CN116845256A - Battery anode, preparation method thereof, fuel battery and battery assembly - Google Patents

Battery anode, preparation method thereof, fuel battery and battery assembly Download PDF

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Publication number
CN116845256A
CN116845256A CN202311106902.9A CN202311106902A CN116845256A CN 116845256 A CN116845256 A CN 116845256A CN 202311106902 A CN202311106902 A CN 202311106902A CN 116845256 A CN116845256 A CN 116845256A
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China
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equal
battery anode
battery
less
anode
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Granted
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CN202311106902.9A
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Chinese (zh)
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CN116845256B (en
Inventor
王杭州
程付鹏
杨征
鲁欣欣
邓晨
李瑞珠
崔天成
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Petrochina Shenzhen New Energy Research Institute Co ltd
Petrochina Co Ltd
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Petrochina Shenzhen New Energy Research Institute Co ltd
Petrochina Co Ltd
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Publication of CN116845256A publication Critical patent/CN116845256A/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
    • H01M4/8652—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites as mixture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
    • H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
    • H01M2004/8684—Negative electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a battery anode and a preparation method thereof, a fuel cell and a battery assembly, wherein the preparation method of the battery anode comprises the following steps: mixing ferric oxide, nickel oxide and copper oxide to obtain mixed powder, mixing the mixed powder with an organic solvent to obtain a first mixed material, printing the first mixed material on an anode preform to form a first battery anode on the anode preform, and sintering the first battery anode to obtain the target battery anode.

Description

Battery anode, preparation method thereof, fuel battery and battery assembly
Technical Field
The invention relates to the technical field of battery preparation, in particular to a battery anode, a preparation method thereof, a fuel cell and a battery assembly.
Background
The anode current collector of the solid oxide fuel cell adopts noble metals such as gold, silver, platinum and the like, so that the cost is high, meanwhile, the chemical properties of the noble metals are stable, the noble metals are difficult to print on the anode surface in the post-treatment process, and the post-treatment process has high requirements and cost.
Disclosure of Invention
In view of the above, the present invention provides a battery anode, a method for preparing the same, a fuel cell, and a battery assembly.
Specifically, the invention is realized by the following technical scheme:
according to a first aspect of the present invention, there is provided a method of manufacturing a battery anode, the method comprising: mixing ferric oxide, nickel oxide and copper oxide to obtain mixed powder, mixing the mixed powder with an organic solvent to obtain a first mixed material, printing the first mixed material on an anode preform to form a first battery anode on the anode preform, and sintering the first battery anode to obtain the target battery anode.
In the embodiment, ferric oxide, nickel oxide and copper oxide are mixed to obtain mixed powder, the mixed powder and an organic solvent are mixed to obtain a first mixed material, the first mixed material is printed on an anode preform to form a first battery anode on the anode preform, and the first battery anode is sintered to obtain a target battery anode.
In some embodiments of the present invention, mixing ferric oxide, nickel oxide and copper oxide to obtain a mixed powder comprises: and mixing the ferric oxide, the nickel oxide and the copper oxide according to a first preset proportion to obtain mixed powder, wherein the first preset proportion is the mass fraction ratio of the ferric oxide to the nickel oxide to the copper oxide.
In the embodiment, the ferric oxide, the nickel oxide and the copper oxide are mixed according to the mass fraction ratio of the ferric oxide, the nickel oxide and the copper oxide to obtain mixed powder, and the proportion of the iron, the nickel and the copper can be reasonably set, so that the prepared anode current collector has good alloy performance, the conductivity is ensured, the current can be better collected and output after the current is collected, and the stable power supply of the battery is ensured.
In some embodiments of the present invention, in the first preset proportion, the range of the mass fraction of the ferric oxide is greater than or equal to 30% and less than or equal to 40%; the range of the mass fraction of the nickel oxide is more than or equal to 50% and less than or equal to 60%; the range of the mass fraction of the copper oxide is more than or equal to 10% and less than or equal to 20%.
In the embodiment, the preparation cost of the anode current collector is reduced while the current collection and output after the current collection are ensured by controlling the value range of the mass fraction of the ferric oxide to be more than or equal to 30 percent and less than or equal to 40 percent, the value range of the mass fraction of the nickel oxide to be more than or equal to 50 percent and less than or equal to 60 percent and the value range of the mass fraction of the copper oxide to be more than or equal to 10 percent and less than or equal to 20 percent.
In some embodiments of the present invention, mixing the mixed powder with the organic solvent to obtain a first mixed material includes: and mixing the mixed powder and the organic solvent on a mixer to obtain a first mixed material.
In this embodiment, carry out the mixing treatment to mixed powder and organic solvent on the blendor, can guarantee the mixing effect of compounding, be convenient for carry out reasonable control to the compounding process simultaneously to guarantee follow-up with the even printing of compounding on the positive pole prefabrication body, obtain inseparable positive pole mass flow body structure, guarantee the conductivity of positive pole mass flow body, thereby transport electric current that can be stable guarantees the power supply effect.
In some embodiments of the present invention, mixing the mixed powder and the organic solvent on a blender to obtain a first blend comprises: and at a first preset temperature, running on a mixer at a first preset rotating speed for a first preset time period to mix the mixed powder and the organic solvent, so as to obtain a first mixed material.
