CN111463407A - Positive electrode-gel polymer electrolyte integrated pole piece, preparation and lithium ion battery - Google Patents

Positive electrode-gel polymer electrolyte integrated pole piece, preparation and lithium ion battery Download PDF

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CN111463407A
CN111463407A CN202010277618.8A CN202010277618A CN111463407A CN 111463407 A CN111463407 A CN 111463407A CN 202010277618 A CN202010277618 A CN 202010277618A CN 111463407 A CN111463407 A CN 111463407A
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positive electrode
gel polymer
solution
pole piece
polymer electrolyte
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CN111463407B (en
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余凤
陈永
赵灵珠
章宏兵
孙志鹏
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Hainan University
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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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0407—Methods of deposition of the material by coating on an electrolyte layer
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides an integrated preparation method of a positive electrode-gel polymer electrolyte, and a prepared integrated pole piece and a lithium ion battery comprising the integrated pole piece. The method comprises the following steps: preparing modified gelatin: dissolving gelatin in phosphoric acid buffer solution, dripping methacrylic anhydride for reaction, dialyzing and freeze-drying; preparing a positive electrode binder solution: preparing aqueous solution from modified gelatin, adding PEGDA and photoinitiator, and mixing; 3, preparing positive electrode slurry: mixing and grinding a positive electrode material, a conductive agent and a positive electrode binder solution; preparing a gel polymer precursor solution: dissolving the modified gelatin into a water solution, adding PEGDA and a photoinitiator, and mixing; manufacturing an integrated pole piece; coating the positive slurry on an aluminum foil, performing ultraviolet curing, drying, cutting and weighing; and (3) blade-coating a precursor solution, carrying out ultraviolet curing, drying and drying to obtain a positive pole piece, and soaking the positive pole piece in electrolyte to obtain an integrated pole piece. The invention provides an effective scheme for the contact between the gel polymer electrolyte and the electrode interface, improves the interface adhesion and impedance, and improves the battery performance.

Description

Positive electrode-gel polymer electrolyte integrated pole piece, preparation and lithium ion battery
Technical Field
The invention relates to an integrated preparation method of a positive electrode-gel polymer electrolyte, an integrated pole piece and a lithium ion battery comprising the integrated pole piece, and belongs to the technical field of lithium ion batteries.
Background
The interfacial contact properties of different electrolytes with electrodes vary greatly. Conventional liquid electrolytes wet the electrodes well, while solid electrolytes are in rigid contact with the electrodes, which results in solid electrolytes that not only have low room temperature ionic conductivity but also have high interfacial resistance. Although the gel polymer electrolyte belongs to the category of solid polymer electrolytes, compared with pure solid polymer electrolytes, the gel polymer electrolyte can improve the interface compatibility between the electrolyte and an electrode to a certain extent, but as the electrolyte is continuously consumed in the circulation process, the contact interface between the gel polymer electrolyte and the electrode develops towards the direction of the solid electrolyte, and the interface compatibility is poor.
Therefore, there is a need to provide an effective solution to improve the interfacial contact between the gel polymer electrolyte and the electrode.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an integrated preparation method of a positive electrode-gel polymer electrolyte, an integrated pole piece and a lithium ion battery comprising the integrated pole piece.
In order to achieve the above technical object, the present invention adopts the following technical solutions.
The invention provides an integrated preparation method of a positive electrode-gel polymer electrolyte, which comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving gelatin powder in Phosphate Buffered Saline (PBS);
step 1.2, slowly dripping Methacrylic Anhydride (MA) and stirring for reaction;
and (3) dialyzing the solution after the reaction in the step 1.3, and freeze-drying to obtain a white foamy solid, namely the modified gelatin.
Specifically, in step 1.1, the gelatin powder is 5-10g, and the phosphate buffer solution is 100m L PBS buffer solution with pH of 7;
the dissolution temperature in step 1.1 is 50-60 ℃, and the dissolution is preferably accelerated by stirring;
in the step 1.2, methacrylic anhydride is 4-8m L, the reaction temperature is 50-60 ℃, and the reaction time is 6-12 h;
in step 1.3, the dialysis time is 3-5 days, the freezing temperature is-20 ℃, and the freezing time is 24-48 h.
