Investigation of Deoxidation Process of MoO3 Using Environmental TEM

In situ environmental transmission electron microscope (ETEM) could provide intuitive and solid proof for the local structure and chemical evolution of materials under practical working conditions. In particular, coupled with atmosphere and thermal field, the behavior of nano catalysts could be directly observed during the catalytic reaction. Through the change of lattice structure, it can directly correlate the relationship between the structure, size and properties of materials in the nanoscale, and further directly and accurately, which is of great guiding value for the study of catalysis mechanism and the optimization of catalysts. As an outstanding catalytic material in the application of methane reforming, molybdenum oxide (MoO3)-based materials and its deoxidation process were studied by in situ ETEM method. The corresponding microstructures and components evolution were analyzed by diffraction, high-resolution transmission electron microscopy (HRTEM) and electron energy loss spectrum (EELS) techniques. MoO3 had a good directional deoxidation process accompanied with the process of nanoparticles crushing and regrowth in hydrogen (H2) and thermal field. However, in the absence of H2, the samples would exhibit different structural evolution.

Effective Deoxidation Process of Titanium Scrap Using MgCl2 Molten Salt Electrolytic

To overcome the scarcity and resource limitations of Ti metal, deoxidation of Ti scrap was conducted through electrolytic refining and chemical reaction with MgCl2 molten salt electrolysis. The oxygen concentration in Ti scraps was decreased by the electrochemical and chemical reactions generated by the applied voltages. The optimized conditions for the process were derived by controlling the conditions and parameters by decreasing the thermodynamic activity of the reactants. The correlation between the deoxidation efficiency and the behavior of the voltage and current was confirmed by setting the conditions of the electrolysis process in various voltage ranges. In addition, the correlation between the presence of impurities and the measured oxygen concentration was evaluated. The surface element analysis result indicated that the salt that was not removed contained a certain amount of oxygen. Thus, the removal efficiencies of impurities and particles by deriving various post-treatment process conditions were analyzed. The results confirmed that the most stable and efficient current was formed at a specific higher voltage. Moreover, the best deoxidation result was 2425 ppm, which was 50% lower than that of the initial Ti scrap.

Effect of Fe2O3 on Electro-Deoxidation in Fe2O3-Al2O3-NaCl-KCl System

The reduction of Fe2O3-Al2O3 is one of the important reactions in the resource utilization of iron-containing oxide waste. Fe2O3-Al2O3 was electro-deoxidized in the NaCl-KCl system by molten salt electrolysis to prepare FeO/Al2O3. The effect of the Fe2O3 content on the electro-deoxidation reaction process was studied. The results show that under the conditions of 850 °C, 2.3 V, and electro-deoxidation for 4 h, FeO/Al2O3 could be obtained by controlling the content of Fe2O3. The deoxidation process was divided into three stages: electric double layer charging, Fe2O3 electro-deoxidation to Fe3O4, and Fe3O4 electro-deoxidation to FeO. With the increase in the Fe2O3 content, the deoxidation reaction rate increased, and the low-valence iron oxide particles obtained by electro-deoxidation became larger. The mechanism of the influence of Fe2O3 on the electro-deoxygenation process was determined by analyzing the experimental results. The increase in the Fe2O3 content increased the concentration of activated molecules in the system, while it reduced the resistance of electro-deoxidation. The migration of active particles in the cathode was smoother, which increased the percentage of deoxygenation of activated molecules, thereby shortening the process of the deoxidation reaction.

Evolution of the Inclusion Population During the Processing of Al-killed Steel

The increasing demand for higher inclusion cleanliness levels motivates the control over the formation and evolution of inclusions in the steel production process. In this work, the evolution of the chemical composition and size distribution of inclusions throughout a slab production process of Al-killed steel, including ladle furnace (LF) treatment and continuous casting (CC), was followed. The initial solid Al2O3 and Al2O3-MgO inclusions were modified to liquid Al2O3-CaO-MgO inclusions during LF treatment. The evolution of the size distributions during LF treatment was associated with the growth and removal of inclusions, as new inclusions were not created after the deoxidation process, according to a population density function (PDF) analysis. Additionally, the size distributions tended to be similar as the LF treatment progressed regardless of their initial features, whereas they differed during CC. Analysis of the upper tails of the distributions through generalized extreme values theory showed that inclusion distributions shifted from larger to smaller sizes as the process progressed. There were great changes in the distributions of large inclusions throughout the LF treatment and between the end of the LF treatment and the start of the CC process. Additionally, distributions of large inclusions differed at the end of the LF treatment, whereas such differences decreased as CC progressed.