In this embodiment, through the restriction of first preset temperature, first preset rotational speed and first preset duration, guarantee the mixed effect of first compounding and organic solvent for mixed powder and organic solvent can abundant mix, form even system, thereby guarantee follow-up with the even printing of first compounding on the positive pole prefabrication body, obtain inseparable positive pole collector structure, guarantee positive pole collector's conductivity, thereby transport electric current that can be stable guarantees the power supply effect.
In some embodiments of the present invention, the value range of the first preset temperature is greater than or equal to 90 ℃ and less than or equal to 150 ℃; the value range of the first preset rotating speed is more than or equal to 100 revolutions per minute and less than or equal to 200 revolutions per minute; the value range of the first preset time length is more than or equal to 10 hours and less than or equal to 20 hours.
In this embodiment, the value range of the first preset temperature is set to be 90 degrees celsius or more and 150 degrees celsius or less; the value range of the first preset rotating speed is set to be more than or equal to 100 revolutions per minute and less than or equal to 200 revolutions per minute; the value range of the first preset duration is set to be more than or equal to 10 hours and less than or equal to 20 hours, and the mixing process can be reasonably controlled, so that the first mixing material which is uniformly dispersed is obtained, the first mixing material is ensured to be uniformly printed on an anode prefabricated body, a compact anode current collector structure is obtained, the conductivity of the anode current collector is ensured, and the power supply effect is ensured.
In some embodiments of the invention, the organic solvent comprises at least ethanol, a dispersant.
In the embodiment, the dispersing agent can ensure that the first powder is suspended in ethanol and does not delaminate, so that the stability of the first powder is ensured, and the dispersing agent is used as slurry in a screen printing process and a sintering process, and meets the preparation requirement of an anode current collector.
In some embodiments of the present invention, the mass fraction ratio of ethanol in the organic solvent ranges from 40% to 50%.
In the embodiment, the distribution ratio of the ethanol in the organic solvent can be reasonably controlled by enabling the value range of the mass fraction ratio of the ethanol in the organic solvent to be more than or equal to 40% and less than or equal to 50%, so that the dispersion effect of the first powder in the mixed material is ensured, the follow-up preparation of the anode current collector with compact structure is ensured, the conductivity of the anode current collector is ensured, meanwhile, the current can be stably conveyed, and the power supply effect is ensured.
In some embodiments of the invention, the dispersant comprises at least ethylcellulose, fish oil, isopropanol, polyvinyl butyral.
In the embodiment, ethyl cellulose, fish oil, isopropanol, polyvinyl butyral and ethanol are mutually insoluble, and base cellulose, fish oil, isopropanol and polyvinyl butyral can be strongly adsorbed at a place with high coverage rate of the particle surface and fully spread to form an adsorption steric hindrance layer with a certain thickness, so that powder particles are in a suspension state, and the dispersion effect of the first powder is ensured.
In some embodiments of the invention, the mass fraction ratio of ethylcellulose in the organic solvent ranges from 5% or more to 10% or less; the range of the mass fraction ratio of the fish oil in the organic solvent is more than or equal to 3% and less than or equal to 5%; the value range of the mass fraction ratio of the isopropanol in the organic solvent is more than or equal to 13% and less than or equal to 20%; the range of the mass fraction ratio of the polyvinyl butyral in the organic solvent is more than or equal to 3% and less than or equal to 5%; the organic solvent also comprises other solutes, and the range of the mass fraction ratio of the other solutes in the organic solvent is more than or equal to 20% and less than or equal to 30%.
In the embodiment, the mass fraction of the ethyl cellulose, the fish oil, the isopropyl alcohol and the polyvinyl butyral in the organic solvent is controlled, so that the proportion of the dispersing agent can be reasonably controlled, the first powder is ensured to suspend in the ethanol and not to delaminate, the stable suspension effect of the first powder is ensured, the sintering characteristic of the anode current collector is ensured, and the compactness, the porosity and the mechanical property of the sintered powder are ensured.
In some embodiments of the invention, sintering the first cell anode to obtain a target cell anode comprises: raising the temperature from room temperature to a first sintering temperature at a first temperature change speed, and performing sintering treatment on the first battery anode for a second preset time period to obtain a sintered battery anode, wherein the temperature range of the room temperature is 20-25 ℃; and increasing the second temperature change speed from the first sintering temperature to the second sintering temperature, and performing sintering treatment on the sintered battery anode for a third preset time length to obtain the target battery anode.
In the embodiment, secondary sintering treatment is carried out on the first battery anode, so that particles of the anode current collector are smaller, the economical degree and tap density are guaranteed, the large and concentrated granularity of the anode current collector is guaranteed, the physical processing performance is guaranteed, the specific capacity of materials is reduced, and the electrical circulation performance and the high-temperature storage performance of the battery anode are improved.
In some embodiments of the present invention, the first temperature change speed has a value range of 0.5 degrees celsius per minute or more and 1.5 degrees celsius per minute or less; the value range of the first sintering temperature is more than or equal to 400 ℃ and less than or equal to 450 ℃.
In this embodiment, by controlling the first temperature change rate and the first sintering temperature, the primary sintering of the battery anode can be controlled, and the condition of uneven particle size distribution of the battery anode can be improved, thereby ensuring the conductivity of the battery anode.
In some embodiments of the present invention, the value range of the second preset duration is greater than or equal to 120 minutes and less than or equal to 300 minutes.
