Device for measuring gas production of negative electrode slurry

Abstract

The utility model provides a device for measuring the gas production of negative electrode slurry, which at least comprises a container, a gas generation device, a gas generation device, a gas generation device, a gas generation device and a gas generation device, and is characterized in that the container comprises a first cavity and a second cavity; the filtering membrane is arranged between the first cavity body and the second cavity body; the gas-liquid separation membrane is arranged between the second cavity and the filtering membrane; and the pressure sensor is arranged on the second cavity so as to monitor the pressure in the second cavity in real time. The gas production condition of the negative electrode slurry is measured by using a pressure difference method, the measurement method is simple and convenient, the precision is high, and the working efficiency is greatly improved.

Description

Technical Field

[0001] The utility model relates to the technical field of battery anode material detection, in particular to a device for measuring the gas production of anode slurry. Background Art

[0002] In the field of new energy materials, silicon-based anode materials have attracted much attention due to their excellent theoretical specific capacity (up to 4200 mAh / g) and are regarded as an ideal choice for the next-generation lithium battery anode materials. However, the significant volume expansion problem of silicon-based materials during charge and discharge seriously restricts their commercialization process. To solve this problem, researchers have effectively alleviated the volume expansion of silicon particles through technical means such as surface modification and element doping. However, these processes have also introduced new challenges, such as incomplete coating and surface alkalinity problems, which may cause gas production during the pulping process and affect the coating quality and effect of the electrode.

[0003] Currently, the detection of the gas production of silicon-based material slurry mainly relies on the drainage method or special instruments, but these methods often have problems such as low efficiency, uncontrollable accuracy, inability to effectively measure subtle differences, and difficulty in comparing samples. For example, although Patent CN116499926A proposes a detection system that can improve the deficiencies of existing test schemes, its efficiency and accuracy still need to be improved. Similarly, although Patents CN215640707U and CN217359471U respectively provide devices for measuring the gas production rate and gas production ratio, the structural complexity and high manufacturing cost of these devices limit their wide application.

[0004] Therefore, developing a new type of, efficient, and low-cost device for measuring the gas production of silicon-based anode materials is of great significance for accelerating the research and development and commercialization process of high-performance silicon-based anode materials. Summary of the Invention

[0005] The utility model provides a device for measuring the gas production of anode slurry to solve the technical problems of low efficiency, uncontrollable accuracy, and high cost of existing gas production measurement devices.

[0006] A device for measuring the gas production of anode slurry provided by the utility model is characterized by at least including:

[0007] A container, including a first cavity and a second cavity, wherein the first cavity accommodates the anode slurry;

[0008] A filter membrane, which is arranged between the first cavity and the second cavity;

[0009] A gas-liquid separation membrane, which is arranged between the second cavity and the filter membrane; and

[0010] A pressure sensor is arranged on the second cavity to monitor the pressure in the second cavity in real time.

[0011] In an embodiment of the present utility model, the device further includes a support plate, the support plate is arranged between the gas-liquid separation membrane and the second cavity, and the support plate is provided with uniformly distributed air-permeable holes.

[0012] In an embodiment of the present utility model, a lining is further arranged inside the container, and the lining is arranged along the periphery of the container.

[0013] In an embodiment of the present utility model, a feed port is arranged on the first cavity, and the feed port is provided with a sealing plug.

[0014] In an embodiment of the present utility model, the thickness of the gas-liquid separation membrane is 0.1 - 200 μm, and the micropore diameter is 0.1 - 100 nm.

[0015] In an embodiment of the present utility model, the pore diameter of the filter membrane is 0.1 - 1 μm.

[0016] In an embodiment of the present utility model, the thickness of the support plate is 0.01 - 1 cm, and the pore diameter of the air-permeable hole is 10 μm - 1 mm.

[0017] In an embodiment of the present utility model, the container is a pressure-resistant container, the material of the container is selected from any one of stainless steel, plastic or ceramic-plastic composite material, and the volume of the container is 100 mL - 10 L.

[0018] In an embodiment of the present utility model, the material of the lining is selected from any one of polytetrafluoroethylene, polyphenylene, quartz, ceramic, stainless steel, titanium material, nickel-based alloy and composite steel plate.

[0019] In an embodiment of the present utility model, the device further includes a dispersion device, the container is placed in the dispersion device, and the dispersion device includes any one of a shaker, a magnetic stirrer or an ultrasonic device.

