CN116247160A - Medical equipment battery positive electrode plate and preparation method thereof - Google Patents
Medical equipment battery positive electrode plate and preparation method thereof Download PDFInfo
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- A61B5/14532—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue for measuring glucose, e.g. by tissue impedance measurement
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Abstract
The invention discloses a medical equipment battery positive plate and a preparation method thereof, wherein a film coating method combining dry mixing and wet mixing is adopted, and as powder blending can reduce the phenomena of uneven distribution and uneven adhesion of conductive materials, the construction of a conductive network is facilitated, the porosity of the positive plate material is increased, so that the polarization of the positive plate is reduced, and the high-current pulse discharge capacity of the battery is improved.
Description
Technical Field
The invention relates to a battery material, in particular to a battery positive plate of medical equipment and a preparation method thereof.
Background
The pancreas in the body of a normal person can automatically monitor the glucose content in the blood of the person and automatically secrete the required insulin/glucagon. However, the pancreas of the diabetic patient has abnormal functions and cannot normally secrete insulin required by the human body. Diabetes is a metabolic disease caused by abnormal pancreatic function of a human body, and diabetes is a life-long disease. At present, the medical technology cannot radically cure diabetes, and the occurrence and development of diabetes and complications thereof can only be controlled by stabilizing blood sugar.
Diabetics need to test blood glucose before injecting insulin into the body. Most of the current detection methods can continuously detect blood sugar and send blood sugar data to remote equipment in real time, so that the blood sugar data is convenient for a user to check, and the detection method is called continuous glucose detection (Continuous Glucose Monitoring, CGM). The method needs a detection device to be attached to the surface of skin, a probe carried by the detection device is penetrated into subcutaneous tissue fluid to complete periodic detection, and a battery is needed to provide high-current pulse discharge during detection.
The porosity of the positive electrode plate of the existing lithium manganese button cell is low, and electrolyte cannot well permeate into the electrode gap to form an electrochemical path, so that the electrochemical response rate of the positive electrode plate is affected; secondly, the positive electrode plate with lower porosity is easy to generate polarization, and the electrochemical response rate of the positive electrode is further influenced. When the conventional battery is subjected to large-current pulse discharge, the electrochemical response rate of the positive electrode plate is slow, so that the instantaneous extremely large voltage drop is caused, and the stable current cannot be normally output.
Therefore, a battery positive electrode plate with larger porosity and rapid electrochemical response is needed in the prior art so as to meet the requirement of high-current pulse discharge.
Disclosure of Invention
The embodiment of the invention discloses a medical equipment battery positive electrode plate, which is characterized in that a film coating method combining dry mixing and wet mixing is adopted, powder blending can avoid uneven distribution of conductive materials and uneven adhesion as much as possible, the construction of a conductive network is facilitated, the porosity of the positive electrode plate is increased, the polarization of the positive electrode plate is reduced, and the high-current pulse discharge capacity is improved.
The invention discloses a medical equipment battery positive plate, which comprises: the substrate is one or more of aluminum foil, foam nickel screen or stainless steel screen; the conductive layer is coated on the surface of the substrate, comprises electrolytic manganese dioxide, a conductive agent and a binder, and is prepared by the following steps:
(1) heat treatment is carried out on electrolytic manganese dioxide to optimize the crystal structure of the electrolytic manganese dioxide, and the heat treatment method comprises the following steps: sieving electrolytic manganese dioxide, selecting particles with granularity less than 200um, placing the particles in a sintering furnace, and heating to 200-300 ℃ for 2-4h;
(2) cooling electrolytic manganese dioxide to below 60 ℃, mixing with a conductive agent and a binder with granularity less than 200um, stirring and grinding to obtain a grinding mixture;
(3) placing the grinding mixture in a vacuum oven, heating to 65-85 ℃ for 3-5 hours to dry the grinding mixture to obtain a positive electrode mixture;
(4) mixing and stirring the positive electrode mixture and an NMP solvent to obtain positive electrode mixed slurry;
(5) and (3) coating the anode mixed slurry on a substrate, placing the substrate in a vacuum oven, heating to 110-130 ℃ for 9-12h, and drying to obtain the conductive layer.
According to one aspect of the invention, the conductive agent is one or more of conductive carbon black, graphite, super p, or carbon nanotubes.