In this embodiment, by controlling the second preset period of time, the sintering effect of the battery anode in the primary sintering process can be ensured, and indexes such as tap density, specific surface area, specific capacity, and cycle capacity retention rate of the battery anode are improved, so that the physical processing performance of the battery anode is ensured.
In some embodiments of the present invention, the second temperature change rate has a value in a range of 2 degrees celsius per minute or more and 5 degrees celsius per minute or less; the value range of the second sintering temperature is more than or equal to 960 ℃ and less than or equal to 1200 ℃.
In the embodiment, the secondary sintering process of the battery anode can be controlled by controlling the second temperature change speed and the second sintering temperature, so that the condition of uneven particle size distribution of the battery anode is further improved, indexes such as tap density, specific surface area, specific capacity, circulation capacity retention rate and the like of the battery anode are improved, the average particle size of an anode current collector is effectively increased, the tap density is improved, the specific surface area is reduced, the internal stress of less materials is reduced, and the electrochemical performance is improved.
In some embodiments of the present invention, the value range of the third preset duration is greater than or equal to 120 minutes and less than or equal to 300 minutes.
In the embodiment, the sintering effect of the battery anode in the secondary sintering process can be ensured by controlling the third preset time length, and the method has simple process, lower preparation and processing cost compared with precious metals such as gold, silver, platinum and the like in the related technology, and is easy for large-scale industrialized production.
According to a second aspect of the present invention there is provided a battery anode made by the method of making a battery anode of the first aspect.
The battery anode of the present invention is made by the method for manufacturing a battery anode of the first aspect, and has all the advantages of the foregoing first aspect or any possible implementation manner of the first aspect, which are not described herein.
According to a third aspect of the present invention, there is provided a fuel cell comprising: a battery cathode; an electrolyte layer; and the battery anode of the second aspect, the electrolyte layer being located between the battery cathode and the battery anode.
The fuel cell of the present invention comprises a cell cathode, an electrolyte layer and a cell anode of the second aspect, the electrolyte layer being between the cell cathode and the cell anode, with all the advantages of any one of the possible implementations of the second aspect or the second aspect described above, which are not described in detail herein.
According to a fourth aspect of the present invention, there is provided a battery assembly comprising: a housing; and at least one fuel cell of the third aspect, the fuel cell being located within the housing.
The fuel cell assembly of the present invention comprises a housing and at least one fuel cell of the third aspect, the housing being capable of providing an installation space for and protecting the fuel cell, the fuel cell being located within the housing, with all the advantages of the third aspect or any possible implementation of the third aspect not being repeated here.
In some embodiments of the invention, the housing is a hollow structure with a circular cross-section.
In this embodiment, the cross-section of casing is circular hollow structure, can provide installation space for fuel cell, and the nimble setting of interior space of being convenient for improves space utilization simultaneously.
In some embodiments of the invention, the housing is a hollow structure having a rectangular cross section.
In this embodiment, the cross-section of casing is rectangular hollow structure, can provide installation space for fuel cell, and the nimble setting of interior space of being convenient for improves space utilization simultaneously.
The technical scheme provided by the invention has at least the following beneficial effects: mixing ferric oxide, nickel oxide and copper oxide to obtain mixed powder, mixing the mixed powder with an organic solvent to obtain a first mixed material, printing the first mixed material on an anode preform to form a first battery anode on the anode preform, and sintering the first battery anode to obtain a target battery anode.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the related art will be briefly described below, and it will be apparent to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic flow chart of a method for preparing a battery anode according to an embodiment of the present invention;
FIG. 2 is a second flow chart of a method for manufacturing a battery anode according to an embodiment of the present invention;
fig. 3 is a schematic block diagram of a fuel cell according to an embodiment of the present invention;
fig. 4 is a schematic block diagram of a battery assembly according to an embodiment of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the embodiment of the invention provides a method for preparing a battery anode, which comprises the following steps:
s102, mixing ferric oxide, nickel oxide and copper oxide to obtain mixed powder;
by carrying out mixed treatment on ferric oxide, nickel oxide and copper oxide, metal is provided for the subsequent preparation of the anode current collector, compared with the anode current collector prepared by gold flakes, silver flakes, platinum flakes or gold paste, silver paste and platinum paste in the related technology, the material is easier to obtain, the cost is lower, and meanwhile, the iron, nickel and copper are more active in chemical property compared with gold, silver and platinum, and are suitable for carrying out subsequent sintering treatment on the anode of the battery, so that the performance requirement of the anode current collector is ensured.
S104, mixing the mixed powder and the organic solvent to obtain a first mixed material;
the mixed powder of iron, nickel and copper is mixed with the organic solvent, so that the mixed powder can be uniformly dispersed in the organic solvent, the uniform current collection of the anode current collector can be ensured, the internal resistance is reduced, a larger current is formed to be output outwards, and the conductivity requirement of the battery is ensured.
S106, printing a first mixed material on the anode preform to form a first battery anode on the anode preform;
Illustratively, the first compound may be printed onto the anode preform by a screen printing process to form an anode current collector on the anode preform, forming a first battery anode. The current collector can be ensured to have good adhesiveness and good ohmic contact characteristic through the screen printing process, and current collection and output after current collection are facilitated.
It will be appreciated that the present application does not impose severe restrictions on the materials of the anode preform, and that the materials of the anode preform may be reasonably selected while meeting performance and cost requirements.
