Preparation equipment for pre-lithiated and sodium-modified powder material

Abstract

The utility model discloses pre-lithiation and sodium treatment powder material preparation equipment, and relates to the technical field of secondary battery material preparation. An atomizer is arranged in the spray dryer, and a drying heater is arranged on the spray dryer; the pre-lithiation and sodium modification device is provided with a gasification device and a pre-lithiation and sodium modification heater; the CVD coating device is provided with a coating gas inlet channel and a coating process heater; a finished product tank; an electrode raw material is prepared into particles through cooperation of an atomizer of a spray dryer and a drying heater, then the particles are filled with lithium / sodium inside and on the surfaces of the particles through a pre-lithiation and sodium-modification device to serve as pre-lithiation materials, then the surfaces of the particles are coated with material layers through a CVD coating device, and the prepared pre-lithiation / sodium-modification powder material is good in particle uniformity and uniform in particle size. It is ensured that the metal lithium / sodium and the electrode material are mixed uniformly enough, and the battery has better first coulombic efficiency.

Description

Technical Field

[0001] The utility model relates to the technical field of secondary battery material preparation, in particular to a device for preparing pre-lithiation and pre-sodium powder materials. Background Art

[0002] Secondary batteries play a significant role in new energy power and energy storage. Currently, the most widely used and actively developed electrode (positive and negative) materials for secondary batteries are lithium-ion and sodium-ion secondary battery electrode materials. Energy density per unit mass and volume is a key indicator of secondary batteries, and improving the initial coulombic efficiency is a key method currently used to increase battery energy density.

[0003] Pre-lithiation / sodiumization technology is an effective means of improving the initial coulombic efficiency of battery materials. Existing pre-lithiation / sodiumization methods primarily include directly adding metallic lithium as a lithium / sodium supplement, using compounds that release lithium / sodium ions during charging as supplements, and electrochemical methods. However, all of these methods can affect battery cycling performance, leading to uneven mixing of metallic lithium / sodium with electrode materials, which in turn increases the internal resistance of the battery electrodes, resulting in insufficient energy density and poor practicality. Utility Model Content

[0004] The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the present invention provides a device for preparing pre-lithiation and pre-sodium powder materials.

[0005] The equipment for preparing pre-lithiation and sodium-containing powder materials according to the embodiment of the present invention includes:

[0006] A feeding device for inputting electrode raw materials; a spray dryer, wherein an atomizer is provided in the spray dryer, and the electrode raw materials of the feeding device can be atomized by the atomizer and then enter the spray dryer, and the spray dryer is provided with a drying heater, and the drying heater can heat the air in the spray dryer; a pre-lithiation device, which is connected to the spray dryer, and the pre-lithiation device is provided with a gasification device and a pre-lithiation heater, and the gasification device is connected to the spray dryer, and the gasification device is provided with a magnetic boat and a lithium-sodium vapor heater, and the The lithium-sodium vapor heater can heat the metal raw material in the magnetic boat into metal vapor, and the electrode raw material and the metal vapor can enter the pre-lithiation-sodium device and be mixed into a pre-lithiation material; the CVD coating device is connected to the pre-lithiation-sodium device, and the CVD coating device is provided with a coating gas inlet channel and a coating process heater, and the coating material can enter the pre-lithiation-sodium device through the coating gas inlet channel, and the coating material and the pre-lithiation material can enter the CVD coating device and be mixed into a finished product material; the finished product tank is used to collect the finished product material produced by the CVD coating device.

[0007] According to some embodiments of the present invention, a storage tank is provided between the spray dryer and the pre-lithiation-sodium device, and the electrode raw material of the spray dryer can pass through the storage tank and then enter the pre-lithiation-sodium device.

[0008] According to some embodiments of the present invention, the storage tank is provided with a storage tank vacuum valve and a storage tank air inlet valve. The storage tank vacuum valve can be connected to a vacuum pumping device to vacuum the storage tank, and the storage tank air inlet valve can be connected to a protective gas source to inject protective gas into the storage tank.

[0009] According to some embodiments of the present invention, the gasification device is provided with a gasification device air inlet pipe, and the gasification device air inlet pipe can be connected to a protective gas source to inject protective gas into the gasification device.

[0010] According to some embodiments of the present invention, a thermal insulation layer is provided on the outer side wall of the gasification device.