According to one aspect of the invention, the binder is one or more of polyvinylidene fluoride, polytetrafluoroethylene, sodium polyacrylate.
According to one aspect of the invention, the binder is polyvinylidene fluoride and sodium polyacrylate in a mass ratio of 1:1.
According to one aspect of the invention, the electrolytic manganese dioxide, the conductive agent and the binder are present in the milling mixture in a mass ratio of 80-96%, 2-10% and 2-10%, respectively.
According to one aspect of the present invention, in the positive electrode mixture slurry, the mass ratio of the positive electrode mixture to the NMP solvent is (0.8-1): 1.
the invention also provides a preparation method of the medical equipment battery positive plate, which comprises the following steps:
(1) performing heat treatment on electrolytic manganese dioxide to optimize the crystal structure of the electrolytic manganese dioxide;
(2) cooling electrolytic manganese dioxide to below 60 ℃, mixing with a conductive agent and a binder, stirring and grinding to obtain a grinding mixture;
(3) placing the ground mixture in a vacuum oven, heating to 65-85 ℃ for 3-5 hours to obtain a positive electrode mixture;
(4) mixing and stirring the positive electrode mixture and an NMP solvent to obtain positive electrode mixed slurry;
(5) coating the anode mixed slurry on a substrate, placing the substrate in a vacuum oven, heating to 110-130 ℃ for 9-12h, and drying to obtain a conductive layer;
(6) and (3) passing the substrate and the conducting layer coated on the surface of the substrate through a roller to obtain the positive electrode plate.
According to one aspect of the present invention, in step (1), the heat treatment method is: firstly, sieving electrolytic manganese dioxide, selecting particles with granularity less than 200um, placing the particles in a sintering furnace, and heating to 200-300 ℃ for 2-4h.
According to one aspect of the invention, in step (1), the heating temperature is 250 ℃ and the duration is 3h.
According to one aspect of the present invention, in step (2), the conductive agent is one or more of conductive carbon black, graphite, super p, or carbon nanotubes.
According to one aspect of the invention, in step (2), the binder is one or more of polyvinylidene fluoride, polytetrafluoroethylene, sodium polyacrylate.
According to one aspect of the invention, in step (2), the electrolytic manganese dioxide, the conductive agent and the binder are present in a mass ratio of 80-96%, 2-10% and 2-10%, respectively.
According to one aspect of the present invention, in step (4), the mass ratio of the positive electrode mixture to the NMP solvent is (0.8-1): 1.
according to one aspect of the invention, in the step (6), the thickness of the positive electrode sheet after passing through the roller is 180-220um.
The invention also discloses a highly integrated analyte detection device, comprising: a bottom case for being fixed on the skin surface of the user; the sensor module is in releasable connection with the bottom shell; the emitter module is electrically connected with the sensor module; and a battery using a positive pole piece of the medical device battery for providing electrical energy.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the medical equipment battery positive electrode plate disclosed by the invention has the advantages that the mixing is uniform, the whole conductive network is perfect, the porosity is higher, the ion conduction efficiency can be improved, the polarization is reduced, the electrolyte is easier to infiltrate, and the requirements of high-current pulse discharge can be met.
Furthermore, the preparation process of the medical equipment battery positive plate is simple, the method is universal, the cost is low, and the method is suitable for large-scale industrialized production.
Further, the thickness of the positive electrode sheet after passing through the roller is smaller, so that the battery can be miniaturized more.
Drawings
FIG. 1 is an electrochemical impedance spectrum of a positive electrode tab of a medical device battery according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an application of an embodiment of the present invention to a highly integrated analyte detection device.
Detailed Description
As described above, the positive electrode plate of the battery in the prior art is generally manufactured by adopting a tabletting method and a paste coating method, and has lower porosity, so that on one hand, electrolyte is less permeated into the electrode gap to influence the response of the positive electrode plate, and on the other hand, polarization is easy to generate, ions in the electrolyte need to overcome the barriers of the battery electrode plate, a diaphragm and the electrolyte, the internal polarization resistance of the electrode plate is shown, and the electrochemical response of the electrode plate can be influenced due to the excessive internal polarization resistance. Due to the problems, the battery has weak large-current pulse discharging capability and slow electrochemical response speed, is easy to cause instantaneous extremely large voltage drop, and cannot stably work under a large-current pulse environment to output current.