It can be understood that the application does not strictly limit the technological parameters of the screen printing process and the parameters of the specification, the material, the number and the like of the screen, and the screen parameters and the technological parameters can be reasonably set under the condition of meeting the performance requirements.
S108, sintering the first battery anode to obtain the target battery anode.
The first battery anode is sintered, and iron atoms, nickel atoms and copper atoms can be moved from an unstable high-energy position to a lower position of free energy, so that a solid particle system in the mixed slurry of iron, nickel and copper forms a stable dispersed powder system, the free energy of the surface of the anode is improved, particles are contacted and combined, pores are eliminated, and a compact structure is formed.
Mixing treatment is carried out on ferric oxide, nickel oxide and copper oxide to obtain mixed powder, raw materials can be provided for preparation of an anode current collector, mixing treatment is carried out on the mixed powder and an organic solvent to obtain a first mixed material, the dispersed mixed material can be formed, the internal resistance of the formed current collector is reduced, performance requirements are guaranteed, the first mixed material is printed on the anode preform to form a first battery anode on the anode preform, the adhesiveness and ohmic contact characteristics of the anode current collector can be improved, current collection and output are facilitated, sintering treatment is carried out on the first battery anode to obtain a target battery anode, the pores of the anode current collector can be eliminated, a compact structure is formed, stable current conveying of a battery is guaranteed, and a power supply effect is guaranteed.
In the embodiment, ferric oxide, nickel oxide and copper oxide are mixed to obtain mixed powder, the mixed powder and an organic solvent are mixed to obtain a first mixed material, the first mixed material is printed on an anode preform to form a first battery anode on the anode preform, and the first battery anode is sintered to obtain a target battery anode.
In some embodiments of the present invention, mixing ferric oxide, nickel oxide and copper oxide to obtain a mixed powder comprises: and mixing the ferric oxide, the nickel oxide and the copper oxide according to a first preset proportion to obtain mixed powder, wherein the first preset proportion is the mass fraction ratio of the ferric oxide to the nickel oxide to the copper oxide.
In the embodiment, the ferric oxide, the nickel oxide and the copper oxide are mixed according to the mass fraction ratio of the ferric oxide, the nickel oxide and the copper oxide to obtain mixed powder, and the proportion of the iron, the nickel and the copper can be reasonably set, so that the prepared anode current collector has good alloy performance, the conductivity is ensured, the current can be better collected and output after the current is collected, and the stable power supply of the battery is ensured.
In some embodiments of the present invention, in the first preset proportion, the range of the mass fraction of the ferric oxide is greater than or equal to 30% and less than or equal to 40%; the range of the mass fraction of the nickel oxide is more than or equal to 50% and less than or equal to 60%; the range of the mass fraction of the copper oxide is more than or equal to 10% and less than or equal to 20%.
In the embodiment, the preparation cost of the anode current collector is reduced while the current collection and output after the current collection are ensured by controlling the value range of the mass fraction of the ferric oxide to be more than or equal to 30 percent and less than or equal to 40 percent, the value range of the mass fraction of the nickel oxide to be more than or equal to 50 percent and less than or equal to 60 percent and the value range of the mass fraction of the copper oxide to be more than or equal to 10 percent and less than or equal to 20 percent.
It is understood that the present application does not impose strict restrictions on the mass fractions of ferric oxide, nickel oxide and copper oxide, and flexible selection of the mass fractions of ferric oxide, nickel oxide and copper oxide can be made under the condition of meeting the process requirements.
In some embodiments of the present application, mixing the mixed powder with the organic solvent to obtain a first mixed material includes: and mixing the mixed powder and the organic solvent on a mixer to obtain a first mixed material.
In this embodiment, carry out the mixing treatment to mixed powder and organic solvent on the blendor, can guarantee the mixing effect of compounding, be convenient for carry out reasonable control to the compounding process simultaneously to guarantee follow-up with the even printing of compounding on the positive pole prefabrication body, obtain inseparable positive pole mass flow body structure, guarantee the conductivity of positive pole mass flow body, thereby transport electric current that can be stable guarantees the power supply effect.
It is understood that the application does not limit the specific process parameters and specific structure of the mixer strictly, and can reasonably select the mixer and set the working parameters of the mixer, such as voltage, current, power, etc., under the condition of meeting the process requirements and the cost requirements.
In some embodiments of the present invention, mixing the mixed powder and the organic solvent on a blender to obtain a first blend comprises: and at a first preset temperature, running on a mixer at a first preset rotating speed for a first preset time period to mix the mixed powder and the organic solvent, so as to obtain a first mixed material.
In this embodiment, through the restriction of the first preset temperature, the first preset rotational speed and the first preset duration, the mixing effect of the first mixed material and the organic solvent is ensured, so that the mixed powder and the organic solvent can be fully mixed to form a uniform dispersion powder system, the first mixed material is ensured to be uniformly printed on the anode preform, a compact anode current collector structure is obtained, the conductivity of the anode current collector is ensured, the stable conveying current is ensured, and the power supply effect is ensured.
In some embodiments of the present invention, the value range of the first preset temperature is greater than or equal to 90 ℃ and less than or equal to 150 ℃; the value range of the first preset rotating speed is more than or equal to 100 revolutions per minute and less than or equal to 200 revolutions per minute; the value range of the first preset time length is more than or equal to 10 hours and less than or equal to 20 hours.