[0020] The beneficial effects of the present utility model: The present utility model provides a device for measuring the gas production of the negative electrode paste. The instruments used in the measuring device are common and low-cost, and the building method is simple, sensitive and fast. And the pressure difference method is used to measure the gas production of the paste, the measuring method is simple and the precision is high, which greatly improves the work efficiency. A gas-liquid separation membrane with a smaller pore diameter is arranged in the measuring device, which can further remove the influence of small liquid droplets and improve the precision of measuring the gas production of the negative electrode paste. Description of the Drawings

[0021] To more clearly illustrate the specific embodiments of the present application or the technical solutions in the prior art, the following will briefly introduce the drawings required for the description of the specific embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0022] Figure 1 It is a schematic structural diagram of a device for measuring the gas generation of the negative electrode slurry provided by an embodiment of the present utility model.

[0023] Explanation of the reference numerals in the drawings

[0024] 1. Container; 11. First cavity; 12. Second cavity; 2. Lining; 3. Sealing plug; 4. Pressure sensor; 5. Filter membrane; 6. Gas-liquid separation membrane; 7. Support plate. Specific embodiments

[0025] The following uses specific examples to illustrate the embodiments of the present utility model. Those skilled in the art can easily understand the other advantages and effects of the present utility model from the content disclosed in this specification. The present utility model can also be implemented or applied through other different specific embodiments. Various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present utility model. It should be noted that, without conflict, the following embodiments and the features in the embodiments can be combined with each other.

[0026] It should be noted that the drawings provided in the following embodiments only schematically illustrate the basic concept of the present utility model. Therefore, only the components related to the present utility model are shown in the drawings, rather than being drawn according to the number, shape, and size of the components in actual implementation. The type, quantity, and ratio of each component in actual implementation can be arbitrarily changed, and the component layout type may also be more complex.

[0027] In the following description, a large number of details are discussed to provide a more thorough explanation of the embodiments of the present utility model. However, it is obvious to those skilled in the art that the embodiments of the present utility model can be implemented without these specific details. In other embodiments, well-known structures and devices are shown in the form of block diagrams rather than in detail to avoid making the embodiments of the present utility model difficult to understand.

[0028] Please refer to Figure 1 , Figure 1 A device for measuring the gas generation of the negative electrode slurry provided by an embodiment of the present utility model, as Figure 1As shown in the figure, this device includes a container 1, a filter membrane 5, a gas-liquid separation membrane 6, and a pressure sensor 4. Among them, the container 1 includes a first cavity 11 and a second cavity 12. The first cavity 11 contains the negative electrode paste. The filter membrane 5 and the gas-liquid separation membrane 6 are sequentially arranged between the first cavity 11 and the second cavity 12. The pressure sensor 4 is arranged on the second cavity 12. The gas generated by the negative electrode paste diffuses through the filter membrane 5 and the gas-liquid separation membrane 6 into the second cavity 12, and the pressure sensor 4 monitors the air pressure in the second cavity 12 in real time. The gas production of the negative electrode paste is measured by the pressure difference method. The measurement method is simple and has high precision, which can greatly improve work efficiency.

[0029] As Figure 1 shown, the container 1 is a pressure-resistant container. When the air pressure in the second cavity 12 increases, the container 1 remains unchanged in shape. The material of the container 1 is, for example, stainless steel, plastic, or ceramic-plastic composite material, etc. And the volume of the container 1 is 100 mL to 10 L. Specifically, for example, it is 100 mL, 200 mL, 500 mL, 800 mL, 1 L, 2 L, 3 L, 4 L, 5 L, 6 L, 7 L, 8 L, 9 L, 10 L. The present utility model does not limit the shape of the container 1, and any shape that can be formed by processing is acceptable.

[0030] As Figure 1 shown, a lining 2 can also be arranged inside the container 1. The lining 2 is arranged along the periphery of the container 1. The material of the lining 2 is, for example, any one of materials such as polytetrafluoroethylene, polyphenylene, quartz, ceramic, stainless steel, titanium material, nickel-based alloy, and composite steel plate.

[0031] As Figure 1 shown, a feed port is arranged on the first cavity 11, and a sealing plug 3 is arranged at the feed port. An air outlet is arranged on the second cavity 12, and a sealing cover (not shown in the figure) is arranged at the air outlet. When injecting the negative electrode paste into the first cavity 11, first rotate the container 1 to make the feed port located at the top of the container 1. After injecting the negative electrode paste from the feed port, cover the sealing plug 3, and then rotate it until the first cavity 11 is located at the bottom of the second cavity 12. After the gas production measurement is completed, open the sealing cover on the second cavity 12 to discharge the gas. In another embodiment, a sealing ring can also be arranged on the outer periphery of the sealing plug 3 to seal the first cavity 11. The present utility model does not limit the connection method between the first cavity 11 and the sealing plug 3. For example, it can be connected by a threaded method, or it can also be connected by a mortise and tenon method.

