Method for sintering battery powder needing atmosphere protection
By loading battery powder under a protected atmosphere and utilizing an automated sintering crucible, the problems of equipment complexity and high cost in the sintering process of all-solid-state battery powder have been solved, achieving a safe and efficient sintering process.
Patent Information
- Application Number
- CN202511355350.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-22
- Publication Date
- 2026-01-23
AI Technical Summary
In existing technologies, the sintering of all-solid-state battery powder needs to be carried out under an inert atmosphere, which leads to increased equipment complexity and cost, and at the same time, the treatment of toxic waste gas generated during the production process is difficult.
Design a sintering crucible. Battery powder is loaded into the crucible and sealed under a protective atmosphere. The crucible is then removed from the protective atmosphere for high-temperature sintering. After sintering, the powder is returned to the protective atmosphere for cooling and refining. The waste gas is treated by using a regulating valve for pressure relief and return gas treatment. The operation is automated by a robotic arm.
It reduces equipment complexity and production costs, improves production efficiency, avoids the problem of the cover not being able to be opened due to negative pressure, and achieves a safe and efficient sintering process.
Smart Images
Figure CN121376910A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of battery powder sintering technology, specifically to a battery powder sintering method requiring atmosphere protection. Background Technology
[0002] Solid-state batteries have gained widespread attention due to their high stability, safety, and energy density. Compared to lithium-ion batteries that use electrolytes, solid-state batteries use a safer and more stable solid electrolyte instead of a liquid electrolyte. For the same volume, they offer higher energy density, longer range, and greater safety. A solid-state battery consists of a positive electrode material, a negative electrode material, and a solid electrolyte. A good solid electrolyte possesses the highest possible ionic conductivity, acts as an electron insulator, and exhibits excellent mechanical properties.
[0003] Sulfide solid electrolytes exhibit ionic conductivity comparable to, or even superior to, liquid electrolytes; however, their air stability and electrochemical stability pose significant bottlenecks to their application. Sulfide solid electrolytes are manufactured by sintering sulfide battery powders. This sintering process requires a protective atmosphere (inert gas protection), but the high-temperature sintering furnaces are excessively large, undoubtedly increasing the overall complexity and cost of the equipment. Furthermore, any toxic waste gases that may be generated during production must be properly treated to ensure production safety. Summary of the Invention
[0004] The technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a battery powder sintering method that does not require atmosphere protection during the sintering stage to reduce costs.
[0005] The technical solution of this invention is to provide a method for sintering battery powder requiring atmosphere protection with the following structure: including the following steps, S1. Under a protective atmosphere, the battery powder is loaded into a custom-made sintering crucible and sealed. S2. Remove the sealed sintering crucible from the protective atmosphere and place it in a high-temperature sintering furnace for high-temperature sintering. S3. After sintering is completed and the temperature is cooled down, the sintering crucible is moved back to the protective atmosphere environment, the sintering crucible is opened, and the sintered battery powder is refined and packaged.
[0006] Preferably, the atmosphere protection environment in step S1 refers to an anhydrous and oxygen-free environment.
[0007] Preferably, the anhydrous and oxygen-free environment is a glove box nitrogen environment or a glove box argon environment.
[0008] Preferably, the sintering crucible in step S1 includes a pot body (1) and a cover (2) detachably connected to the pot body (1); the cover (2) has a through hole (21) in the middle that runs through its upper and lower end faces, and a connecting pipe (23) extending vertically upward is connected to the through hole (21), and a regulating valve (3) is connected to the connecting pipe (23). The regulating valve (3) has a pressure relief function and can open or close the through hole (21).
[0009] Preferably, the regulating valve (3) includes a valve body (31) connected to a connecting pipe (23), and the inner cavity of the valve body (31) is connected to the pot body (1) through the connecting pipe (23); the valve body (31) is also provided with an exhaust hole and a return hole connected to its inner cavity, and a check valve (32) and a switch valve (33) are respectively connected to the exhaust hole and the return hole.