In this embodiment, the value range of the first preset temperature is set to be 90 degrees celsius or more and 150 degrees celsius or less; the value range of the first preset rotating speed is set to be more than or equal to 100 revolutions per minute and less than or equal to 200 revolutions per minute; the value range of the first preset duration is set to be more than or equal to 10 hours and less than or equal to 20 hours, and the mixing process can be reasonably controlled, so that the first mixing material which is uniformly dispersed is obtained, the first mixing material is ensured to be uniformly printed on an anode prefabricated body, a compact anode current collector structure is obtained, the conductivity of the anode current collector is ensured, and the power supply effect is ensured.
In some embodiments of the invention, the organic solvent comprises at least ethanol, a dispersant.
In the embodiment, the dispersing agent can ensure that the first powder is suspended in ethanol and does not delaminate, so that the stability of the first powder is ensured, and the dispersing agent is used as slurry in a screen printing process and a sintering process, and meets the preparation requirement of an anode current collector.
In some embodiments of the present invention, the mass fraction ratio of ethanol in the organic solvent ranges from 40% to 50%.
In the embodiment, the distribution ratio of the ethanol in the organic solvent can be reasonably controlled by enabling the value range of the mass fraction ratio of the ethanol in the organic solvent to be more than or equal to 40% and less than or equal to 50%, so that the dispersion effect of the first powder in the mixed material is ensured, the follow-up preparation of the anode current collector with compact structure is ensured, the conductivity of the anode current collector is ensured, meanwhile, the current can be stably conveyed, and the power supply effect is ensured.
In some embodiments of the invention, the dispersant comprises at least ethylcellulose, fish oil, isopropanol, polyvinyl butyral.
In the embodiment, ethyl cellulose, fish oil, isopropanol, polyvinyl butyral and ethanol are mutually insoluble, and base cellulose, fish oil, isopropanol and polyvinyl butyral can be strongly adsorbed at a place with high coverage rate of the particle surface and fully spread to form an adsorption steric hindrance layer with a certain thickness, so that powder particles are in a suspension state, and the dispersion effect of the first powder is ensured.
In some embodiments of the invention, the mass fraction ratio of ethylcellulose in the organic solvent ranges from 5% or more to 10% or less; the range of the mass fraction ratio of the fish oil in the organic solvent is more than or equal to 3% and less than or equal to 5%; the value range of the mass fraction ratio of the isopropanol in the organic solvent is more than or equal to 13% and less than or equal to 20%; the range of the mass fraction ratio of the polyvinyl butyral in the organic solvent is more than or equal to 3% and less than or equal to 5%; the organic solvent comprises other solutes, and the range of the mass fraction ratio of the other solutes in the organic solvent is more than or equal to 20% and less than or equal to 30%.
In the embodiment, the mass fraction of the ethyl cellulose, the fish oil, the isopropyl alcohol and the polyvinyl butyral in the organic solvent is controlled, so that the proportion of the dispersing agent can be reasonably controlled, the first powder is ensured to suspend in the ethanol and not to delaminate, the stable suspension effect of the first powder is ensured, the sintering characteristic of the anode current collector is ensured, and the compactness, the porosity and the mechanical property of the sintered powder are ensured.
Referring to fig. 2, in some embodiments of the invention, sintering a first cell anode to obtain a target cell anode comprises:
s202, raising the temperature from room temperature to a first sintering temperature at a first temperature change speed, and performing sintering treatment on the first battery anode for a second preset time length to obtain a sintered battery anode;
s204, increasing the second temperature change speed from the first sintering temperature to the second sintering temperature, and performing sintering treatment on the sintered battery anode for a third preset time length to obtain the target battery anode.
In the embodiment, secondary sintering treatment is carried out on the first battery anode, so that particles of the anode current collector are smaller, the economical degree and tap density are guaranteed, the large and concentrated granularity of the anode current collector is guaranteed, the physical processing performance is guaranteed, the specific capacity of materials is reduced, and the electrical circulation performance and the high-temperature storage performance of the battery anode are improved.
In some embodiments of the present application, the first temperature change speed has a value range of 0.5 degrees celsius per minute or more and 1.5 degrees celsius per minute or less; the value range of the first sintering temperature is more than or equal to 400 ℃ and less than or equal to 450 ℃; the temperature range of room temperature is 20 degrees celsius to 25 degrees celsius.
In this embodiment, by controlling the first temperature change rate and the first sintering temperature, the primary sintering of the battery anode can be controlled, and the condition of uneven particle size distribution of the battery anode can be improved, thereby ensuring the conductivity of the battery anode.
It is understood that the present application does not impose strict restrictions on the first temperature change rate and the first sintering temperature, and that the values of the first temperature change rate and the first sintering temperature may be reasonably selected under the condition of meeting the process requirements and the cost requirements.
In some embodiments of the present application, the value range of the second preset duration is greater than or equal to 120 minutes and less than or equal to 300 minutes.
In this embodiment, by controlling the second preset period of time, the sintering effect of the battery anode in the primary sintering process can be ensured, and indexes such as tap density, specific surface area, specific capacity, and cycle capacity retention rate of the battery anode are improved, so that the physical processing performance of the battery anode is ensured.
It can be understood that the present application does not strictly limit the second preset duration, and the value of the second preset duration can be reasonably selected under the condition of meeting the process requirement and the cost requirement.