[0011] According to some embodiments of the present invention, the magnetic boat includes a sample container and a splash-proof cover. The metal raw material is contained in the sample container. The splash-proof cover can cover the sample container, and the splash-proof cover has air holes.

[0012] According to some embodiments of the present invention, a magnetic boat air inlet pipe is provided on the magnetic boat, and the magnetic boat air inlet pipe can be connected to a protective gas source to inject protective gas into the magnetic boat.

[0013] According to some embodiments of the present invention, a high-pressure gas inlet is provided on the pre-lithiation and sodiumization device, and the high-pressure gas inlet is connected to a high-pressure protective gas source, so that the high-pressure protective gas in the high-pressure gas inlet can enter the pre-lithiation and sodiumization device.

[0014] According to some embodiments of the present invention, the CVD coating device is provided with an outlet valve, and the outlet valve is capable of discharging the gas in the CVD coating device.

[0015] According to some embodiments of the present invention, a finished product tank is provided with a finished product tank vacuum valve and a finished product tank air inlet valve. The finished product tank vacuum valve can be connected to a vacuum pumping device to vacuum the finished product tank, and the finished product tank air inlet valve can be connected to a protective gas source to inject protective gas into the finished product tank.

[0016] According to the pre-lithiation and pre-sodium powder material preparation equipment of the embodiment of the present invention, there are at least the following technical effects: the electrode raw material is prepared into particles by the atomizer of the spray dryer in combination with the drying heater, and then the particles are filled with lithium / sodium as pre-lithiation material inside and on the surface of the particles through the pre-lithiation and pre-sodium device, and then the material layer is coated on the surface of the particles through the CVD coating device. The above method is suitable for the preparation of pre-lithiation and pre-sodium powder materials. The prepared pre-lithiation and pre-sodium powder material particles have good uniformity, ensuring that the metallic lithium / sodium and the electrode material are mixed sufficiently evenly, and the prepared battery has a better first coulombic efficiency.

[0017] Additional aspects and advantages of the present invention will be given in part in the following description and will become apparent from the following description or learned through practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Additional aspects and advantages of the present invention will become apparent and readily understood from the description of the embodiments in conjunction with the following drawings, in which:

[0019] Figure 1 It is a structural diagram of the utility model;

[0020] Figure 2 This is a schematic structural diagram of the pre-lithiation and sodiumization device in the present invention;

[0021] Figure 3 It is a structural diagram of the gasification device in the utility model;

[0022] Figure 4 It is a structural diagram of the feeding device in the utility model.

[0023] Reference numerals:

[0024] Feeding device 100, feeding valve 110, agitator 120; spray dryer 200, atomizer 210, drying heater 220; storage tank 300, storage tank vacuum valve 310, storage tank air inlet valve 320; pre-lithiation and sodiumization device 400, high-pressure gas inlet duct 410, gas heater 411, gas distribution pipe 412, gas distribution nozzle 413, pre-lithiation and sodiumization heater 420; vaporization device 500, magnetic boat 510, sample container 511, splash-proof cover 512, air vent 513, magnetic boat inlet pipe 514, lithium-sodium vapor heater 520, vaporization device inlet pipe 530, insulation layer 540; CVD coating device 600, coating gas inlet duct 610, coating process heater 620, air outlet valve 630; finished product tank 700, finished product tank vacuum valve 710, finished product tank air inlet valve 720. DETAILED DESCRIPTION

[0025] The following describes embodiments of the present invention in detail. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended only to explain the present invention and are not to be construed as limiting the present invention.

[0026] In the description of the present invention, it should be understood that descriptions involving orientations, such as up, down, front, back, left, right, etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, they cannot be understood as limitations on the present invention.

[0027] In the description of this utility model, "a plurality" means more than two, and "greater than," "less than," "exceed," etc. are understood to exclude the number itself. The use of "first" or "second" is solely for the purpose of distinguishing technical features and should not be construed as indicating or implying relative importance, or implicitly indicating the number or order of the technical features indicated.

[0028] In the description of the present invention, unless otherwise clearly defined, terms such as setting, installing, and connecting should be understood in a broad sense, and technicians in the relevant technical field can reasonably determine the specific meanings of the above terms in the present invention based on the specific content of the technical solution.

[0029] Reference below Figure 1 and Figure 2 The present invention describes an apparatus for preparing pre-lithiation and pre-sodium powder materials according to an embodiment of the present invention.