In order to solve the problem, the invention provides a positive electrode plate of a medical equipment battery and a preparation method thereof, wherein all equipment and raw materials are available from the market or are commonly used in the industry, and the methods in the following examples are conventional methods in the field unless otherwise specified.
Example 1
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 200 ℃ for 4 hours. The purpose of this step is to allow the electrolytic manganese dioxide to lose part of its bound water, shift the X-ray diffraction peak, reduce the interplanar spacing, and enhance the mn—o bonding force, thereby enhancing the discharge capacity of the electrolytic manganese dioxide.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 9g of electrolytic manganese dioxide, 0.5g of conductive agent with granularity less than 200um and 0.5g of binder with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then subjected to manual or electric grinding to obtain 10g of grinding mixture, and the grinding mixture can pass through a 300-mesh (granularity 48 um) screen. The purpose of this step is to ensure the uniformity of the mixture, and avoid the phenomenon of uneven dispersion of the conductive agent and the binder.
In other embodiments of the present invention, the electrolytic manganese dioxide, the conductive agent and the binder may be mixed in the mass proportions of 80% -96%, 2% -10% and 2% -10%, respectively, not limited to the above proportions.
In a preferred embodiment of the present invention, the conductive agent may be one or more of conductive carbon black, graphite, super p, or carbon nanotubes.
In a preferred embodiment of the present invention, the binder may be one or more of PVDF (polyvinylidene fluoride), polytetrafluoroethylene, sodium polyacrylate.
(3) And (3) placing the ground mixture in a vacuum oven, heating to 65 ℃ for 5 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the positive electrode mixture.
(4) 10g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that the uniform mixing is ensured, and the positive electrode slurry with the solid content of 50% is obtained. The purpose of this step is to ensure that the components in the positive electrode slurry are uniformly dispersed, and the solid content has a certain relation with the viscosity of the positive electrode slurry, and the positive electrode slurry with 50% of the solid content has good viscosity, and the film forming effect after being coated on the substrate is good, so that the phenomena of powder falling or cracking can be reduced.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 110 ℃ for 12 hours, and ensuring that the moisture is completely dried.
In a preferred embodiment of the invention, the substrate material is one of aluminum foil or foam nickel mesh, and has a thickness of 12-18um.
In a more preferred embodiment of the invention, the substrate material is aluminum foil, 15um thick.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 180-220 mu m, and a positive electrode plate finished product is obtained. The thickness of the positive pole piece can be controlled by adjusting the working parameters of the coating machine and the roller press, and the pole piece can also have a relatively perfect conductive network on the premise of ensuring higher compaction density, so that the working requirements of high-current pulse discharge can be met.
Fig. 1 is a comparison chart of electrochemical impedance spectra, wherein a solid line gamma is an electrochemical impedance curve of a positive electrode plate gamma processed by a process step (a film coating method combined by dry and wet materials) according to an embodiment of the present invention, and a dotted line beta is an electrochemical impedance curve of a positive electrode plate beta processed by a process step (a tabletting and paste coating method) according to the prior art. As can be seen from the figure, at R sei The curvature of the solid line gamma is smaller than that of the broken line beta, which shows that the polarization degree of the positive electrode plate gamma is smaller than that of the positive electrode plate beta, and the electrolyte wettability of the positive electrode plate gamma is better than that of the positive electrode plate beta, so that the resistance of the positive electrode plate gamma is smaller than that of the positive electrode plate beta during high-current pulse discharge, and the discharge capacity of the battery is improved. Next, at R ct The curvature of the solid line gamma is still smaller than the curvature of the broken line beta, which indicates that the resistance of the positive electrode gamma is smaller than that of the positive electrode beta, because the porosity of the positive electrode gamma is larger than that of the positive electrode beta in the same environment in the battery, the positive electrode gamma can accommodate more electrolyte with higher concentration, and the discharge capability of the battery in the process of large current pulse is further improved.
Example two
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 300 ℃ for 2 hours.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 9g of electrolytic manganese dioxide, 0.5g of super p (or conductive carbon black, graphite and carbon nano tube) with granularity less than 200um, 0.25g of PVDF (polyvinylidene fluoride) with granularity less than 200um and 0.25g of sodium polyacrylate with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then subjected to manual or electric grinding to obtain 10g of grinding mixture, and the grinding mixture can pass through a screen mesh with 300 meshes (granularity of 48 um).