[0010] Preferably, the top of the outer peripheral wall of the pot body (1) is provided with a radially extending flange (11), and the flange (11) is provided with a plurality of first connecting holes (111) evenly spaced along its circumference. The cover body (2) is provided with second connecting holes (22) corresponding one-to-one with the first connecting holes (111). The second connecting hole (22) is provided with a bolt, and the connecting end of the bolt passes through the second connecting hole (22) and the first connecting hole (111) in sequence and is connected with a nut to press the cover body (2) onto the flange (11).
[0011] Preferably, the flange (11) is provided with an annular groove (12) with an open top, and a sealing gasket (13) made of graphite is placed in the annular groove (12). The upper end face of the sealing gasket (13) is sealed and fitted with the lower end face of the cover (2).
[0012] Preferably, in step S2, the distance between the heating layer of the high-temperature sintering furnace and the sintering crucible is kept consistent to ensure uniform sintering temperature.
[0013] Preferably, the sintering temperature of the high-temperature sintering furnace in step S2 is 500-800℃, and the sintering time is 2-24h.
[0014] Preferably, the sintering process of the sintering crucible in step S2 can be automatically transferred and placed by a robotic arm to improve production efficiency.
[0015] With the above structure, the battery powder sintering method requiring atmosphere protection according to the present invention has the following advantages compared with the prior art: 1. This invention designs a sintering crucible that can accommodate battery powder. The process of loading battery powder into the sintering crucible is carried out under a protective atmosphere. After loading is completed, the sintering crucible is removed from the protective atmosphere environment. Then, the sintering crucible is placed in a high-temperature sintering furnace for high-temperature sintering. During this process, the sintering crucible is sealed to prevent external air from entering. Therefore, the high-temperature sintering furnace does not need to be in a protective atmosphere environment, thereby reducing the complexity of the equipment and the production cost.
[0016] 2. Since sulfide battery powder produces waste gas during high-temperature sintering, a regulating valve is installed on the sintering crucible. When the pressure inside the sintering crucible is too high, the pressure will be released through the regulating valve. After sintering, the sintering crucible is placed back into the atmosphere protection environment, cooled down, and then the regulating valve is opened to allow the gas to return, so as to avoid the situation where the lid cannot be opened due to negative pressure inside the crucible.
[0017] 3. The regulating valve is set up with three parts: valve body, check valve and on / off valve. Before sintering, the on / off valve is closed. The waste gas generated by the battery powder in the pot during high-temperature sintering will be discharged through the check valve to avoid excessive pressure in the pot. The check valve has a one-way on / off function to prevent external air from entering the pot. After sintering, the sintering crucible is placed back into the atmosphere protection environment. After cooling down, the on / off valve can be opened to allow the return gas.
[0018] 4. The sealing gasket between the pot body and the lid is made of graphite, which is not only heat-resistant but also does not react with the battery powder inside the pot, thus providing a good seal.
[0019] 5. The sintering process of the sintering crucible can be equipped with an automated program, and the transfer and placement can be automatically carried out by a robotic arm, which can greatly improve production efficiency. Attached Figure Description
[0020] Figure 1 This is a schematic diagram of the sintering crucible in this invention.
[0021] Figure 2 This is a partial cross-sectional view of the invention under explosive conditions.
[0022] Figure 3 This is a schematic diagram of the pot body in this invention.
[0023] Explanation of reference numerals in the attached figures: 1. Pot body; 11. Flange; 111. First connecting hole; 12. Annular groove; 13. Sealing gasket; 2. Cover body; 21. Through hole; 22. Second connecting hole; 23. Connecting pipe; 3. Regulating valve; 31. Valve body; 32. Check valve; 33. Switch valve. Detailed Implementation
[0024] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.
[0025] In the description of this invention, it should be understood that the terms "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention. At the same time, the terms "first," "second," etc., are only used to distinguish the names of various components and do not have a primary or secondary relationship. Therefore, they should not be construed as limitations on this invention.
[0026] This invention discloses a method for sintering battery powder requiring atmospheric protection, comprising the following steps: S1. In an inert gas environment (such as nitrogen or argon) in the glove box, the battery powder is loaded into a custom sintering crucible and sealed.