[0030] like Figure 1 and Figure 2 As shown, the pre-lithiation and sodiumization powder material preparation equipment according to the embodiment of the present invention includes a feeding device 100, a spray dryer 200, a pre-lithiation and sodiumization device 400, a CVD coating device 600 and a finished product tank 700.

[0031] The feeding device 100 is used to input electrode raw materials; the spray dryer 200 is provided with an atomizer 210, and the electrode raw materials of the feeding device 100 can be atomized by the atomizer 210 and then enter the spray dryer 200. The spray dryer 200 is provided with a drying heater 220, and the drying heater 220 can heat the air in the spray dryer 200; the pre-lithiation device 400 is connected to the spray dryer 200, and the pre-lithiation device 400 is provided with a gasification device 500 and a pre-lithiation heater 420. The gasification device 500 is connected to the spray dryer 200, and the gasification device 500 is provided with a magnetic boat 510 and a lithium-sodium steam heater 520. 0, the lithium-sodium vapor heater 520 can heat the metal raw material in the magnetic boat 510 into metal vapor, and the electrode raw material and the metal vapor can enter the pre-lithiation-sodium device 400 and be mixed into a pre-lithiation material; the CVD coating device 600 is connected to the pre-lithiation-sodium device 400, and the CVD coating device 600 is provided with a coating gas inlet 610 and a coating process heater 620, and the coating material can enter the pre-lithiation-sodium device 400 through the coating gas inlet 610, and the coating material and the pre-lithiation material can enter the CVD coating device 600 and be mixed into a finished product material; the finished product tank 700 is used to collect the finished product material made by the CVD coating device 600.

[0032] For example, taking the pre-lithiation working requirements as an example, Figure 1 As shown, the feeding device 100 has a cavity for inputting electrode raw materials into the preparation device of the present invention.

[0033] like Figure 1 and Figure 2 As shown, the spray dryer 200 has a cavity. It is connected to the feed device 100. An atomizer 210 is provided within the spray dryer 200. The electrode raw material from the feed device 100 is atomized by the atomizer 210 and then enters the spray dryer 200, where it is formed into spray-like particles. The spray dryer 200 is also equipped with a drying heater 220, which heats the air within the spray dryer 200 to remove moisture from the electrode raw material.

[0034] Reference Figure 2 、 Figure 3 The pre-lithiation and sodiumization device 400 has a cavity and is in communication with the spray dryer 200. The pre-lithiation and sodiumization device 400 is provided with a gasification device 500 and a pre-lithiation and sodiumization heater 420. The electrode raw materials from the spray dryer 200 can enter the pre-lithiation and sodiumization device 400, that is, after the moisture is removed, the electrode raw materials will be sent to the pre-lithiation and sodiumization device 400.

[0035] The gasification device 500 has a cavity and is connected to the pre-lithiation device 400. A magnetic boat 510 and a lithium-sodium vapor heater 520 are provided in the gasification device 500. The magnetic boat 510 has a cavity for accommodating the metal raw material to be heated. The lithium-sodium vapor heater 520 can heat the metal raw material in the magnetic boat 510 into metal vapor, and the metal vapor in the gasification device 500 can enter the pre-lithiation device 400. The pre-lithiation heater 420 can heat the pre-lithiation material in the pre-lithiation device 400. The electrode raw material and the metal vapor are mixed into the pre-lithiation material in the pre-lithiation device 400.

[0036] Reference Figure 1 The CVD coating device 600 is provided with a coating gas inlet 610 and a coating process heater 620. The CVD coating device 600 has a cavity and is connected to the pre-lithiation sodium device 400. The pre-lithiation material in the pre-lithiation sodium device 400 can enter the CVD coating device 600, and the coating material can enter the pre-lithiation sodium device 400 through the coating gas inlet 610. The coating process heater 620 can heat the coating material and the pre-lithiation material in the CVD coating device 600, and the coating material and the pre-lithiation material in the CVD coating device 600 are mixed to form a finished material.

[0037] The finished product tank 700 has a cavity and is in communication with the CVD coating device 600. The finished product material in the CVD coating device 600 can enter the finished product tank 700.

