the melt was measured by reduce pressure test. The phases in the surface oxide film were analyzed by X-ray diffractometry (XRD), and the morphology of the surface oxide film was observed by scanning electronic microscopy (SEM). The results show that RE-modification reduces the hydrogen content of A356 aluminum alloy greatly. Contrarily, Sr-modification increases the hydrogen content remarkably. After being treated with RE, a large number of LaAl11O18 consisting of Al2O3 and La2O3, are generated in the surface oxide film of A356 alloy. The surface oxide film of Sr-modification is almost composed of Al2SrO4. According to the results of SEM, the surface oxide film of Sr-modification is very easy to crack, destroy the continuity and compactness of surface oxide film, accelerate the vapor diffusing into the melt, consequently, increase the hydrogen content of A356 alloy melt significantly. But RE-modification makes the surface oxide film compact, and restrains the aluminum exposed to water, so reduces the hydrogen content of A356 alloy melt.

Influences of pulse frequency on formation and properties of composite anodic oxide films on Ti-10V-2Fe-3Al alloy

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.

Effect of Sb on the properties of anodic Pb(Ⅱ) oxide film formed in alkaline solution

The composition and properties of the anodic films formed on Pb and Pb-3at.%Sb alloy at -0.10 V (vs. Hg/HgO) for 2.5 h in 0.1 mol.dm-3 NaOH solution (25℃) were investigated by cyclic voltammetry, linear sweep voltammetry, open circuit decay curve, photocurrent technique, X-ray diffraction (XRD) and scanning electron microscopy (SEM). It was found that the anodic film formed oh Pb mainly consists of t-PbO, while that on Pb-3at.%Sb consists of o-PbO, t-PbO and a small amount of orthorhombic Sb2O3. The dominant component of the film anodically grown on Pb-3at.%Sb for less than 5 min is o-PbO, however, t-PbO is the major component of the anodic film formed for 1 h or longer. It is established that Sb suppresses the growth of t-PbO. The anodic film formed on Pb-3at.%Sb is less porous than that on Pb. The bandgap energies of t-PbO and o-PbO in the films were determined by photocurrent measurements to be 1.83-1.84 eV and 2.60 eV, respectively.