[0027] S2. Remove the sealed sintering crucible from the glove box and automatically place it into the high-temperature sintering furnace using a robotic arm for high-temperature sintering at 600℃ for 12 hours. The high-temperature sintering furnace needs to be specially customized, with the heating layer and the sintering crucible at the same distance to ensure maximum uniformity of sintering temperature, resulting in better and more consistent sintered materials. After sintering, the sintering crucible is automatically removed from the high-temperature sintering furnace using a robotic arm.
[0028] S3. After cooling down, move the sintering crucible back to the protective atmosphere environment, open the sintering crucible, and refine and package the sintered battery powder.
[0029] like Figure 1 , Figure 2 and Figure 3 As shown, the sintering crucible includes a pot body 1 and a lid 2 that is detachably connected to the pot body 1; the lid 2 is provided with a through hole 21 that runs through its upper and lower end faces, and a regulating valve 3 is connected to the through hole 21. The regulating valve 3 can open or close the through hole 21, and the regulating valve 3 has a pressure relief function.
[0030] The through hole 21 is located in the middle of the cover body 2, and a vertically upward extending connecting pipe 23 is connected to the through hole 21. The valve body 31 is connected to the connecting pipe 23 of the through hole 21. The connecting pipe 23 and the cover body 2 are integrally formed, which can reduce the processing steps of the cover body 2 and thus save costs.
[0031] The regulating valve 3 includes a valve body 31 connected to a connecting pipe 23, with the connecting pipe 23 communicating with the inner cavity of the valve body 31. The valve body 31 also has an exhaust port and a return port communicating with its inner cavity, with a check valve 32 and a switching valve 33 respectively connected to the exhaust port and the return port. The check valve 32 is a one-way valve, and both the check valve 32 and the switching valve 33 are existing technologies and will not be described in detail here.
[0032] Before sintering, the switch valve 33 is closed. The waste gas generated by the battery powder in the pot body 1 during high-temperature sintering will be discharged through the check valve 32 to avoid excessive pressure in the pot body 1. The check valve 32 has a one-way on / off function, which can prevent external air from entering the pot body 1. After sintering, the sintering crucible is placed back into the atmosphere protection environment. After cooling down, the gas can be returned by opening the switch valve 33.
[0033] The top of the outer peripheral wall of the pot body 1 is provided with a radially extending flange 11. The flange 11 is provided with a plurality of first connecting holes 111 evenly spaced along its circumference. The lid body 2 is provided with second connecting holes 22 corresponding to the first connecting holes 111 one by one. The second connecting holes 22 are provided with bolts. The connecting end of the bolt passes through the second connecting hole 22 and the first connecting hole 111 in sequence and is connected to the nut to press the lid body 2 tightly on the flange 11, so that the pot body 1 and the lid body 2 are tightly connected.
[0034] The flange 11 is provided with an annular groove 12 with an open top. A sealing gasket 13 made of graphite is placed in the annular groove 12. The upper end face of the sealing gasket 13 is sealed and fitted with the lower end face of the cover 2, which can further improve the sealing performance and prevent air from entering the pot body 1. In addition, the graphite sealing gasket is not only resistant to high temperature, but also does not react with the battery powder in the pot body 1.
[0035] The present invention discloses a method for sintering battery powder requiring atmosphere protection. The method involves designing a sintering crucible that can accommodate the battery powder. The process of loading the battery powder into the sintering crucible is carried out under atmosphere protection. After loading is completed, the sintering crucible is removed from the atmosphere protection environment. Then, the sintering crucible is placed in a high-temperature sintering furnace for high-temperature sintering. During this process, the sintering crucible is sealed to prevent external air from entering. Therefore, the high-temperature sintering furnace does not need to be in an atmosphere protection environment, thereby reducing the complexity of the equipment and the production cost.
[0036] The sintering crucible of this invention is made of titanium alloy, which has high hardness, high temperature resistance, deformation resistance, wear resistance, corrosion resistance, and long service life. It is widely used in high-temperature powder sintering, rare earth smelting, and chemical corrosion-resistant containers. It is suitable for sulfide systems and is used for sulfide powder sintering. It is corrosion-resistant and high-temperature resistant, and no atmosphere protection is required during high-temperature sintering. After sintering, the device will not deform during and after cooling, and there will be no gas leakage, which can significantly reduce the preparation cost of mass-produced sintered battery powder. Since sulfide battery powder will generate waste gas during high-temperature sintering, this invention is equipped with a regulating valve on the sintering crucible. When the pressure inside the sintering crucible is too high, the regulating valve will release the pressure. After sintering, the sintering crucible is placed back into the atmosphere protection environment, and after cooling, the regulating valve is opened to return the gas, avoiding the situation where the lid cannot be opened due to negative pressure inside the crucible.