[0038] During actual operation, the electrode raw materials are loaded into the feeding device 100. The electrode raw materials are then heated by the atomizer 210 of the spray dryer 200 in conjunction with the drying heater 220 to first prepare nanometer to micrometer-sized powder particles with good sphericity. The particles are then filled with metallic lithium vapor prepared by the gasification device 500 as a pre-lithiation material inside and on the surface of the particles through the pre-lithiation sodium device 400, so that the metallic lithium can be evenly distributed inside and on the surface of the particles. Then, a material layer is coated on the surface of the pre-lithiation particles through the CVD coating device 600. Finally, the pre-lithiation particles are collected in the finished product tank 700, and the material preparation is completed.

[0039] The above method can precisely control and uniformly prepare pre-lithiation and coating material particles with different contents as needed. The prepared pre-lithiation powder material particles have good uniformity, ensuring that the metallic lithium / sodium and the electrode material are mixed sufficiently evenly. The prepared battery has better first coulombic efficiency, so the above technology has good application value.

[0040] Similarly, the above method is also applicable to the pre-sodium preparation requirements.

[0041] The above method is applicable to the preparation of positive electrode materials and negative electrode materials.

[0042] In some embodiments of the present invention, referring to Figure 1 、 Figure 4 The feeding device 100 is provided with a feeding valve 110 , and the electrode material can be loaded into the feeding device 100 through the feeding valve 110 .

[0043] In some embodiments of the present invention, a stirrer 120 is provided in the feeding device 100. Since the electrode material is often a mixture of multiple materials, continuous stirring by the stirrer 120 can make the electrode material more uniform.

[0044] In some embodiments of the present invention, referring to Figure 1 A storage tank 300 is provided between the spray dryer 200 and the pre-lithiation device 400. The storage tank 300 has an inner cavity. The electrode raw material of the spray dryer 200 can pass through the storage tank 300 before entering the pre-lithiation device 400. In this way, the storage tank 300 can temporarily store the material prepared by the spray dryer 200.

[0045] In some specific embodiments of the present invention, the drying heater 220 is used to inject hot air into the spray dryer 200 to heat the air in the spray dryer 200 .

[0046] In a further embodiment of the present invention, a storage tank vacuum valve 310 and a storage tank air inlet valve 320 are provided on the storage tank 300. The storage tank vacuum valve 310 can be connected to a vacuum pumping device to vacuum the storage tank 300, and the storage tank air inlet valve can be connected to a protective gas source to inject protective gas into the storage tank 300, thereby ensuring that the electrode material stored in the storage tank 300 is more stable.

[0047] In some specific embodiments of the present invention, refer to Figure 2 、 Figure 3 The pre-lithiation heater 420 is a heating coil, and the pre-lithiation heater 420 surrounds the side wall of the pre-lithiation device 400.

[0048] In some specific embodiments of the present invention, a valve is provided between the pre-lithiation and sodiumization device 400 and the gasification device 500 .

[0049] In some embodiments of the present invention, a gasification device air inlet pipe 530 is provided on the gasification device 500. The gasification device air inlet pipe 530 can be connected to a protective gas source to inject protective gas into the gasification device 500 to ensure that the metal vapor prepared in the gasification device 500 is sufficiently stable.

[0050] In some embodiments of the present invention, a heat-insulating layer 540 is provided on the outer wall of the gasification device 500 to reduce heat loss when the gasification device 500 is heated.

[0051] In some embodiments of the present invention, a magnetic boat 510 includes a sample container 511 and a splash-proof cover 512. The metal raw material is contained in the sample container 511. The splash-proof cover 512 can be closed over the sample container 511 and has a vent 513. This prevents the metal liquid from splashing out of the magnetic boat 510 when the metal raw material in the sample container 511 is heated. However, after the metal raw material in the sample container 511 is heated to metal vapor, it can still enter the inner cavity of the vaporization device 500 through the vent 513.

[0052] In some embodiments of the present invention, a magnetic boat air inlet pipe 514 is provided on the magnetic boat 510. The magnetic boat air inlet pipe 514 can be connected to a protective gas source to inject protective gas into the magnetic boat 510 to ensure that the metal raw materials and metal vapor in the magnetic boat 510 are sufficiently stable.