[0032] As Figure 1As shown, the filter membrane 5 and the gas-liquid separation membrane 6 are sequentially arranged between the first cavity 11 and the second cavity 12. Among them, the pore size of the filter membrane 5 is, for example, 0.1 - 1 μm, specifically, for example, 0.1 μm, 0.2 μm, 0.3 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm, 1 μm. The filter membrane 5 can isolate the negative electrode slurry from the gas-liquid separation membrane 6, preventing the negative electrode material in the negative electrode slurry from adhering to the gas-liquid separation membrane 6 and causing pollution and blockage. Moreover, within this range of the pore size of the filter membrane 5, the gas generated by the negative electrode slurry can permeate, while the permeation of the slurry is blocked. The thickness of the gas-liquid separation membrane 6 is 0.1 - 200 μm, specifically, for example, 0.1 μm, 1 μm, 10 μm, 20 μm, 50 μm, 100 μm, 120 μm, 150 μm, 200 μm. The pore size of the gas-liquid separation membrane 6 is 0.1 - 100 nm, specifically, for example, 0.1 nm, 0.5 nm, 1 nm, 5 nm, 10 nm, 20 nm, 50 nm, 80 nm, 100 nm. Within this range of the thickness and pore size of the gas-liquid separation membrane 6, the liquid in the negative electrode slurry can be filtered out, thereby further improving the measurement accuracy of gas production.

[0033] As Figure 1 shown, the container 1 can also be provided with a support plate 7. The support plate 7 covers the surface of the gas-liquid separation membrane 6. The support plate 7 is used to maintain the shape of the gas-liquid separation membrane 6 and prevent the gas-liquid separation membrane 6 from being deformed under pressure. The thickness of the support plate 7 is 0.01 - 1 cm, specifically, the thickness is, for example, 0.01 cm, 0.02 cm, 0.05 cm, 0.08 cm, 0.1 cm, 0.2 cm, 0.5 cm, 0.8 cm, 1 cm. The support plate 7 is provided with uniformly distributed air-permeable holes, and the pore size of the air-permeable holes is 10 μm - 1 mm, specifically, the pore size is, for example, 10 μm, 20 μm, 50 μm, 80 μm, 100 μm, 200 μm, 500 μm, 800 μm, 1 mm. The present invention does not limit the connection method between the support plate 7 and the container 1. For example, it can be connected by a card slot, for example, it can also be connected by a pin, and for example, it can also be connected by a hinge. The material of the support plate 7 is selected from any one of materials such as polytetrafluoroethylene, polyphenylene, quartz, ceramic, stainless steel, titanium material, nickel-based alloy, and composite steel plate.

[0034] As Figure 1 shown, a pressure sensor 4 is provided on the second cavity 12 to monitor the air pressure in the second cavity 12 in real time. The detection range of the pressure sensor 4 is -100 kPa - 10 MPa.

[0035] As Figure 1As shown, this device may also include a dispersion device. The container 1 is placed in the dispersion device, and the dispersion device includes any one of a shaker, a magnetic stirrer, or an ultrasonic device to homogenize the slurry in the container 1 and accelerate the gas production rate, so that this gas production detection device can detect the gas production of the negative electrode slurry more efficiently and sensitively.

[0036] The present utility model provides a device for measuring the gas production of negative electrode slurry. The instruments used in this measuring device are common and low-cost, and the construction method is simple, sensitive, and fast. Moreover, the pressure difference method is used to measure the gas production of the slurry, and the measuring method is simple and has high precision, greatly improving the work efficiency.

[0037] Test example

[0038] The test environment is 25°C, and the detection range of the pressure sensor 4 is 0 - 10 kPa (accuracy 0.25%, the read pressure value is the relative pressure, so all subsequent pressure values need to be added with 100 kPa); the container 1 is made of stainless steel, the inner liner 2 is made of polytetrafluoroethylene, and the volume of the first cavity 11 is 80 cm 3 , and the volume of the second cavity 12 is 500 cm 3 .

[0039] Weigh 30 g of silicon-carbon negative electrode material, introduce it into the first cavity 11, add 50 mL of water, cover it with the sealing plug 3, shake the container 1 to disperse the silicon-carbon evenly in the water, and then place the container 1 on the shaker. Shake it on the shaker for 6 h, then let it stand for 5 minutes, and record the pressure value as P1 after the pressure value stabilizes.

