Method for preparing lead-based inert anode material based on laser three-dimensional forming

Through laser stereo forming technology, Pb powder and Co2O3 powder are mixed to prepare lead-based inert anode material, which solves the corrosion and dissolution loss problems of Pb-based anode materials, improves the strength and corrosion resistance of the material, reduces energy consumption, and improves the efficiency of the zinc electrodeposition process and product purity.

CN120515992APending Publication Date: 2025-08-22CHANGCHUN UNIV OF TECH
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Patent Information

Application Number
CN202510711778.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-29
Publication Date
2025-08-22

AI Technical Summary

Technical Problem

In the existing zinc electrodeposition process, Pb-based anode materials have corrosion, dissolution loss and excessive aging, which are low in strength and easy to bend, resulting in high energy consumption, low product purity and environmental pollution problems.

Method used

Using laser stereo forming technology, the lead-based inert anode material is prepared by mixing Pb powder and Co2O3 powder, mixing with a ball mill and vacuum drying, and the lead-based inert anode material is optimized, and the material composition is optimized. The laser stereo forming process is used for additive manufacturing.

Benefits of technology

It improves the strength and corrosion resistance of lead-based inert anode materials, reduces corrosion and dissolution losses, reduces energy consumption, and improves product purity and manufacturing efficiency.

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Abstract

The invention provides a method for preparing a lead-based inert anode material based on laser three-dimensional forming, and belongs to the technical field of metal additive manufacturing. The method comprises the steps that Pb powder and Co2O3 powder are mixed according to the mass ratio of 99: 1 and then put into a ball mill, and powder mixing operation is completed in the ball mill according to a first parameter; then the mixed powder is dried according to a second parameter; and establishing a three-dimensional model, and performing laser three-dimensional forming based on the third parameter to prepare the lead-based inert anode material. The method is easy to operate, good in repeatability, high in efficiency and excellent in material performance, and the application of the laser three-dimensional forming technology in manufacturing of the lead-based inert anode material is explored. And meanwhile, the material performance is changed, the phenomena of corrosion, dissolution loss and excessive aging of the Pb-based anode material are reduced, the strength and the corrosion resistance are improved, and the problems of high energy consumption, low product purity and the like of a zinc electrodeposition process are solved.
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Description

Technical Field

[0001] The present invention belongs to the technical field of metal additive manufacturing, and specifically relates to a method for preparing a lead-based inert anode material based on laser stereo forming. Background Art

[0002] Over 80% of the world's zinc is produced by hydrometallurgical processes, primarily zinc electrodeposition. Lead is widely used as an anode material in zinc electrodeposition due to its good conductivity, ease of processing, low cost, and corrosion resistance. While zinc electrodeposition offers advantages such as mild metallurgical conditions, rapid deposition rates, and scalable production, it still faces limitations in terms of energy consumption, product purity, and environmental impact. Corrosion, dissolution loss, and excessive aging of lead-based anode materials are the primary causes of these problems. Furthermore, lead has low strength, is prone to bending, and can even cause short circuits.

[0003] To address these issues, many researchers have focused on the anode's base material. Based on this base material, they have optimized its performance by optimizing alloy composition, designing novel structures, and developing anode coatings. Optimization of alloy composition is primarily achieved by adjusting the elemental content of the base material, through the addition of alloys, oxides, and foreign nano-ceramic particles and rare earth oxides.

[0004] Laser stereo forming (LSF) technology has developed rapidly in recent years. It is an advanced manufacturing technique capable of forming metal parts and has been widely applied in various fields. As a new technology for rapidly forming metal parts, it solves the technical challenge of simultaneously meeting multiple performance requirements. As an advanced materials manufacturing technology, LSF utilizes laser cladding to achieve layer-by-layer deposition, offering high efficiency, high precision, and integrated manufacturing. LSF plays a significant role in the manufacturing field due to its technological advantages, and also provides a new technology for the manufacture of lead-based inert anode materials. Summary of the Invention

[0005] The purpose of the present invention is to provide a method for preparing lead-based inert anode materials based on laser stereo forming, so as to utilize advanced additive manufacturing technology to solve the problems in the above-mentioned background technology.