[0053] In some embodiments of the present invention, a high-pressure gas inlet 410 is provided on the pre-lithiation and sodiumization device 400. The high-pressure gas inlet 410 is connected to a high-pressure shielding gas source, and the high-pressure shielding gas in the high-pressure gas inlet 410 can enter the pre-lithiation and sodiumization device 400. That is, the high-pressure gas inlet 410 is connected to the shielding gas source, and the high-pressure gas inlet 410 is also connected to the pre-lithiation and sodiumization device 400. During the process of mixing the electrode raw material and the metal vapor into the pre-lithiation and sodiumization device 400 to form the pre-lithiation material, the high-pressure gas inlet 410 inputs the high-pressure shielding gas into the pre-lithiation and sodiumization device 400, which can not only pressurize the pre-lithiation and sodiumization device 400 to ensure a smooth preparation process, but also use the shielding gas to ensure a stable preparation process.

[0054] In a further embodiment of the present invention, a gas distribution pipe 412 is provided in the pre-lithiation and sodiumization device 400, and a plurality of gas distribution nozzles 413 are provided on the gas distribution pipe 412. The gas distribution pipe 412 is connected to the high-pressure gas inlet 410. The high-pressure protective gas entering the high-pressure gas inlet 410 can be injected into the pre-lithiation and sodiumization device 400 after passing through the gas distribution pipe 412 and the gas distribution nozzles 413 in sequence.

[0055] In some embodiments of the present invention, a gas heater 411 is provided on the high-pressure gas inlet duct 410. The gas heater 411 can heat the high-pressure protective gas in the high-pressure gas inlet duct 410 to prevent the high-pressure protective gas from being overcooled and affecting the pre-lithiation material preparation process in the pre-lithiation sodium heater 420.

[0056] In some specific embodiments of the present invention, the gasification device 500 is located on the upper side of the side wall of the pre-lithiation and sodiumization device 400, and the high-pressure gas inlet 410 is located on the lower side of the side wall of the pre-lithiation and sodiumization device 400.

[0057] In some specific embodiments of the present invention, the air distribution pipe 412 is disc-shaped or ring-shaped.

[0058] In some specific embodiments of the present invention, the coating process heater 620 is a heating coil, and the coating process heater 620 surrounds the side wall of the CVD coating device 600 .

[0059] In some embodiments of the present invention, referring to Figure 1 The CVD coating device 600 is provided with an outlet valve 630, which can discharge the gas in the CVD coating device 600. The outlet valve 630 is used to discharge the excess gas in the CVD coating device 600, including the protective gas and the gas formed by the reaction, to avoid excessive pressure in the CVD coating device 600.

[0060] In some embodiments of the present invention, a finished product tank vacuum valve 710 and a finished product tank air inlet valve 720 are provided on the finished product tank 700. The finished product tank vacuum valve 710 can be connected to a vacuum pumping device to vacuum the finished product tank 700, and the finished product tank air inlet valve 720 can be connected to a protective gas source to inject protective gas into the finished product tank 700 to ensure that the finished product in the finished product tank 700 is sufficiently stable.

[0061] Other structures and operations of the preparation equipment according to the embodiment of the present invention are known to ordinary technicians in this field and will not be described in detail here.

[0062] Reference below Figure 1 and Figure 2 The following describes in detail the equipment for preparing pre-lithiation and sodium-containing powder materials according to an embodiment of the present invention using a specific embodiment. It is worth noting that the following description is merely an illustrative example and does not specifically limit the present invention.

[0063] like Figure 1 and Figure 2 As shown, the pre-lithiation and sodiumization powder material preparation equipment of the present invention includes a feeding device 100, a spray dryer 200, a storage tank 300, a pre-lithiation and sodiumization device 400, a CVD coating device 600 and a finished product tank 700 from top to bottom.

[0064] The feeding device 100 is provided with a feeding valve 110 , and the feeding device 100 is provided with an agitator 120 .

[0065] The spray dryer 200 is provided with an atomizer 210. The spray dryer 200 is provided with a drying heater 220.

[0066] The storage tank 300 is provided with a storage tank vacuum valve 310 and a storage tank air inlet valve 320 .

[0067] The pre-lithiation and sodiumization device 400 is provided with a gasification device 500 , a high-pressure gas inlet 410 , and a pre-lithiation and sodiumization heater 420 .