Step 2, preparing a positive electrode binder solution
Dissolving the modified gelatin prepared in the step 1 to prepare an aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
specifically, the modified gelatin is prepared into a solution with the mass percentage of 3-8%, preferably, in a water bath at 40 ℃;
the mass ratio of the modified gelatin to the polyethylene glycol diacrylate (PEGDA) is 5: 1-1: 1;
the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.05-0.5 wt%.
Step 3, preparing anode slurry
Mixing and grinding a positive electrode material, a conductive agent and the positive electrode binder solution prepared in the step 2 to obtain positive electrode slurry;
specifically, the cathode material is lithium iron phosphate, and the using amount of the lithium iron phosphate is 0.064 g;
the conductive agent is KB carbon, and the using amount of the conductive agent is 0.008 g;
the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1;
the mixing and grinding time is 5-10 min.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 to prepare an aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution;
specifically, the modified gelatin is prepared into a 5-10% solution, preferably, in a water bath at 40 ℃;
the mass ratio of the modified gelatin to the polyethylene glycol diacrylate (PEGDA) is 2:1-1: 2;
the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.05-0.5 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
Coating the positive electrode slurry obtained in the step (3) on a current collector in a blade mode, curing under an ultraviolet lamp, drying, and weighing cut pieces;
specifically, the current collector is an aluminum foil;
the curing time is 60-120 s;
the drying condition is drying in a blast oven at 80 ℃ for 3-5 h;
then, blade-coating the gel polymer precursor solution prepared in the step (4) on the positive electrode plate, curing under an ultraviolet lamp again, drying, and drying to obtain a positive electrode plate;
specifically, the curing time is 60-120 s;
the drying condition is that the drying is carried out for 3 to 5 hours by a forced air oven at the temperature of 80 ℃;
the drying condition is that the mixture is stored for 24 to 36 hours in a vacuum drying oven at the temperature of 110 ℃;
and soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
The invention also provides an anode-gel polymer electrolyte integrated pole piece which is prepared by adopting the method.
The invention also provides a lithium ion battery which comprises the positive electrode-gel polymer electrolyte integrated pole piece, and the lithium ion battery has the advantages of good cycle stability, high battery capacity retention rate and good coulombic efficiency; and the positive electrode-gel polymer electrolyte integrated pole piece can well improve the problem of interface impedance between the electrode and the polymer electrolyte, thereby improving the performance of the battery.
By adopting the technical scheme, the invention achieves the following technical effects.
The present invention proposes an effective solution to improve the interfacial contact between the gel polymer electrolyte and the electrode. The design of integrating the gel polymer electrolyte and the anode is provided, and the integrated anode-gel polymer electrolyte material is prepared by a solvent-free ultraviolet curing method.
The invention can not only enhance the interface adhesive force between the positive electrode layer and the gel polymer electrolyte membrane, thereby improving the interface impedance and improving the performance of the battery; meanwhile, the pores in the positive electrode are filled with the gel polymer electrolyte, so that the wetting capacity of the gel polymer electrolyte on the positive electrode is improved.
In addition, the invention also has the following technical effects:
the positive pole binding agent solution prepared by the method has good dispersion effect and strong viscosity, and the prepared pole piece has stable structure and is not easy to chap.
The lithium ion battery prepared by the method has better cycle stability, high battery capacity retention rate and good coulombic efficiency.
The positive electrode-gel polymer electrolyte integrated pole piece has the advantages of simple preparation process, low preparation cost and no environmental pollution.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to these drawings without inventive effort.
FIG. 1 is a schematic diagram of a preparation method of the positive electrode-gel polymer integrated pole piece of the invention;
fig. 2 is a surface topography and profile topography map of the positive electrode-gel polymer electrolyte integrated pole piece prepared in example 1 of the present invention and a comparison map of the non-integrated pole piece.
Fig. 3 is a cycle performance test chart of the lithium ion battery and the non-integrated battery of example 8 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
The invention provides an integrated preparation method of a positive electrode-gel polymer electrolyte, a prepared integrated pole piece of the positive electrode-gel polymer electrolyte and a lithium ion battery comprising the integrated pole piece.