In the embodiment of the invention, the polyvinylidene fluoride and the sodium polyacrylate are used as the binder together, so that the binding effect can be better provided, and the positive electrode slurry has better film forming effect in the follow-up coating and rolling process flow, and the possibility of powder falling or cracking is further reduced.
(3) And (3) placing the ground mixture in a vacuum oven, heating to 65 ℃ for 5 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the positive electrode mixture.
(4) 10g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that the uniform mixing is ensured, and the positive electrode slurry with the solid content of 50% is obtained.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 110 ℃ for 12 hours, and ensuring that the moisture is completely dried.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 180-220 mu m, and a positive electrode plate finished product is obtained.
Example III
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 300 ℃ for 2 hours.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 9g of electrolytic manganese dioxide, 0.5g of super p (or conductive carbon black, graphite and carbon nano tube) with granularity less than 200um, 0.25g of PVDF (polyvinylidene fluoride) with granularity less than 200um and 0.25g of sodium polyacrylate with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then subjected to manual or electric grinding to obtain 10g of grinding mixture, and the grinding mixture can pass through a screen mesh with 300 meshes (granularity of 48 um).
(3) And (3) placing the ground mixture in a vacuum oven, heating to 65 ℃ for 5 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the positive electrode mixture.
(4) 12.5g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that uniform mixing is ensured, and the positive electrode slurry with the solid content of 44.4% is obtained.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 110 ℃ for 12 hours, and ensuring that the moisture is completely dried.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 180-220 mu m, and a positive electrode plate finished product is obtained.
With continued reference to the electrochemical impedance spectrum contrast chart shown in fig. 1, the solid line Θ is an electrochemical impedance curve of the positive electrode sheet Θ processed according to the process step (dry-wet mixing combined film coating method) of the embodiment of the present invention, and the dotted line β is an electrochemical impedance curve of the positive electrode sheet β processed by the process step of the prior art (tabletting and pasting method). As can be seen from the figure, at R sei In the stage, the curvature of the solid line Θ is smaller than that of the broken line beta, which indicates that the polarization degree of the positive electrode sheet Θ is smaller than that of the positive electrode sheet beta, so that the resistance of the positive electrode sheet Θ is smaller than that of the positive electrode sheet beta during high-current pulse discharge, and the discharge capacity of the battery is improved. Next, at R ct In the stage of the process, the process comprises the steps of,the curvature of the solid line Θ is still smaller than that of the broken line beta, which indicates that the resistance of the positive electrode sheet Θ is smaller than that of the positive electrode sheet beta, because the porosity of the positive electrode sheet Θ is larger than that of the positive electrode sheet beta in the same environment in the battery, the positive electrode sheet Θ can accommodate more electrolyte with higher concentration, and the discharge capability of the battery in the process of high current pulse is further improved.
Example IV
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 300 ℃ for 2 hours.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 8g of electrolytic manganese dioxide, 1g of super p (or conductive carbon black, graphite and carbon nano tube) with granularity less than 200um, 0.5g of PVDF (polyvinylidene fluoride) with granularity less than 200um and 0.5g of sodium polyacrylate with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then manually or electrically ground to obtain 10g of grinding mixture, and the grinding mixture can pass through a screen mesh with 300 meshes (granularity of 48 um).
(3) And (3) placing the ground mixture in a vacuum oven, heating to 65 ℃ for 5 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the positive electrode mixture.
(4) 10g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that the uniform mixing is ensured, and the positive electrode slurry with the solid content of 50% is obtained.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 110 ℃ for 12 hours, and ensuring that the moisture is completely dried.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 180-220 mu m, and a positive electrode plate finished product is obtained.
Example five
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 300 ℃ for 2 hours.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 8g of electrolytic manganese dioxide, 1g of super p (or conductive carbon black, graphite and carbon nano tube) with granularity less than 200um, 0.5g of PVDF (polyvinylidene fluoride) with granularity less than 200um and 0.5g of sodium polyacrylate with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then manually or electrically ground to obtain 10g of grinding mixture, and the grinding mixture can pass through a screen mesh with 300 meshes (granularity of 48 um).
(3) And (3) placing the ground mixture in a vacuum oven, heating to 85 ℃ for 3 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the anode mixture.