[0068] A magnetic boat 510 is installed within the vaporization device 500. The vaporization device 500 is equipped with a lithium-sodium vapor heater 520, a vaporization device air inlet pipe 530, and an insulation layer 540. The magnetic boat 510 includes a sample container 511 and a splash cover 512, which is provided with an air vent 513. The sample container 511 is connected to the magnetic boat air inlet pipe 514. A gas heater 411 is provided on the high-pressure gas inlet duct 410. A gas distribution pipe 412 is provided within the pre-lithiation-sodium device 400, and a gas distribution nozzle 413 is provided on the gas distribution pipe 412. The gas distribution pipe 412 is connected to the high-pressure gas inlet duct 410.

[0069] The CVD coating device 600 is provided with a coating gas inlet channel 610 , a coating process heater 620 , and a gas outlet valve 630 .

[0070] The finished product tank 700 is provided with a finished product tank vacuum valve 710 and a finished product tank air intake valve 720 .

[0071] In some embodiments of the present invention, the working steps are as follows.

[0072] Step S1: A mixed solution of the negative electrode material porous carbon, the conductive agent SP, carbon nanotubes (mass ratio 95:3:2), and the solvent N-methylpyrrolidone (NMP) is continuously introduced into the feed device 100 through the feed valve 110. The mixture is continuously stirred by the stirrer 120 to ensure a uniform solution. The hot air in the spray dryer 200 is heated to 210°C. The valve connecting the feed device 100 and the spray dryer 200 is opened. The mixture is spray-dried to form particles with uniform material distribution. The storage tank vacuum valve 310 of the storage tank 300 is opened to evacuate the tank. Then, the storage tank inlet valve 320 is opened to introduce 99.99% argon gas. The prepared material particles are introduced into the argon-filled storage tank 300 through the valve connected to the spray dryer 200.

[0073] Step S2: Open the valve of the high-pressure gas inlet 410 to introduce 99.99% argon gas. Open the gas heater 411 to heat it to 100° C. and introduce the high-temperature and high-pressure argon gas into the tank body of the pre-lithiation sodium device 400 through the gas distribution nozzle 413 of the disc-shaped gas distribution pipe 412 to discharge the air in the tank body.

[0074] The pre-lithiation heater 420 of the pre-lithiation device 400 is turned on until the temperature inside the tank reaches 1450°C.

[0075] A 99.999% lithium metal block is placed in a sample container 511 of a magnetic boat 510 within a vaporizer 500 under a 99.99% argon protective atmosphere. A splash-proof cover 512 is then placed. The valve on the magnetic boat inlet pipe 514, which is located on the gasifier 500 sealing cover, is opened to allow 99.99% argon to flow in. The valve between the vaporizer 500 and the pre-lithiation / sodiumization device 400, which is hermetically connected to the pre-lithiation / sodiumization device 400, is opened to allow the gas within the vaporizer 500 to be discharged into the pre-lithiation / sodiumization device 400 and discharged from the tank along with the high-temperature, high-pressure argon gas within the tank. The valve between the vaporizer 500 and the pre-lithiation / sodiumization device 400 and the valve on the magnetic boat inlet pipe 514 are then closed. The magnetic boat inlet pipe 514 is opened to allow 99.99% argon to flow in. The lithium-sodium vapor heater 520 of the vaporizer 500 is turned on to 1450°C to generate lithium vapor. The lithium vapor enters the cavity of the vaporizer 500 through the vent 25 of the splash shield 512 via argon gas. After a certain heating period, the valve of the magnetic boat inlet pipe 514 is opened to allow 99.99% argon gas to enter. The valve between the vaporizer 500 and the pre-lithiation sodium device 400 is opened to allow the lithium vapor generated by the vaporizer 500 to enter the tank of the pre-lithiation sodium device 400. After the designated period of time, the valve between the vaporizer 500 and the pre-lithiation sodium device 400 and the valve of the magnetic boat inlet pipe 514 are closed, and the temperature of the lithium-sodium vapor heater 520 of the vaporizer 500 is lowered to 450°C.

[0076] Step S3: Open the air inlet valve 320 of the storage tank and continuously introduce a 99.99% argon protective atmosphere, open the sealing valve connected to the storage tank 300 and the pre-lithiation device 400, and introduce the material particles prepared in step S1 in the storage tank 300 into the pre-lithiation device 400 filled with metallic lithium vapor, and continuously introduce high-temperature argon gas into the gas distribution nozzle 413 to keep the pre-lithiation device 400 open. After the material particles in the tank are fully in contact with the lithium vapor in the tank for a certain period of time, the pre-lithiation heater 420 is gradually lowered to 50°C in the tank, and the metallic lithium vapor in the pre-lithiation device 400 is opened to uniformly deposit in the pores and surface of the material particles to obtain pre-lithiation material particles.