Referring to fig. 1, an integrated preparation method of a cathode-gel polymer electrolyte includes the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving gelatin powder in Phosphate Buffered Saline (PBS);
step 1.2, slowly dripping Methacrylic Anhydride (MA) and stirring for reaction;
and (3) dialyzing the solution after the reaction in the step 1.3, and freeze-drying to obtain a white foamy solid, namely the modified gelatin.
Specifically, in step 1.1, the gelatin powder is 5-10g, and the phosphate buffer solution is 100m L PBS buffer solution with pH of 7;
the dissolution temperature in step 1.1 is 50-60 ℃, and the dissolution is preferably accelerated by stirring;
in the step 1.2, methacrylic anhydride is 4-8m L, the reaction temperature is 50-60 ℃, and the reaction time is 6-12 h;
in step 1.3, the dialysis time is 3-5 days, the freezing temperature is-20 ℃, and the freezing time is 24-48 h.
Step 2, preparing a positive electrode binder solution
Dissolving the modified gelatin prepared in the step 1 to prepare an aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
specifically, the modified gelatin is prepared into a 3-8% solution, preferably, in a water bath at 40 ℃;
the mass ratio of the modified gelatin to the polyethylene glycol diacrylate (PEGDA) is 5: 1-1: 1;
the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.05-0.5 wt%.
Step 3, preparing anode slurry
Mixing and grinding a positive electrode material, a conductive agent and the positive electrode binder solution prepared in the step 2 to obtain positive electrode slurry;
specifically, the cathode material is lithium iron phosphate, and the using amount of the lithium iron phosphate is 0.064 g;
the conductive agent is KB carbon, and the using amount of the conductive agent is 0.008 g;
the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1;
the mixing and grinding time is 5-10 min.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 to prepare an aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution;
specifically, the modified gelatin is prepared into a 5-10% solution, preferably, in a water bath at 40 ℃;
the mass ratio of the modified gelatin to the polyethylene glycol diacrylate (PEGDA) is 2:1-1: 2;
the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.05-0.5 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
Coating the positive electrode slurry obtained in the step (3) on a current collector in a blade mode, curing under an ultraviolet lamp, drying, and weighing cut pieces;
specifically, the current collector is an aluminum foil;
the curing time is 60-120 s;
the drying condition is drying in a blast oven at 80 ℃ for 3-5 h;
then, blade-coating the gel polymer precursor solution prepared in the step (4) on the positive electrode plate, curing under an ultraviolet lamp again, drying, and drying to obtain a positive electrode plate;
specifically, the curing time is 60-120 s;
the drying condition is that the drying is carried out for 3 to 5 hours by a forced air oven at the temperature of 80 ℃;
the drying condition is that the mixture is stored for 24 to 36 hours in a vacuum drying oven at the temperature of 110 ℃;
and soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
The above method is described below by specific examples, and it should be noted that, although the following examples are prepared according to the corresponding parameter conditions, the other parameters in the above method are selected for preparation, and the corresponding positive electrode-gel polymer electrolyte integrated pole piece and the lithium battery containing the same can also be prepared.
Example 1
An integrated preparation method of a positive electrode-gel polymer electrolyte comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving 5g of gelatin powder in 100ml of Phosphate Buffered Saline (PBS) with pH of 7, heating to 60 ℃, and stirring to fully dissolve the gelatin powder;
step 1.2, slowly adding 4m L Methacrylic Anhydride (MA) dropwise, stirring for reaction, and continuously reacting for 6 hours at 50 ℃;
dialyzing the solution obtained after the reaction in the step 1.3 for 3d, and freeze-drying the solution at the temperature of minus 20 ℃ for 24h to obtain white foamy solid, namely the modified gelatin.
Step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare a 5% aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
the mass ratio of the modified gelatin to the glycol diacrylate (PEGDA) is 5: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.5 wt%.
Step 3, preparing anode slurry
And (3) mixing and grinding the positive electrode material, the conductive agent and the positive electrode binder solution prepared in the step (2) for 5min to obtain positive electrode slurry.