(4) 10g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that the uniform mixing is ensured, and the positive electrode slurry with the solid content of 50% is obtained.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 110 ℃ for 12 hours, and ensuring that the moisture is completely dried.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 180-220 mu m, and a positive electrode plate finished product is obtained.
Example six
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 300 ℃ for 2 hours.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 8g of electrolytic manganese dioxide, 1g of super p (or conductive carbon black, graphite and carbon nano tube) with granularity less than 200um, 0.5g of PVDF (polyvinylidene fluoride) with granularity less than 200um and 0.5g of sodium polyacrylate with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then manually or electrically ground to obtain 10g of grinding mixture, and the grinding mixture can pass through a screen mesh with 300 meshes (granularity of 48 um).
(3) And (3) placing the ground mixture in a vacuum oven, heating to 85 ℃ for 3 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the anode mixture.
(4) 10g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that the uniform mixing is ensured, and the positive electrode slurry with the solid content of 50% is obtained.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 130 ℃ for 9 hours, and ensuring that the moisture is completely dried.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 180-220 mu m, and a positive electrode plate finished product is obtained.
Example seven
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 300 ℃ for 2 hours.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 8g of electrolytic manganese dioxide, 1g of super p (or conductive carbon black, graphite and carbon nano tube) with granularity less than 200um, 0.5g of PVDF (polyvinylidene fluoride) with granularity less than 200um and 0.5g of sodium polyacrylate with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then manually or electrically ground to obtain 10g of grinding mixture, and the grinding mixture can pass through a screen mesh with 300 meshes (granularity of 48 um).
(3) And (3) placing the ground mixture in a vacuum oven, heating to 85 ℃ for 3 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the anode mixture.
(4) 10g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that the uniform mixing is ensured, and the positive electrode slurry with the solid content of 50% is obtained.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 130 ℃ for 9 hours, and ensuring that the moisture is completely dried.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 200 mu m, and a positive electrode plate finished product is obtained.
In the embodiment of the invention, the electrolytic manganese dioxide particles are heated to 300 ℃ to obtain a better crystal form, the porosity of the pole piece obtained by the coating process is larger, the material distribution is uniform, and the wettability of the electrolyte is better.
With continued reference to fig. 1, the solid line α is an electrochemical impedance curve of the positive electrode sheet α processed according to the process step (dry-wet mixing combined film coating method) according to an embodiment of the present invention. As can be seen from the figure, at R sei The solid line alpha curvature is smaller than the dotted line beta curvature and the solid lines gamma and theta curvature, which show that the polarization degree of the positive electrode plate alpha is smaller than the positive electrode plate beta and the positive electrode plates gamma and theta, and the electrolyte wettability of the positive electrode plate alpha is better than that of the positive electrode plate beta and the positive electrode plates gamma and theta, so that the resistance of the positive electrode plate alpha is smaller than that of the positive electrode plates beta, gamma and theta when the high-current pulse discharges, and the discharge capacity of the battery is improved. Next, at R ct The solid line alpha curvature is still smaller than the broken line beta and the solid lines gamma, theta curvature, which indicates that the resistance of the positive electrode plate alpha is smaller than the resistance of the positive electrode plates beta, gamma, theta, due to the equivalent ring in the batteryIn the environment, the porosity of the positive pole piece alpha is larger than that of the positive pole pieces beta, gamma and theta, and the positive pole piece alpha can accommodate more electrolyte with higher concentration, so that the discharge capacity of the battery in the process of large current pulse is further improved.
The thickness of the positive plate of the lithium-manganese battery in the prior art is generally 2mm. Under the process steps of the embodiment of the invention, the thickness of the positive pole piece is kept at about 200um by controlling the working parameters of the roller press, the normal conductive network and larger porosity of the pole piece can be maintained, the miniaturized design of the battery can be met, and the discharge capacity of the heavy current pulse can be met.
Example eight
(1) Screening electrolytic manganese dioxide, a conductive agent and a binder, selecting electrolytic manganese dioxide particles with granularity less than 200um by a screen or an air classifier, placing the electrolytic manganese dioxide particles into a quartz boat, performing heat treatment in a sintering furnace, and heating to 250 ℃ for 3 hours.