[0006] In order to solve the above problems, the present invention provides the following technical solutions: A method for preparing a lead-based inert anode material based on laser stereo forming, comprising the following steps: Pb powder and Co2O3 powder were mixed in a mass ratio of 99:1 and added into a ball mill; Setting the process parameters of the ball mill with the first parameters, and starting the ball mill to complete the powder mixing operation; Among them, the first parameters include a rotation speed of 200 r / min~500 r / min, an intermittent working mode combining forward and reverse rotation is adopted during the powder mixing operation, the working time is 5 min~10 min, the pause time is 3 min~4 min, and then the reverse work is continued, and the ball milling time of the mixed powder is 4 h~5 h.

[0007] Further, the mixed powder is vacuum dried with a second parameter, and the powder drying furnace is left to stand at room temperature; The second parameter includes a drying temperature of 100°C to 120°C and a drying time of 4h to 5h.

[0008] Use CAD software to create a three-dimensional digital model of the lead-based inert anode material according to the designed dimensions to ensure that it meets the design requirements; Furthermore, based on the third parameter, the mixed powder after the drying process is subjected to additive manufacturing by using a laser stereo forming process.

[0009] The third parameters include laser power of 100W to 1000W, scanning rate of 300mm / min to 800mm / min, overlap rate of 50%, powder feeding disk speed of 0.1 r / min to 0.5 r / min, Z-axis unidirectional travel of 0.3mm to 0.35mm, spot diameter of 2mm to 3mm, and restraining gas flow rate of 4 L / min to 6L / min. Argon is selected as the powder feeding gas.

[0010] Compared with the prior art, the present invention has the following beneficial effects: This invention discloses a method for preparing a lead-based inert anode material using laser stereolithography. The method utilizes Pb powder and Co2O3 powder as printing materials, mixes the powders in a ball mill, and then dries the mixed powder. Laser stereolithography is then used to prepare the lead-based inert anode material. Compared to existing technologies, this method utilizes modified Co2O3 particles to optimize material composition and alter material properties, reducing corrosion, dissolution loss, and excessive aging of the Pb-based anode material while increasing its strength and corrosion resistance. This method also reduces the high energy consumption and low product purity associated with zinc electrodeposition.

[0011] Furthermore, laser stereo forming technology was used to prepare anode materials. The preparation process is simple and convenient, with good repeatability, short cycle, high efficiency and excellent performance. The application of laser stereo forming technology in the manufacture of lead-based inert anode materials was explored. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 This is a flow chart of a method for preparing a lead-based inert anode material based on laser stereo forming in an embodiment of the present invention; Figure 2This is a schematic diagram of the principle of laser stereo forming in a method for preparing a lead-based inert anode material based on laser stereo forming in the first embodiment of the present invention.

[0013] Figure 2 In the figure, 1. reflector; 2. laser beam; 3. powder nozzle; 4. deposition layer; 5. substrate; 6. equipment workbench. DETAILED DESCRIPTION

[0014] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0015] Example 1

[0016] A method for preparing a lead-based inert anode material based on laser stereo forming, comprising the following steps: Pb powder and Co2O3 powder were mixed in a mass ratio of 99:1 and added into a ball mill; The process parameters of the ball mill are set to the first parameters, and the ball mill is started to complete the powder mixing operation; Among them, the first parameters include a rotation speed of 200 r / min, an intermittent working mode combining forward and reverse rotations during powder mixing operation, a working time of 5 minutes, a pause time of 3 minutes, and then continued reverse operation, and a ball milling time of the mixed powder of 4 hours.

[0017] Further, the mixed powder is vacuum dried with a second parameter, and the powder drying furnace is allowed to stand to room temperature; The second parameter includes a drying temperature of 100° C. and a drying time of 4 hours.

[0018] Use CAD software to draw a three-dimensional digital model of the lead-based inert anode material according to the designed dimensions to ensure that it meets the design requirements; Furthermore, the laser stereo forming printing parameters are set based on the third parameter, and the equipment is started to perform additive manufacturing using the laser stereo forming process on the mixed powder after the drying process.

[0019] The third parameters include a laser power of 100 W, a scanning rate of 300 mm / min, an overlap rate of 50%, a powder feeding disk rotation speed of 0.1 r / min, a Z-axis one-way stroke of 0.3 mm, a spot diameter of 2 mm, a constrained gas flow rate of 4 L / min, and argon is used as the powder feeding gas.