In some embodiments of the present application, the second temperature change rate has a value in a range of 2 degrees celsius per minute or more and 5 degrees celsius per minute or less; the value range of the second sintering temperature is more than or equal to 960 ℃ and less than or equal to 1200 ℃.
In the embodiment, the secondary sintering process of the battery anode can be controlled by controlling the second temperature change speed and the second sintering temperature, so that the condition of uneven particle size distribution of the battery anode is further improved, indexes such as tap density, specific surface area, specific capacity, circulation capacity retention rate and the like of the battery anode are improved, the average particle size of an anode current collector is effectively increased, the tap density is improved, the specific surface area is reduced, the internal stress of less materials is reduced, and the electrochemical performance is improved.
It is understood that the present application does not impose strict restrictions on the second temperature change rate and the second sintering temperature, and that the values of the second temperature change rate and the second sintering temperature may be reasonably selected under the condition of meeting the process requirements and the cost requirements.
In some embodiments of the present application, the value range of the third preset duration is greater than or equal to 120 minutes and less than or equal to 300 minutes.
In the embodiment, the sintering effect of the battery anode in the secondary sintering process can be ensured by controlling the third preset time length, and the method has simple process, lower preparation and processing cost compared with precious metals such as gold, silver, platinum and the like in the related technology, and is easy for large-scale industrialized production.
It can be understood that the present application does not strictly limit the third preset time period, and the numerical value of the third preset time period can be reasonably selected under the condition of meeting the process requirement and the cost requirement.
Based on the same inventive concept, the battery anode of the embodiment of the present application is manufactured by the manufacturing method of the battery anode of any one of the above embodiments.
The battery anode of the embodiment of the application is made by the method for preparing the battery anode of any embodiment, and has all the beneficial effects of the method for preparing the battery anode of any possible implementation manner, which are not described herein.
Based on the same inventive concept, referring to fig. 3, a fuel cell 300 of an embodiment of the present application includes: a battery cathode 302; an electrolyte layer 304; and a battery anode 306 of any of the embodiments described above, the electrolyte layer 304 being located between the battery cathode 302 and the battery anode 306.
The fuel cell 300 of the present invention includes a cell cathode 302, an electrolyte layer 304, and a cell anode 306 according to any of the above embodiments, wherein the electrolyte layer 304 has all the advantages of the cell anode 306 according to any of the above possible implementations between the cell cathode 302 and the cell anode 306, and is not described herein.
The fuel cell 300 of the present invention may be a solid oxide fuel cell in which fuel gas is continuously supplied to the side of the cell anode 306, for example: hydrogen gas [ ]) Methane (/ ->) City gas, etc., the surface of the cell anode 306 having a catalytic effect adsorbs the fuel gas and diffuses through the porous structure of the cell anode 306 to the interface of the cell anode 306 and the electrolyte layer 304. Oxygen or air is continuously introduced into one side of the battery cathode 302, and oxygen is adsorbed on the surface of the battery cathode 302 with a porous structure, so that +.>Get electrons become +.>Under the action of chemical potential, +.>Enters the solid oxygen ion conductor that functions as electrolyte layer 304, diffuses due to the concentration gradient, eventually reaches the interface of solid electrolyte layer 304 and cell anode 306, reacts with the fuel gas, and the lost electrons return to the cathode through an external circuit.
Based on the same inventive concept, referring to fig. 4, a battery assembly 400 includes: a housing 402; and at least one fuel cell 300 of any of the above embodiments, the fuel cell 300 being located within the housing 402.
The battery assembly 400 of the present invention includes a housing 402 and the fuel cell 300 of any of the foregoing embodiments, where the housing 402 can provide an installation space for the fuel cell 300 and protect the fuel cell 300, and the fuel cell 300 is located in the housing 402, and all the advantages of any of the foregoing possible implementations are not described herein.
It can be understood that the single cells have limited voltage and limited power, so that in order to make the solid oxide fuel cell possible for practical application, the power of the solid oxide fuel cell needs to be increased, and a plurality of single cells are assembled into a battery pack in a serial, parallel or series-parallel manner.
In some embodiments of the invention, the housing 402 is a hollow structure with a circular cross-section.
In this embodiment, the housing 402 has a hollow structure with a circular cross section, which can provide an installation space for the fuel cell 300 while facilitating flexible arrangement of the internal space and improving space utilization.
In some embodiments of the invention, the housing 402 is a hollow structure having a rectangular cross-section.
In this embodiment, the housing 402 has a rectangular hollow structure in cross section, which can provide an installation space for the fuel cell 300, while facilitating flexible arrangement of the internal space and improving space utilization.
It is understood that the housing 402 can be circular or rectangular in cross-section and can form a flat tubular solid fuel cell stack.
The application does not impose strict restrictions on the specific shape of the cross section of the housing 402 and the structure of the solid fuel cell stack, and can be reasonably selected according to cost and process requirements under the condition of meeting installation requirements.