Wherein the anode material is 0.064g of lithium iron phosphate; the conductive agent is KB carbon 0.008 g; the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 10% aqueous solution, then adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution. The mass ratio of the gelatin to the polyethylene glycol diacrylate (PEGDA) is 1: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.5 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
And (3) coating the positive electrode slurry on an aluminum foil in a scraping manner, carrying out ultraviolet curing for 60s, taking out, drying for 3h at 80 ℃ in a blast oven, weighing cut pieces after the surface of the electrode piece is basically dried, then coating the gel polymer precursor solution prepared in the step (4) on the electrode piece in a scraping manner, carrying out ultraviolet irradiation for 60s, drying for 3h in the blast oven at 80 ℃, and then transferring to a vacuum drying oven at 110 ℃ for storage for 24h to obtain the positive electrode piece.
And soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
Example 2
An integrated preparation method of a positive electrode-gel polymer electrolyte comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving 5g of gelatin powder in 100ml of Phosphate Buffered Saline (PBS) with pH of 7, heating to 60 ℃, and stirring to fully dissolve the gelatin powder;
step 1.2, slowly adding 4m L Methacrylic Anhydride (MA) dropwise, stirring for reaction, and continuously reacting for 6 hours at 50 ℃;
dialyzing the solution obtained after the reaction in the step 1.3 for 3d, and freeze-drying the solution at the temperature of minus 20 ℃ for 24h to obtain white foamy solid, namely the modified gelatin.
Step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare a 5% aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
the mass ratio of the modified gelatin to the glycol diacrylate (PEGDA) is 4: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.5 wt%.
Step 3, preparing anode slurry
And (3) mixing and grinding the positive electrode material, the conductive agent and the positive electrode binder solution prepared in the step (2) for 5min to obtain positive electrode slurry.
Wherein the anode material is 0.064g of lithium iron phosphate; the conductive agent is KB carbon 0.008 g; the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 10% aqueous solution, then adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution. The mass ratio of the gelatin to the polyethylene glycol diacrylate (PEGDA) is 1: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.5 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
And (3) coating the positive electrode slurry on an aluminum foil in a scraping manner, carrying out ultraviolet curing for 60s, taking out, drying for 3h at 80 ℃ in a blast oven, weighing cut pieces after the surface of the electrode piece is basically dried, then coating the gel polymer precursor solution prepared in the step (4) on the electrode piece in a scraping manner, carrying out ultraviolet irradiation for 60s, drying for 3h in the blast oven at 80 ℃, and then transferring to a vacuum drying oven at 110 ℃ for storage for 24h to obtain the positive electrode piece.
And soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
Example 3
An integrated preparation method of a positive electrode-gel polymer electrolyte comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving 5g of gelatin powder in 100ml of Phosphate Buffered Saline (PBS) with pH of 7, heating to 60 ℃, and stirring to fully dissolve the gelatin powder;
step 1.2, slowly adding 4m L Methacrylic Anhydride (MA) dropwise, stirring for reaction, and continuously reacting for 6 hours at 50 ℃;
dialyzing the solution obtained after the reaction in the step 1.3 for 3d, and freeze-drying the solution at the temperature of minus 20 ℃ for 24h to obtain white foamy solid, namely the modified gelatin.
Step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare a 5% aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
the mass ratio of the modified gelatin to the glycol diacrylate (PEGDA) is 3: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.5 wt%.
Step 3, preparing anode slurry
And (3) mixing and grinding the positive electrode material, the conductive agent and the positive electrode binder solution prepared in the step (2) for 5min to obtain positive electrode slurry.
Wherein the anode material is 0.064g of lithium iron phosphate; the conductive agent is KB carbon 0.008 g; the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 10% aqueous solution, then adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution. The mass ratio of the gelatin to the polyethylene glycol diacrylate (PEGDA) is 1: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.5 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
And (3) coating the positive electrode slurry on an aluminum foil in a scraping manner, carrying out ultraviolet curing for 60s, taking out, drying for 3h at 80 ℃ in a blast oven, weighing cut pieces after the surface of the electrode piece is basically dried, then coating the gel polymer precursor solution prepared in the step (4) on the electrode piece in a scraping manner, carrying out ultraviolet irradiation for 60s, drying for 3h in the blast oven at 80 ℃, and then transferring to a vacuum drying oven at 110 ℃ for storage for 24h to obtain the positive electrode piece.
And soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12h, and the electricity is usedThe electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
Example 4
An integrated preparation method of a positive electrode-gel polymer electrolyte comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving 5g of gelatin powder in 100ml of Phosphate Buffered Saline (PBS) with pH of 7, heating to 60 ℃, and stirring to fully dissolve the gelatin powder;
step 1.2, slowly adding 4m L Methacrylic Anhydride (MA) dropwise, stirring for reaction, and continuously reacting for 6 hours at 50 ℃;
dialyzing the solution obtained after the reaction in the step 1.3 for 3d, and freeze-drying the solution at the temperature of minus 20 ℃ for 24h to obtain white foamy solid, namely the modified gelatin.
Step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare a 5% aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
the mass ratio of the modified gelatin to the glycol diacrylate (PEGDA) is 2: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.5 wt%.
Step 3, preparing anode slurry
And (3) mixing and grinding the positive electrode material, the conductive agent and the positive electrode binder solution prepared in the step (2) for 5min to obtain positive electrode slurry.
Wherein the anode material is 0.064g of lithium iron phosphate; the conductive agent is KB carbon 0.008 g; the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 10% aqueous solution, then adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution. The mass ratio of the gelatin to the polyethylene glycol diacrylate (PEGDA) is 1: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.5 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
And (3) coating the positive electrode slurry on an aluminum foil in a scraping manner, carrying out ultraviolet curing for 60s, taking out, drying for 3h at 80 ℃ in a blast oven, weighing cut pieces after the surface of the electrode piece is basically dried, then coating the gel polymer precursor solution prepared in the step (4) on the electrode piece in a scraping manner, carrying out ultraviolet irradiation for 60s, drying for 3h in the blast oven at 80 ℃, and then transferring to a vacuum drying oven at 110 ℃ for storage for 24h to obtain the positive electrode piece.
And soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
Example 5
An integrated preparation method of a positive electrode-gel polymer electrolyte comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving 5g of gelatin powder in 100ml of Phosphate Buffered Saline (PBS) with pH of 7, heating to 60 ℃, and stirring to fully dissolve the gelatin powder;
step 1.2, slowly adding 4m L Methacrylic Anhydride (MA) dropwise, stirring for reaction, and continuously reacting for 6 hours at 50 ℃;
dialyzing the solution obtained after the reaction in the step 1.3 for 3d, and freeze-drying the solution at the temperature of minus 20 ℃ for 24h to obtain white foamy solid, namely the modified gelatin.
Step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare a 5% aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
the mass ratio of the modified gelatin to the glycol diacrylate (PEGDA) is 1: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.5 wt%.
Step 3, preparing anode slurry
And (3) mixing and grinding the positive electrode material, the conductive agent and the positive electrode binder solution prepared in the step (2) for 5min to obtain positive electrode slurry.
Wherein the anode material is 0.064g of lithium iron phosphate; the conductive agent is KB carbon 0.008 g; the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 10% aqueous solution, then adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution. The mass ratio of the gelatin to the polyethylene glycol diacrylate (PEGDA) is 1: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.5 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
And (3) coating the positive electrode slurry on an aluminum foil in a scraping manner, carrying out ultraviolet curing for 60s, taking out, drying for 3h at 80 ℃ in a blast oven, weighing cut pieces after the surface of the electrode piece is basically dried, then coating the gel polymer precursor solution prepared in the step (4) on the electrode piece in a scraping manner, carrying out ultraviolet irradiation for 60s, drying for 3h in the blast oven at 80 ℃, and then transferring to a vacuum drying oven at 110 ℃ for storage for 24h to obtain the positive electrode piece.
And soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
Example 6
An integrated preparation method of a positive electrode-gel polymer electrolyte comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, 10g of gelatin powder is dissolved in 100ml of Phosphate Buffered Saline (PBS) with pH value of 7, heated to 50 ℃, and stirred to be fully dissolved;
step 1.2, slowly and dropwise adding 8m L of Methacrylic Anhydride (MA), stirring for reaction, and continuously reacting for 12 hours at the temperature of 60 ℃;
dialyzing the solution obtained after the reaction in the step 1.3 for 5d, and freeze-drying the solution at the temperature of minus 20 ℃ for 28h to obtain white foamy solid, namely the modified gelatin.