(2) After the electrolytic manganese dioxide in the step (1) is cooled to below 60 ℃, 8g of electrolytic manganese dioxide, 1g of super p (or conductive carbon black, graphite and carbon nano tube) with granularity less than 200um, 0.5g of PVDF (polyvinylidene fluoride) with granularity less than 200um and 0.5g of sodium polyacrylate with granularity less than 200um are respectively weighed by an electronic day, placed in a grinding dish, fully stirred and mixed, and then manually or electrically ground to obtain 10g of grinding mixture, and the grinding mixture can pass through a screen mesh with 300 meshes (granularity of 48 um).
(3) And (3) placing the ground mixture in a vacuum oven, heating to 85 ℃ for 3 hours, and drying water possibly existing in the mixture to ensure that the sample is dried, thereby obtaining the anode mixture.
(4) 10g of NMP (N-methylpyrrolidone) solvent is dripped into a dry glass bottle, then the positive electrode mixture is slowly added into the glass bottle, and the mixture is stirred by a magnetic stirrer for 3 hours, so that the uniform mixing is ensured, and the positive electrode slurry with the solid content of 50% is obtained.
(5) And (3) coating the positive electrode slurry on the surface of the substrate by using a flat plate coating machine to obtain a conductive layer, then placing the conductive layer and the substrate in a vacuum oven for baking, heating to 130 ℃ for 9 hours, and ensuring that the moisture is completely dried.
(6) And rolling the conductive layer and the substrate by using an electric vertical roller press, so that the overall thickness of the conductive layer and the substrate can be reduced to 180-220 mu m, and a positive electrode plate finished product is obtained.
FIG. 2 is a schematic perspective view of a highly integrated analyte sensing device according to an embodiment of the present invention. Highly integrated analyte detection device 10 includes a bottom housing 101, a sensor module 102, an emitter module 103, and a battery 105. A first engaging portion 1011 for fixing the transmitter 103 is provided on a side wall of the bottom case 101, and a second engaging portion 1030 corresponding to the first engaging portion 1011 is provided on a side wall of the transmitter, and the first engaging portion 1011 and the second engaging portion 1030 are engaged with each other to fix the transmitter 103 and the bottom case 101. The bottom case 101 is further provided with an assembly hole 1012 for assisting in mounting the sensor 102, and the shape of the assembly hole 1012 is matched with the shape of the edge of the sensor 102 so as to assist in mounting the sensor 102 on the bottom case 101. The bottom case 101 is further sealed with a battery 105, and a positive electrode sheet (not shown) of the battery 105 is manufactured by the process steps of the foregoing embodiment, and the overall thickness of the bottom case 101 may be thinner as the positive electrode sheet of the battery 105 becomes thinner. When the transmitter 103 is engaged with the bottom case 101, the battery 105 is used to provide power to the transmitter 103. The emitter 103 emits signals outwards at a certain frequency, the battery 105 is required to provide pulse current output with equal frequency, and the positive electrode plate manufactured by adopting the process steps in the embodiment can improve the discharging capability of the battery 105, so that the emitter 103 works under a high-reliability working condition, and the reliability of the analyte detection device is improved.
In summary, the invention provides a medical equipment battery positive electrode plate and a preparation method thereof, and a film coating method combining dry mixing and wet mixing is adopted, so that the phenomena of uneven distribution and uneven adhesion of conductive materials can be reduced by powder blending, the construction of a conductive network is facilitated, the porosity of the positive electrode plate material is higher, the polarization of the positive electrode plate material is reduced, the resistance of the positive electrode plate is reduced, and the high-current pulse discharge capacity of the battery is improved.
While certain specific embodiments of the invention have been described in detail by way of example, it will be appreciated by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.
Claims (15)
1. A medical device battery positive electrode sheet, characterized in that the positive electrode sheet comprises:
the substrate is one or more of aluminum foil, foam nickel screen and stainless steel screen;
the conductive layer is coated on the surface of the substrate, comprises electrolytic manganese dioxide, a conductive agent and a binder, and is prepared by the following steps:
(1) heat treating the electrolytic manganese dioxide to optimize the electrolytic manganese dioxide crystal structure, wherein the heat treatment method comprises the following steps: screening the electrolytic manganese dioxide, selecting particles with granularity less than 200um, placing the particles in a sintering furnace, and heating to 200-300 ℃ for 2-4 hours;
(2) cooling the electrolytic manganese dioxide to below 60 ℃, mixing with a conductive agent and a binder with particle sizes smaller than 200 mu m, stirring and grinding to obtain a grinding mixture;
(3) placing the grinding mixture in a vacuum oven, heating to 65-85 ℃ for 3-5 hours to dry the grinding mixture to obtain a positive electrode mixture;
(4) mixing and stirring the positive electrode mixture and an NMP solvent to obtain positive electrode mixed slurry;
(5) and coating the anode mixed slurry on the substrate, placing the substrate in a vacuum oven, heating to 110-130 ℃ for 9-12h, and drying to obtain the conductive layer.