[0077] Step S4: open the valve of the coating gas inlet 610 on the CVD coating device 600, and introduce a mixture of silane and acetylene (volume ratio 7:3), open the pre-lithiation heater 420 of the CVD coating device 600 to the temperature in the CVD coating device 600 tank of 450°C, silane decomposes into amorphous nano-silicon and hydrogen, acetylene decomposes into carbon black, open the sealing valve connected to the CVD coating device 600 and the pre-lithiation device 400, and introduce the pre-lithiation material carbon material particles prepared in step S3 into the CVD coating device 600 tank, open the outlet valve 630, discharge the hydrogen and reaction gas in the tank, and the amorphous nano-silicon decomposed by silane and the acetylene decompose into carbon black, which are evenly coated on the surface of the pre-lithiation material carbon material particles prepared in step S3, thereby preparing a silicon-carbon-coated pre-lithiation porous carbon negative electrode material.

[0078] Step S5: Open and activate the sealing valve connecting the CVD coating device 600 and the finished product tank 700, and pass the silicon-carbon-coated pre-lithiated porous carbon negative electrode material prepared in step S4 into the finished product tank 700.

[0079] In some embodiments of the present invention, the working steps are as follows.

[0080] Step S1: A mixed solution of the positive electrode material lithium nickel cobalt manganese oxide LiNi0.9Co0.2Mn0.8O2, the conductive agent SP, carbon nanotubes (mass ratio 97:1:2) and the solvent N-methylpyrrolidone (NMP) is continuously introduced into the feeding device 100 through the feeding valve 110 and continuously stirred uniformly by the stirrer 120.

[0081] Step S4: Open the valve of the coating gas inlet 610 on the CVD coating apparatus 600, introduce 99.99% acetylene gas, and turn on the pre-lithiation sodium heater 420 of the CVD coating apparatus 600 to a temperature of 180°C inside the tank of the CVD coating apparatus 600. This produces carbon-coated pre-lithiated lithium nickel cobalt manganese oxide (LiNi0.9Co0.2Mn0.8O2).

[0082] In some embodiments of the present invention, the working steps are as follows.

[0083] Step S1: A mixed solution of the negative electrode material silicon carbon, the conductive agent SP, carbon nanotubes (mass ratio 95:2:3) and the solvent N-methylpyrrolidone (NMP) is continuously introduced into the feeding device 100 through the feeding valve 110 and continuously stirred uniformly by the stirrer 120.

[0084] Step S4: Open the valve of the coating gas inlet 610 on the CVD coating device 600, introduce 99.99% ethyl gas, and turn on the pre-lithiation sodium heater 420 of the CVD coating device 600 to a temperature of 180°C inside the tank of the CVD coating device 600. A carbon-coated pre-lithiation silicon-carbon negative electrode material is prepared.

[0085] According to the pre-lithiation and sodiumization powder material preparation equipment of the embodiment of the present invention, by such a setting, at least some of the following effects can be achieved: the electrode raw material is first prepared into nanometer to micron-sized powder particles with good sphericity by the atomizer 210 of the spray dryer 200 in conjunction with the drying heater 220, and then the particles are filled with the metal lithium / sodium vapor prepared by the gasification device 500 inside and on the surface of the particles through the pre-lithiation and sodiumization device 400, so that the metal lithium / sodium can be evenly distributed inside and on the surface of the particles, and then the material layer is coated on the surface of the pre-lithiation particles by the CVD coating device 600. The above method is suitable for the preparation of pre-lithiation and pre-sodiumization powder materials, and can accurately control and uniformly prepare pre-lithiation / sodiumization and coating material particles with different contents as needed. The prepared pre-lithiation / sodiumization powder material particles have good uniformity, ensuring that the metal lithium / sodium and the electrode material are mixed sufficiently evenly, and the prepared battery has a better first coulombic efficiency, so the above technology has good application value.