Step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare a 3% aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
the mass ratio of the modified gelatin to the glycol diacrylate (PEGDA) is 5: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.05 wt%.
Step 3, preparing anode slurry
And (3) mixing and grinding the positive electrode material, the conductive agent and the positive electrode binder solution prepared in the step (2) for 5-10 min to obtain positive electrode slurry.
Wherein the anode material is 0.064g of lithium iron phosphate; the conductive agent is KB carbon 0.008 g; the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 10% aqueous solution, then adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution. The mass ratio of the gelatin to the polyethylene glycol diacrylate (PEGDA) is 2: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.05 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
And (3) coating the positive electrode slurry on an aluminum foil in a scraping manner, carrying out ultraviolet curing for 120s, taking out, drying for 5h at 80 ℃ in a blast oven, weighing cut pieces after the surface of the electrode piece is basically dried, then coating the gel polymer precursor solution prepared in the step (4) on the electrode piece in a scraping manner, carrying out ultraviolet illumination for 120s, then drying for 5h in the blast oven at 80 ℃, and then transferring to a vacuum drying oven at 110 ℃ for storage for 36h to obtain the positive electrode piece.
And soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
Example 7
An integrated preparation method of a positive electrode-gel polymer electrolyte comprises the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin
Step 1.1, dissolving 8g of gelatin powder in 100ml of Phosphate Buffered Saline (PBS) with pH of 7, heating to 55 ℃, and stirring to fully dissolve the gelatin powder;
step 1.2, slowly and dropwise adding 6m L of Methacrylic Anhydride (MA), stirring for reaction, and continuously reacting for 10 hours at 55 ℃;
dialyzing the solution obtained after the reaction in the step 1.3 for 4d, and freeze-drying the solution at the temperature of minus 20 ℃ for 26h to obtain white foamy solid, namely the modified gelatin.
Step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 8% aqueous solution, adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
the mass ratio of the modified gelatin to the glycol diacrylate (PEGDA) is 5: 1; the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.2 wt%.
Step 3, preparing anode slurry
And (3) mixing and grinding the positive electrode material, the conductive agent and the positive electrode binder solution prepared in the step (2) for 5-10 min to obtain positive electrode slurry.
Wherein the anode material is 0.064g of lithium iron phosphate; the conductive agent is KB carbon 0.008 g; the mass ratio of the positive electrode material to the conductive agent to the positive electrode binder solution in terms of solid content is 8:1: 1.
And 4, step 4: preparing gel polymer precursor solution
Dissolving the modified gelatin prepared in the step 1 in water bath at 40 ℃ to prepare 10% aqueous solution, then adding polyethylene glycol diacrylate (PEGDA) and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution. The mass ratio of the gelatin to the polyethylene glycol diacrylate (PEGDA) is 1: 2; the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.2 wt%.
And 5: integrated pole piece for preparing positive electrode-gel polymer electrolyte
And (3) coating the positive electrode slurry on an aluminum foil in a scraping manner, carrying out ultraviolet curing for 90s, taking out, drying for 4h at 80 ℃ in a blast oven, weighing cut pieces after the surface of the electrode piece is basically dried, then coating the gel polymer precursor solution prepared in the step (4) on the electrode piece in a scraping manner, carrying out ultraviolet irradiation for 90s, drying for 4h in the blast oven at 80 ℃, and then transferring to a vacuum drying oven at 110 ℃ for storage for 30h to obtain the positive electrode piece.
And soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
Specifically, the soaking time is 12 hours, and the electrolyte is lithium hexafluorophosphate (L iPF)6) The solvent is ethyl carbonate/dimethyl carbonate ═ 1:1(v/v), and the electrolyte is lithium hexafluorophosphate (L iPF)6) Has a concentration of 1 mol/L.
Example 8
A lithium ion battery, in particular to a button battery, which is assembled by adopting the positive electrode-gel electrolyte integrated pole piece prepared in the embodiment 1.