Example 1
A method for preparing a novel flat tube SOFC (Solid Oxide Fuel Cell ) single cell anode current collector, comprising:
step S1: and (3) preparing current collector powder A: fe (Fe) 2 O 3 : niO: cuo=30%: 50%:10% (mass fraction);
step S2: mixing the current collecting powder A with an organic solvent B to form a mixture C, wherein the organic solvent B comprises the following components: 40% of ethanol, 5% of ethyl cellulose, 3% of fish oil (mass fraction), 3% of PVB and 13% of isopropanol; and (3) flowing powder A: organic solvent b=1: 3 (mass fraction), placing on a mixer for mixing, and setting parameters: the revolution is 100r/min, the temperature is 90 ℃ and the time is 10h;
step S3: screen printing the mixed material C on the surface of the anode of the flat tube battery through a screen printing process;
Step S4: placing the flat tube battery subjected to silk screen printing in an atmosphere furnace for sintering, wherein the sintering stage 1 is as follows: heating to 420 ℃ at room temperature (1 ℃/min), and preserving heat for 120min, wherein the atmosphere is as follows: air/O 2 The flow rate is 100sccm; sintering stage 2: the temperature is raised to 960 ℃ at 420 ℃ and the temperature is kept for 120min.
The thickness of the SOFC single cell anode current collector is 15 micrometers, and the flat tubular solid fuel cell is prepared. The operating conditions for testing the performance of the battery were: contains high purity H 2 Is fuel gas, and the flow is 120sccm; air is oxidant, flow is 450sccm, open circuit voltage at 500 ℃ is 1.12V, and power density can reach 0.23W/cm 2 。
Example 2
A novel preparation method of a flat tube type SOFC single cell anode current collector comprises the following steps:
step S1: and (3) preparing current collector powder A: fe (Fe) 2 O 3 : niO: cuo=40%: 60 percent: 20% (mass fraction);
step S2: mixing the current collecting powder A with an organic solvent B to form a mixture C, wherein the organic solvent B comprises the following components: 50% of ethanol, 10% of ethyl cellulose, 5% of fish oil (mass fraction), 5% of PVB and 20% of isopropanol; and (3) flowing powder A: organic solvent b=1: 8 (mass fraction), placing on a mixer for mixing, and setting parameters: the revolution is 200r/min, the temperature is 150 ℃ and the time is 20h;
step S3: screen printing the mixed material C on the surface of the anode of the flat tube battery through a screen printing process;
Step S4: placing the flat tube battery subjected to silk screen printing in an atmosphere furnace for sintering, wherein the sintering stage 1 is as follows: heating to 420 ℃ (1 ℃/min) at room temperature, and preserving heat for 300min, wherein the atmosphere is as follows: air/O 2 The flow rate is 500sccm; sintering stage 2: the temperature is raised to 1200 ℃ at 420 ℃ and is kept for 300min.
The performances of the novel flat tube type SOFC single cell anode current collector prepared under the process conditions of the preparation examples I to II for preparing SOFC are shown in the following table 1:
TABLE 1
Preparation example one Preparation example two
Preparation of current collector powder A Fe2O3: niO: cuo=30%: 50%:10% (mass fraction) Fe2O3: niO: cuo=40%: 60 percent: 20% (mass fraction)
Organic solvent B component 40% of ethanol, 5% of ethyl cellulose and 3% of fish oil (mass fraction) Number), PVB3%, isopropanol 13%; and (3) flowing powder A: organic solvents B=1: 3 (mass fraction) Ethanol 50%, ethyl cellulose 10%, fish oil 5% (mass fraction) Number), PVB5%, isopropanol 20%; and (3) flowing powder A: organic solvent b= 1:8 (mass fraction)
S2 parameter setting The revolution is 100r/min, the temperature is 90 ℃ and the time is 10h The revolution is 200r/min, the temperature is 150 ℃ and the time is 20h;
s4 sintering stage 1 Heating to 420 deg.C (1 deg.C/min), and maintaining the temperature 120min, atmosphere: air/O2, flow 100sccm Heating to 420 deg.C (1 deg.C/min), maintaining for 300min, atmosphere: air/O2, flow 500sccm;
s4 sintering stage 2 Heating to 960 deg.C at 420 deg.C, and maintaining for 120min The temperature is raised to 1200 ℃ at 420 ℃ and is kept for 300min.
Open circuit potential (V) 1.12 1.15
Power density (W/cm 2) 0.23 0.34
The thickness of the SOFC single cell anode current collector is 15 micrometers, and the flat tubular solid fuel cell is prepared. The operating conditions for testing the performance of the battery were: contains high purity H 2 Is fuel gas, and the flow is 180sccm; air is oxidant, the flow is 500sccm, the open circuit voltage at 500 ℃ is 1.15V, and the power density can reach 0.34W/cm 2 。
While this specification contains many specific implementation details, these should not be construed as limitations on the scope of any invention or of what may be claimed, but rather as descriptions of features of specific embodiments of particular inventions. Certain features that are described in this specification in the context of separate embodiments can also be implemented in combination in a single embodiment. On the other hand, the various features described in the individual embodiments may also be implemented separately in the various embodiments or in any suitable subcombination. Furthermore, although features may be acting in certain combinations and even initially claimed as such, one or more features from a claimed combination can in some cases be excised from the combination, and the claimed combination may be directed to a subcombination or variation of a subcombination.
Thus, particular embodiments of the subject matter have been described. Other embodiments are within the scope of the following claims. In some cases, the actions recited in the claims can be performed in a different order and still achieve desirable results. Furthermore, the processes depicted in the accompanying drawings are not necessarily required to be in the particular order shown, or sequential order, to achieve desirable results. In some implementations, multitasking and parallel processing may be advantageous.