[0086] Throughout this specification, references to the terms "some embodiments" or "it is contemplated that" indicate that a specific feature, structure, material, or characteristic described in conjunction with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0087] Although the embodiments of the present invention have been shown and described, those skilled in the art will appreciate that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and purpose of the present invention, and that the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A device for preparing pre-lithiation and pre-sodium powder materials, characterized in that: include: A feeding device (100) for inputting electrode raw materials; A spray dryer (200), wherein an atomizer (210) is provided in the spray dryer (200), and the electrode raw material of the feeding device (100) can be atomized by the atomizer (210) and then enter the spray dryer (200), and a drying heater (220) is provided on the spray dryer (200); A pre-lithiation sodium device (400) is connected to the spray dryer (200), and a gasification device (500) and a pre-lithiation sodium heater (420) are provided on the pre-lithiation sodium device (400). The gasification device (500) is connected to the spray dryer (200), and a magnetic boat (510) and a lithium-sodium steam heater (520) are provided in the gasification device (500). The lithium-sodium steam heater (520) can heat the metal raw material in the magnetic boat (510) into metal steam, and the electrode raw material and the metal steam can enter the pre-lithiation sodium device (400) and be mixed into a pre-lithiation material; A CVD coating device (600) is connected to the pre-lithiation sodium device (400), and the CVD coating device (600) is provided with a coating gas inlet channel (610) and a coating process heater (620). The coating material can enter the pre-lithiation sodium device (400) through the coating gas inlet channel (610), and the coating material and the pre-lithiation material can enter the CVD coating device (600) and be mixed into a finished product material; The finished product tank (700) is used to collect the finished product material produced by the CVD coating device (600).

2. The pre-lithiation and sodiumization powder material preparation equipment according to claim 1, characterized in that: A storage tank (300) is provided between the spray dryer (200) and the pre-lithiation-sodium device (400), and the electrode raw material of the spray dryer (200) can pass through the storage tank (300) and then enter the pre-lithiation-sodium device (400).

3. The pre-lithiation and sodiumization powder material preparation equipment according to claim 2, characterized in that: The storage tank (300) is provided with a storage tank vacuum valve (310) and a storage tank air inlet valve (320). The storage tank vacuum valve (310) can be connected to a vacuum pumping device to evacuate the storage tank (300), and the storage tank air inlet valve can be connected to a protective gas source to inject protective gas into the storage tank (300).

4. The equipment for preparing pre-lithiation and sodium-based powder materials according to claim 1, characterized in that: The gasification device (500) is provided with a gasification device air inlet pipe (530), and the gasification device air inlet pipe (530) can be connected to a protective gas source to inject protective gas into the gasification device (500).

5. The equipment for preparing pre-lithiation and sodium powder materials according to claim 1, characterized in that: A heat-insulating layer (540) is provided on the outer side wall of the gasification device (500).

6. The equipment for preparing pre-lithiation and sodium-based powder materials according to claim 1, characterized in that: The magnetic boat (510) includes a sample container (511) and a splash-proof cover (512). The metal raw material is contained in the sample container (511). The splash-proof cover (512) can cover the sample container (511). The splash-proof cover (512) has an air hole (513).

7. The equipment for preparing pre-lithiation and sodium-based powder materials according to claim 1, characterized in that: The magnetic boat (510) is provided with a magnetic boat air inlet pipe (514), and the magnetic boat air inlet pipe (514) can be connected to a protective gas source to inject protective gas into the magnetic boat (510).

8. The equipment for preparing pre-lithiation and sodium-based powder materials according to claim 1, characterized in that: The pre-lithiation and sodiumization device (400) is provided with a high-pressure gas inlet channel (410), the high-pressure gas inlet channel (410) is connected to a high-pressure protective gas source, and the high-pressure protective gas in the high-pressure gas inlet channel (410) can enter the pre-lithiation and sodiumization device (400).

9. The equipment for preparing pre-lithiation and sodium-based powder materials according to claim 1, characterized in that: The CVD coating device (600) is provided with an outlet valve (630), and the outlet valve (630) is capable of discharging gas in the CVD coating device (600).

10. The equipment for preparing pre-lithiation and sodium-based powder materials according to claim 1, characterized in that: The finished product tank (700) is provided with a finished product tank vacuum valve (710) and a finished product tank air inlet valve (720). The finished product tank vacuum valve (710) can be connected to a vacuum pumping device to evacuate the finished product tank (700), and the finished product tank air inlet valve (720) can be connected to a protective gas source to inject protective gas into the finished product tank (700).

Images