[0040] According to the formula pV = nRT, since, the corresponding gas production is, at 25°C, T = 298.15 K, the corresponding molar volume of the gas Vm is about 24.5 L / mol, combined with the volume of the second cavity 12 V1 = 500 cm 3 , R = 8.31 J / (mol·K), so the gas production V = 4.944×10 -6 P1.

[0041] According to the above calculation formula, calculate the gas production at 6 h, 12 h, 24 h, and 48 h respectively, and make Table 1.

[0042] Table 1 Gas production at different times

[0043] Time 6h 12h 24h 48h Pressure value (kPa) 100.37 100.96 102.00 102.80 <![CDATA[Gas production volume V (cm 3 )]]> 0.183 0.471 0.978 1.374 <![CDATA[Gas production per unit (cm 3 / kg)]]> 6.1 15.7 32.6 45.8 <![CDATA[The value detected by the gas production equipment instrument (cm 3 / kg)]]> 6.03 16.78 31.35 46.60

[0044] The pressure value is the value obtained by adding 100 kPa to the pressure gauge reading. It can be seen from Table 1 that this method is consistent with the data detected by the gas production equipment we purchased, and has high accuracy.

[0045] The above embodiments are only illustrative of the principles and effects of the present invention and are not intended to limit the present invention. Any person familiar with this technology can modify or change the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical ideas disclosed by the present invention should still be covered by the claims of the present invention. As used in the description herein and throughout the claims below, unless otherwise specified, "a" and "the" include plural referents. Similarly, as used in the description herein and throughout the claims below, unless otherwise specified, the meaning of "in" includes "in" and "on".

[0046] The foregoing description of the embodiments of the present invention (including what is described in the abstract of the specification) is not intended to be exhaustive or to limit the present invention to the precise forms disclosed herein. While specific embodiments of the present invention and examples of the present invention have been described herein for illustrative purposes only, various equivalent modifications will be apparent to and can be made by those skilled in the art within the spirit and scope of the present invention. As noted, these modifications can be made to the present invention as described in the foregoing description of the embodiments of the present invention, and these modifications will be within the spirit and scope of the present invention.

Claims

1. A device for measuring the gas production of a negative electrode paste, characterized in that, Comprising at least: A container including a first cavity and a second cavity, wherein the first cavity accommodates a negative electrode paste; A filter membrane disposed between the first cavity and the second cavity; A gas-liquid separation membrane disposed between the second cavity and the filter membrane; And A pressure sensor disposed on the second cavity to monitor the pressure in the second cavity in real time.

2. The device for measuring gas generation of the negative electrode paste according to claim 1, characterized in that, The device further includes a support plate disposed between the gas-liquid separation membrane and the second cavity, and the support plate is provided with uniformly distributed ventilation holes.

3. The device for measuring the gas generation of the negative electrode paste according to claim 1, characterized in that, A lining is further disposed inside the container, and the lining is disposed along the periphery of the container.

4. The device for measuring gas generation of the negative electrode paste according to claim 1, wherein, A feed port is provided on the first cavity, and the feed port is provided with a sealing plug.

5. The device for measuring the gas production of the negative electrode paste according to claim 1, characterized in that, The thickness of the gas-liquid separation membrane is 0.1 - 200 μm, and the micropore diameter is 0.1 - 100 nm.

6. The device for measuring the gas production of the negative electrode paste according to claim 1, characterized in that, The pore diameter of the filter membrane is 0.1 - 1 μm.

7. The device for measuring gas generation of the negative electrode paste according to claim 2, characterized in that, The thickness of the support plate is 0.01 - 1 cm, and the pore diameter of the ventilation holes is 10 μm - 1 mm.

8. The device for measuring the gas generation of the negative electrode paste according to claim 1, characterized in that, The container is a pressure-resistant container, and the material of the container is selected from any one of stainless steel, plastic, or ceramic-plastic composite material, and the volume of the container is 100 mL - 10 L.

9. The device for measuring the gas production of the negative electrode paste according to claim 3, characterized in that, The material of the lining is selected from any one of polytetrafluoroethylene, polyphenylene, quartz, ceramic, stainless steel, titanium material, nickel-based alloy, and composite steel plate.

10. The device for measuring gas production of the negative electrode paste according to claim 1, wherein The device further includes a dispersion device, the container is placed in the dispersion device, and the dispersion device includes any one of a shaker, a magnetic stirrer, or an ultrasonic device.

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