It should be noted that in this document, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The foregoing is only a specific embodiment of the invention to enable those skilled in the art to understand or practice the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (20)

1. A method for preparing a battery anode, comprising:
mixing ferric oxide, nickel oxide and copper oxide to obtain mixed powder;
mixing the mixed powder with an organic solvent to obtain a first mixed material;
printing the first mix on an anode preform to form a first cell anode on the anode preform;
and sintering the first battery anode to obtain the target battery anode.
2. The method for preparing a battery anode according to claim 1, wherein the mixing treatment of ferric oxide, nickel oxide and copper oxide to obtain mixed powder comprises:
And mixing the ferric oxide, the nickel oxide and the copper oxide according to a first preset proportion to obtain the mixed powder, wherein the first preset proportion is the mass fraction ratio of the ferric oxide to the nickel oxide to the copper oxide.
3. The method for producing a battery anode according to claim 2, wherein,
in the first preset proportion, the range of the mass fraction of the ferric oxide is more than or equal to 30% and less than or equal to 40%;
the range of the mass fraction of the nickel oxide is more than or equal to 50% and less than or equal to 60%;
the range of the mass fraction of the copper oxide is more than or equal to 10% and less than or equal to 20%.
4. The method of claim 1, wherein the mixing the mixed powder with the organic solvent to obtain the first mixed material comprises:
and mixing the mixed powder and the organic solvent on a mixer to obtain the first mixed material.
5. The method of claim 4, wherein mixing the mixed powder and the organic solvent in a mixer to obtain the first mixed material comprises:
And at a first preset temperature, running on the mixer at a first preset rotating speed for a first preset time period to mix the mixed powder and the organic solvent, so as to obtain the first mixed material.
6. The method for producing a battery anode according to claim 5, wherein,
the value range of the first preset temperature is more than or equal to 90 ℃ and less than or equal to 150 ℃;
the value range of the first preset rotating speed is more than or equal to 100 revolutions per minute and less than or equal to 200 revolutions per minute;
the value range of the first preset time length is more than or equal to 10 hours and less than or equal to 20 hours.
7. The method for producing a battery anode according to any one of claims 1 to 6, wherein,
the organic solvent at least comprises ethanol and a dispersing agent.
8. The method for producing a battery anode according to claim 7, wherein,
the value range of the mass fraction ratio of the ethanol in the organic solvent is more than or equal to 40% and less than or equal to 50%.
9. The method for producing a battery anode according to claim 7, wherein,
the dispersing agent at least comprises ethyl cellulose, fish oil, isopropanol and polyvinyl butyral.
10. The method for producing a battery anode according to claim 9, wherein,
the value range of the mass fraction ratio of the ethyl cellulose in the organic solvent is more than or equal to 5% and less than or equal to 10%;
the range of the mass fraction ratio of the fish oil in the organic solvent is more than or equal to 3% and less than or equal to 5%;
the value range of the mass fraction ratio of the isopropanol in the organic solvent is more than or equal to 13% and less than or equal to 20%;
the range of the mass fraction ratio of the polyvinyl butyral in the organic solvent is more than or equal to 3% and less than or equal to 5%;
the organic solvent also comprises other solutes, and the range of the mass fraction ratio of the other solutes in the organic solvent is more than or equal to 20% and less than or equal to 30%.
11. The method of any one of claims 1 to 6, wherein the sintering the first battery anode to obtain a target battery anode comprises:
raising the temperature from room temperature to a first sintering temperature at a first temperature change speed, and performing sintering treatment on the first battery anode for a second preset time period to obtain a sintered battery anode, wherein the temperature range of the room temperature is 20-25 ℃;
And increasing the second temperature change speed from the first sintering temperature to the second sintering temperature, and performing sintering treatment on the sintered battery anode for a third preset time length to obtain the target battery anode.
12. The method for producing a battery anode according to claim 11, wherein,
the value range of the first temperature change speed is more than or equal to 0.5 ℃ per minute and less than or equal to 1.5 ℃ per minute;
the value range of the first sintering temperature is more than or equal to 400 ℃ and less than or equal to 450 ℃.
13. The method for producing a battery anode according to claim 11, wherein,
the value range of the second preset time length is more than or equal to 120 minutes and less than or equal to 300 minutes.
14. The method for producing a battery anode according to claim 11, wherein,
the value range of the second temperature change speed is more than or equal to 2 ℃ per minute and less than or equal to 5 ℃ per minute;
the value range of the second sintering temperature is more than or equal to 960 ℃ and less than or equal to 1200 ℃.
15. The method for producing a battery anode according to claim 11, wherein,
the value range of the third preset time length is more than or equal to 120 minutes and less than or equal to 300 minutes.
16. A battery anode, characterized in that,
the battery anode made by the method of making a battery anode as claimed in any one of claims 1 to 15.
17. A fuel cell, the fuel cell comprising:
a battery cathode;
an electrolyte layer;
the battery anode of claim 16, the electrolyte layer being located between the battery cathode and the battery anode.
18. A battery assembly, the battery assembly comprising:
a housing;
and at least one fuel cell of claim 17, said fuel cell being located within said housing.
19. The battery assembly of claim 18, wherein the battery assembly comprises,
the shell is of a hollow structure with a circular section.
20. The battery assembly of claim 18, wherein the battery assembly comprises,
the shell is of a hollow structure with a rectangular section.
CN202311106902.9A 2023-08-30 2023-08-30 Battery anode, preparation method thereof, fuel battery and battery assembly Active CN116845256B (en)

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