[0020] Example 2

[0021] A method for preparing a lead-based inert anode material based on laser stereo forming, comprising the following steps: Pb powder and Co2O3 powder were mixed in a mass ratio of 99:1 and added into a ball mill; The process parameters of the ball mill are set to the first parameters, and the ball mill is started to complete the powder mixing operation; Among them, the first parameters include a rotation speed of 350 r / min, an intermittent working mode combining forward and reverse rotations during powder mixing operation, a working time of 7 minutes, a pause time of 3 minutes, and then continued reverse operation, and a ball milling time of the mixed powder of 4 hours.

[0022] Further, the mixed powder is vacuum dried with a second parameter, and the powder drying furnace is allowed to stand to room temperature; The second parameters include a drying temperature of 110°C and a drying time of 4 hours.

[0023] Use CAD software to draw a three-dimensional digital model of the lead-based inert anode material according to the designed dimensions to ensure that it meets the design requirements; Furthermore, the laser stereo forming printing parameters are set based on the third parameter, and the equipment is started to perform additive manufacturing using the laser stereo forming process on the mixed powder after the drying process.

[0024] The third parameters include a laser power of 500 W, a scanning rate of 500 mm / min, an overlap rate of 50%, a powder feeding disk rotation speed of 0.3 r / min, a Z-axis unidirectional stroke of 0.3 mm, a spot diameter of 2 mm, a constrained gas flow rate of 5 L / min, and argon is used as the powder feeding gas.

[0025] Example 3

[0026] A method for preparing a lead-based inert anode material based on laser stereo forming, comprising the following steps: Pb powder and Co2O3 powder were mixed in a mass ratio of 99:1 and added into a ball mill; The process parameters of the ball mill are set to the first parameters, and the ball mill is started to complete the powder mixing operation; Among them, the first parameters include a rotation speed of 500 r / min, an intermittent working mode combining forward and reverse rotations during the powder mixing operation, a working time of 10 minutes, a pause time of 4 minutes, and then continuing to work in the reverse direction, and a ball milling time of the mixed powder of 5 hours.

[0027] Further, the mixed powder is vacuum dried with a second parameter, and the powder drying furnace is allowed to stand to room temperature; The second parameter includes a drying temperature of 120° C. and a drying time of 5 hours.

[0028] Use CAD software to draw a three-dimensional digital model of the lead-based inert anode material according to the designed dimensions to ensure that it meets the design requirements; Furthermore, the laser stereo forming printing parameters are set based on the third parameter, and the equipment is started to perform additive manufacturing using the laser stereo forming process on the mixed powder after the drying process.

[0029] The third parameters include a laser power of 1000 W, a scanning rate of 800 mm / min, an overlap rate of 50%, a powder feeding disk rotation speed of 0.5 r / min, a Z-axis one-way stroke of 0.35 mm, a spot diameter of 3 mm, a constrained gas flow rate of 6 L / min, and argon is used as the powder feeding gas.

Claims

1. A method for preparing a lead-based inert anode material based on laser stereo forming, characterized in that: include: Pb powder and Co2O3 powder were mixed in a mass ratio of 99:1 and then placed in a ball mill; The ball mill completes a powder mixing operation based on a first parameter, and performs a drying process on the mixed powder based on a second parameter; Based on the third parameter, the mixed powder that has completed the drying process is additively manufactured using a laser stereo forming process to complete the manufacturing of the lead-based inert anode material.

2. The Pb powder according to claim 1, characterized in that The particle size of the Pb powder is 20-100 μm.

3. The method for preparing a lead-based inert anode material based on laser stereo forming according to claim 1, characterized in that: The first parameters include a rotation speed of 200 r / min~500 r / min, an intermittent working mode combining forward and reverse rotation during powder mixing operation, a working time of 5 min~10 min, a pause time of 3 min~4 min, and then continuing reverse work, and a ball milling time of the mixed powder of 4 h~5 h.

4. The method for preparing a lead-based inert anode material based on laser stereo forming according to claim 1, characterized in that: The second parameters include a drying temperature of 100° C. to 120° C. and a drying time of 4 h to 5 h.

5. The method for preparing a lead-based inert anode material based on laser stereo forming according to claim 1, characterized in that: The third parameters include laser power of 100 W to 1000 W, scanning rate of 300 mm / min to 800 mm / min, overlap rate of 50%, powder feeding disk speed of 0.1 r / min to 0.5 r / min, Z-axis one-way stroke of 0.3 mm to 0.35 mm, spot diameter of 2 mm to 3 mm, and constraint gas flow rate of 4 L / min to 6 L / min. Argon is selected as the powder feeding gas.