2. The medical device battery positive electrode sheet according to claim 1, wherein the conductive agent is one or more of conductive carbon black, graphite, super p, or carbon nanotubes.
3. The medical device battery positive electrode sheet according to claim 1, wherein the binder is one or more of polyvinylidene fluoride, polytetrafluoroethylene, and sodium polyacrylate.
4. The medical equipment battery positive electrode plate according to claim 3, wherein the binder is polyvinylidene fluoride and sodium polyacrylate, and the mass ratio is 1:1.
5. The medical device battery positive electrode sheet according to claim 1, wherein the electrolytic manganese dioxide, the conductive agent and the binder are present in the ground mixture in a mass ratio of 80-96%, 2-10% and 2-10%, respectively.
6. The positive electrode sheet for a medical device battery according to claim 1, wherein in the positive electrode mixed slurry, a mass ratio of the positive electrode mixture to the NMP solvent is (0.8-1): 1.
7. a method for preparing the positive electrode plate of the medical equipment battery as claimed in claim 1, comprising the following steps:
(1) performing heat treatment on electrolytic manganese dioxide to optimize the crystal structure of the electrolytic manganese dioxide;
(2) cooling electrolytic manganese dioxide to below 60 ℃, mixing with a conductive agent and a binder, stirring and grinding to obtain a grinding mixture;
(3) placing the ground mixture in a vacuum oven, heating to 65-85 ℃ for 3-5 hours to obtain a positive electrode mixture;
(4) mixing and stirring the positive electrode mixture and an NMP solvent to obtain positive electrode mixed slurry;
(5) coating the anode mixed slurry on a substrate, placing the substrate in a vacuum oven, heating to 110-130 ℃ for 9-12h, and drying to obtain a conductive layer;
(6) and (3) passing the substrate and the conducting layer coated on the surface of the substrate through a roller to obtain the positive electrode plate.
8. The method for producing a positive electrode sheet for a medical device battery according to claim 7, wherein in the step (1), the heat treatment method is: screening the electrolytic manganese dioxide, selecting particles with granularity smaller than 200um, placing the particles in a sintering furnace, and heating to 200-300 ℃ for 2-4h.
9. The method for preparing a positive electrode sheet of a medical device battery according to claim 8, wherein the heating temperature is 250 ℃ and the duration is 3 hours.
10. The method for preparing a positive electrode sheet of a medical device battery according to claim 7, wherein in the step (2), the conductive agent is one or more of conductive carbon black, graphite, super p or carbon nanotubes.
11. The method for preparing a positive electrode sheet of a medical device battery according to claim 7, wherein in the step (2), the binder is one or more of polyvinylidene fluoride, polytetrafluoroethylene and sodium polyacrylate.
12. The method of producing a positive electrode sheet for a medical device battery according to claim 7, wherein in the step (2), the electrolytic manganese dioxide, the conductive agent and the binder are present in a mass ratio of 80 to 96%, 2 to 10% and 2 to 10%, respectively.
13. The method for producing a positive electrode sheet for a medical device battery according to claim 7, wherein in the step (4), the mass ratio of the positive electrode mixture to the NMP solvent is (0.8-1): 1.
14. the method for manufacturing a positive electrode sheet for a medical device battery according to claim 7, wherein in the step (6), the thickness of the positive electrode sheet after passing through the roller is 180-220 μm.
15. A highly integrated analyte sensing device comprising:
the bottom shell is used for being fixed on the skin surface of a user;
the sensor module is in releasable connection with the bottom shell and is used for detecting analyte parameter information in a user;
a transmitter module electrically connected to the sensor module for transmitting the analyte parameter information to an outside world; and
a battery using the medical device battery positive electrode sheet of claim 1, the battery being for providing electrical energy.
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| CN202111492199.0A CN116247160A (en) | 2021-12-08 | 2021-12-08 | Medical equipment battery positive electrode plate and preparation method thereof |
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