[0037] To further ensure the sealing performance of the sintering crucible, this invention provides a sealing gasket made of graphite between the crucible body and the lid. This gasket is not only heat-resistant but also does not react with the battery powder inside the crucible, thus providing a good sealing effect.
[0038] The sintering process of the sintering crucible of the present invention is equipped with an automated program, which realizes the automatic transfer and placement of the sintering crucible through a robotic arm, greatly improving production efficiency.
[0039] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.
Claims
1. A method for sintering battery powder requiring atmospheric protection, characterized in that: Includes the following steps, S1. Under a protective atmosphere, the battery powder is loaded into a custom-made sintering crucible and sealed. S2. Remove the sealed sintering crucible from the protective atmosphere and place it in a high-temperature sintering furnace for high-temperature sintering. S3. After sintering is completed and the temperature is cooled down, the sintering crucible is moved back to the protective atmosphere environment, the sintering crucible is opened, and the sintered battery powder is refined and packaged.
2. The method for sintering battery powder requiring atmosphere protection according to claim 1, characterized in that: The atmosphere protection environment in step S1 refers to an anhydrous and oxygen-free environment.
3. The method for sintering battery powder requiring atmosphere protection according to claim 2, characterized in that: The anhydrous and oxygen-free environment is either a nitrogen environment or an argon environment in a glove box.
4. The method for sintering battery powder requiring atmosphere protection according to claim 1, characterized in that: The sintering crucible in step S1 includes a pot body (1) and a lid (2) detachably connected to the pot body (1); the lid (2) has a through hole (21) in the middle that runs through its upper and lower end faces, and a connecting pipe (23) extending vertically upward is connected to the through hole (21), and a regulating valve (3) is connected to the connecting pipe (23). The regulating valve (3) has a pressure relief function and can open or close the through hole (21).
5. The method for sintering battery powder requiring atmosphere protection according to claim 4, characterized in that: The regulating valve (3) includes a valve body (31) connected to a connecting pipe (23). The inner cavity of the valve body (31) is connected to the pot body (1) through the connecting pipe (23). The valve body (31) is also provided with an exhaust port and a return port connected to its inner cavity. A check valve (32) and a switch valve (33) are respectively connected to the exhaust port and the return port.
6. The method for sintering battery powder requiring atmosphere protection according to claim 5, characterized in that: The top of the outer peripheral wall of the pot body (1) is provided with a radially extending flange (11). The flange (11) is provided with a plurality of first connecting holes (111) evenly spaced along its circumference. The cover body (2) is provided with second connecting holes (22) corresponding one-to-one with the first connecting holes (111). The second connecting hole (22) is provided with a bolt. The connecting end of the bolt passes through the second connecting hole (22) and the first connecting hole (111) in sequence and is connected to a nut to press the cover body (2) onto the flange (11).
7. A method for sintering battery powder requiring atmosphere protection according to claim 6, characterized in that: The flange (11) is provided with an annular groove (12) with an open top. A sealing gasket (13) made of graphite is placed in the annular groove (12). The upper end face of the sealing gasket (13) is sealed and fitted with the lower end face of the cover (2).
8. The method for sintering battery powder requiring atmosphere protection according to claim 1, characterized in that: In step S2, the distance between the heating layer of the high-temperature sintering furnace and the sintering crucible is kept consistent to ensure uniform sintering temperature.
9. A method for sintering battery powder requiring atmosphere protection according to claim 1, characterized in that: In step S2, the sintering temperature of the high-temperature sintering furnace is 500-800℃, and the sintering time is 2-24h.
10. A method for sintering battery powder requiring atmosphere protection according to claim 1, characterized in that: In step S2, the sintering process of the sintering crucible can be automatically transferred and placed by a robotic arm to improve production efficiency.