MATERIALS FOR STEEL DIFFUSION DEOXIDATION

The work carried out tests and implementation of a diffusion alumina-containing deoxidizer (RDA) for steels produced by LTD Metallurg SRD RAC according to TS 0826-003-47647304-2001. The deoxidizer was used instead of traditional mixtures consisting of lime, FS65 ferrosilicon and fluorspar. RDA is a mixture of powders of carbon-, silicon- and aluminum-containing materials produced by physicochemical methods and had high dispersion. With the use of RDA, 2,704.82 tons of billets were smelted, treated and poured. Carbonaceous material and FS65 were excluded from the diffusion deoxidation process. Fluorspar consumption was reduced by 50 %. The average consumption of RDA for this period was 0.41 kg / t (for comparison: the consumption of FS65 for diffusion deoxidation is 1 kg / t).

Preparation of V–4Cr–4Ti Alloys from Mixed Oxides via Electro-Deoxidation Process in Molten Salt

V–4Cr–4Ti alloys exhibit important advantages as a candidate structural materials for fusion reactor first-walls and blanket applications. V–4Cr–4Ti alloys were prepared by direct electrochemical reduction of the solid mixture of V2O3, Cr2O3 and TiO2 in the molten CaCl2–NaCl eutectic at 1073 K. The influence of cell voltage, sintering temperature and electrolysis time on the electrolysis process are reported. The microstructure and phase compositions of the products were analyzed by scanning electron microscopy (SEM) and X-ray diffraction (XRD) during the electrolysis process. The results showed that V–4Cr–4Ti alloys can be obtained at the voltage of 3.1 V and the time of 0.5 h. Cr2O3 was first reduced to Cr metal, while V2O3 and TiO2 was reduced to low-valence oxide of vanadium and titanium. The reduction rate increases with increasing cell voltage, with much perovskite oxide formed during the electrolysis process.

Deoxidation Process of Oxidized Zirconium Alloy

When zirconium alloy is corroded, an oxide film is formed on the surface, which hinders the ion transfer during the corrosion process. Therefore, the analysis of the oxide film is an important part of the research on the corrosion resistance of zirconium alloys. In this paper, two kinds of Zr-Sn-Nb alloys were corroded in 400 °C/10.3 MPa pure steam and 500 °C/10.3 MPa pure steam in autoclave to obtain samples with oxide thickness of 14 um and 18 um respectively. Then they were annealed at 800 °C at a pressure of 10-4 Pa for 18 h. XRD and WDS studies were used to analyze the structure and oxygen content of the oxide film after annealing. The results indicate that the oxide films of alloys change from zirconium dioxide to zirconium after annealing. The oxygen diffuses into the substrate and its content decreases continuously with increasing diffusion distance. Combined with the SEM analysis of cross-section samples, it is found that the annealed samples are composed of several layers. An oxygen-saturated zirconium layer, a transitional layer with micro-cracks, an oxygen-dissolved α-Zr layer and a β-Zr layer are identified. Based on these results, the mechanism of the ion transfer in the oxide film during annealing is analyzed deeply. It is proposed that space charges in the oxide film have a major impact on deoxidation kinetics. This study provides a new research method for the corrosion mechanism of zirconium alloys.

Development of Method for Direct Deoxidation of Titanium using Mixtures of Magnesium Chloride and Rare-Earth Chlorides

To decrease the cost of Ti sponge, Ti scrap is added during the remelting process to produce an ingot. However, the use of Ti scrap as an additive during this process is limited because Ti scrap is contaminated by oxygen (O) and iron (Fe), which are not removable during the remelting process. Here we introduce a new electrochemical deoxidation process for Ti scrap using a mixture of magnesium chloride (MgCl2) and rare-earth chlorides (RECl3, RE: Y and Ho) as a flux. Ti and carbon were used as the cathode and anode, respectively. Mg is deposited on the Ti cathode and reduces the oxygen in the Ti to oxide ions (O2). The activity of the generated O2” in the system, aQi-, is maintained at a low level through the formation of rare-earth oxy chloride (REOCl), and is further decreased by the formation of carbon oxides on the anode. During this process, the concentration of oxygen in the Ti is effectively decreased to 100 mass ppm in the MgCl2-YCl3 flux at 1,200 K. This new deoxidation method is considered applicable to the recycling process of Ti scrap containing large amounts of oxygen.