Method for preparing titanium or titanium alloy in molten salt by use of pulse power supply

A technology of pulse power supply and titanium alloy, which is applied in the field of material metallurgy, can solve problems such as not being seen, and achieve the effects of easy control, simple operation process, and improvement of the surface condition of the cathode

Inactive Publication Date: 2013-11-27
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Molten Salt Electrolysis TiO 2 The preparation of metal titanium usually uses a direct current of no more than 3.2V, and the method of preparing titanium or titanium alloys in molten salt electrolysis by pulse power supply has not been reported yet.

Method used

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  • Method for preparing titanium or titanium alloy in molten salt by use of pulse power supply
  • Method for preparing titanium or titanium alloy in molten salt by use of pulse power supply
  • Method for preparing titanium or titanium alloy in molten salt by use of pulse power supply

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Use TiO with an average particle size of 0.7 μm 2Powder (purity above 98%), add 6% carbon powder and 6% PVA aqueous solution (8% concentration) to mix and stir evenly, and mold it into a cylindrical thin plate with a diameter of 60mm x a height of about 6mm under a pressure of 5MPa electrode. First dry naturally at room temperature for 48 hours, heat up to 350°C to anneal to remove PVA, and then sinter at 950°C to obtain TiO 2 The electrode weighs about 27g.

[0033] Prepared TiO 2 The electrode porosity is above 47%, and the crystal structure is rutile. With high-purity graphite plate as anode, multiple TiO 2 The electrode pieces are connected in series on the molybdenum rod as the cathode, with a total weight of about 150g. The electrolytic cell is a high-purity graphite crucible, CaCl 2 Molten salt is placed in it for electrolysis. Vacuum before electrolysis, when the vacuum is higher than 10Pa, continuously fill with argon, CaCl 2 The molten salt was dried at...

Embodiment 2

[0038] TiO with an average particle size of 0.7 μm 2 In the powder, add 7% carbon powder and 7% distilled water to mix and stir evenly, and mold it under 10MPa pressure to form a thin plate-shaped electrode with a length of 200mm, a width of 60mm, and a height of 6mm. Dry naturally at room temperature for 72 hours, then slowly heat up to 900 °C for 8 hours to prepare TiO 2 The electrode weighs about 120g, and it is divided into two halves, and the weight is about 60g.

[0039] With high-purity and high-density graphite as the anode, multiple TiO 2 The electrode pieces are connected in series on the molybdenum rod as the cathode, with a total weight of about 180g, and the electrolytic cell is a graphite crucible, CaCl 2 Molten salt is placed in it for electrolysis. After the molten salt temperature rises to 880°C and stabilizes, electrolysis begins. Perform DC voltage electrolysis of 3.0-3.2V, superimpose pulse power at intervals, and superimpose pulse power for about 5 min...

Embodiment 3

[0042] TiO with an average particle size of 0.7 μm and 1.5 μm 2 and Al 2 o 3 The powders are mixed at a mass ratio of 1:1, and the PVA solution and carbon powder are added and mixed mechanically and stirred evenly, and then pressed into a cylindrical electrode using a mold. First dry naturally at room temperature for 48 hours, anneal to remove PVA, and then sinter at high temperature to obtain TiO 2 -Al 2 o 3 The mixture electrode weighs about 27g, and the weight after drilling is about 25g. The process parameters of electrode preparation are listed in Table 1.

[0043] Table 1 Example 3 electrode preparation process parameters

[0044]

[0045] Prepared TiO 2 -Al 2 o 3 The electrode porosity is about 46%, and the two oxide powders still maintain very fine particles, and there is a certain degree of sintering connection between the particles. According to XRD phase analysis, after sintering, TiO 2 From anatase to rutile, Al 2 o 3 There was no structural change ...

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Abstract

The invention discloses a method for preparing titanium or titanium alloy in molten salt by use of a pulse power supply, which comprises the following steps of adding carbon powder and a polyvinyl alcohol solution or distilled water into the TiO2 powder as an adhesive, uniformly stirring, and then performing compression moulding to obtain a cathode electrode; by taking graphite as an anode, performing electrolysis in an argon-atmosphere electrolytic furnace while overlapping pulse current on the DC (direct current) voltage; after the electrolysis is over, extracting the cathode solid electrolysis product, and cooling to room temperature; and performing washing-ultrasonic auxiliary acid pickling-washing-drying treatment on the electrolysis product to obtain metal titanium. In molten salt electrolysis, on the basis of DC electrolysis, after the pulse power supply is applied, effective current of the molten salt electrolysis is further increased, and the current density is improved; the electrolysis effect is further improved; by use of the intermittent effect of pulse current, the diffusion of oxygen ions near the cathode is promoted, the cathode surface conditions are improved, and the molten salt is promoted to flow and diffuse into the electrode; and the operation technology is simple, the control is easy, and the technology is stable.

Description

technical field [0001] The invention belongs to the technical field of material metallurgy, and in particular relates to a method for preparing titanium or titanium alloy in molten salt by using a pulse power supply. Background technique [0002] At present, the preparation of metallic titanium by molten salt electrolysis (FFC) method is considered to be one of the most potential researches in titanium production methods. Compared with the preparation of sponge titanium by magnesia thermal reduction method currently used in industry, the advantages of FFC method are more obvious. , with raw material (TiO 2 ) are easy to obtain, low reaction temperature, short process flow, low equipment investment and low energy consumption. The method is carried out at about 900°C, excluding the titanium melting process, and the electrolytic cell only operates at a voltage of about 3V; at present, when using molten salt electrolysis to prepare metallic titanium, the direct current electrol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25C3/28C25C3/36
Inventor 刘喜波罗志涛
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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