The specific assembly method and sequence are as follows: and stacking the negative electrode battery shell, the elastic sheet, the steel sheet, the lithium sheet, the gel polymer electrolyte-positive electrode integrated pole piece and the positive electrode battery shell in sequence, and finally putting the positive electrode battery shell into a battery sealing machine for packaging to obtain the button battery.
Test results
Referring to fig. 2, a surface morphology and a profile morphology of the positive electrode-gel polymer electrolyte integrated pole piece prepared in example 1 of the present invention are shown, and a morphology comparison graph of the non-integrated pole piece is shown.
Wherein, the graph a and the graph b are respectively the surface appearance and the section appearance of the non-integrated pole piece, and the graph c and the graph d are respectively the surface appearance and the section appearance of the positive pole-gel polymer electrolyte integrated pole piece prepared in the embodiment 1.
The rest of the non-integrated pole piece is the same as that of the embodiment 1, except that the step 4 is not carried out: preparing a gel polymer precursor solution, and performing the blade coating of the gel polymer precursor solution of the step 5 and the related steps thereafter.
The figure shows that the surface of the anode-gel polymer electrolyte integrated pole piece is smoother and the roughness is reduced. Meanwhile, the interface bonding condition of the gel polymer electrolyte and the anode material is good as can be seen from the section morphology.
Referring to fig. 3, there are shown graphs for testing cycle performance of the lithium ion battery (a), and the non-integrated battery (b) according to example 8 of the present invention.
The non-integral cell was otherwise identical to that of example 8, except that separate pole pieces and separator membranes were used.
The lithium ion battery prepared by the method has more excellent and stable coulombic efficiency, the first coulombic efficiency (86.15%) of the lithium ion battery prepared by the method is far higher than that of a non-integrated battery (72.90%), and the coulombic efficiency in the 200-circle circulation process is stable.
The technical solution provided by the present invention is not limited by the above embodiments, and all technical solutions formed by utilizing the structure and the mode of the present invention through conversion and substitution are within the protection scope of the present invention.

Claims (9)

1. An integrated preparation method of a positive electrode-gel polymer electrolyte is characterized by comprising the following steps:
step 1, chemically modifying gelatin to obtain modified gelatin;
step 1.1, dissolving gelatin powder in phosphoric acid buffer solution;
step 1.2, slowly dripping methacrylic anhydride, and stirring for reaction;
dialyzing the solution after the reaction in the step 1.3, and freeze-drying to obtain a white foamy solid, namely modified gelatin;
step 2, preparing a positive electrode binder solution;
dissolving the modified gelatin prepared in the step 1 to prepare an aqueous solution, adding polyethylene glycol diacrylate and a photoinitiator, and uniformly mixing to obtain a positive electrode binder solution;
step 3, preparing anode slurry;
mixing and grinding a positive electrode material, a conductive agent and the positive electrode binder solution prepared in the step 2 to obtain positive electrode slurry;
and 4, step 4: preparing a gel polymer precursor solution;
dissolving the modified gelatin prepared in the step 1 to prepare an aqueous solution, adding polyethylene glycol diacrylate and a photoinitiator, and uniformly mixing to obtain a gel polymer precursor solution;
and 5: preparing an anode-gel polymer electrolyte integrated pole piece;
coating the positive electrode slurry obtained in the step (3) on a current collector in a blade mode, curing under an ultraviolet lamp, drying, and weighing cut pieces; then, blade-coating the gel polymer precursor solution prepared in the step (4) on the positive electrode plate, secondarily curing the gel polymer precursor solution under an ultraviolet lamp, and secondarily drying and drying the gel polymer precursor solution to obtain a positive electrode plate; and soaking the positive pole piece in the electrolyte to obtain the positive pole-gel polymer electrolyte integrated pole piece.
2. The integrated preparation method of the cathode-gel polymer electrolyte as claimed in claim 1, wherein:
in the step 1.1, the gelatin powder is 5-10g, and the phosphate buffer solution is 100m L PBS buffer solution with pH of 7;
the dissolving temperature of the step 1.1 is 50-60 ℃, and the dissolution is accelerated by stirring;
in the step 1.2, methacrylic anhydride is 4-8m L, the reaction temperature is 50-60 ℃, and the reaction time is 6-12 h;
in step 1.3, the dialysis time is 3-5 days, the freezing temperature is-20 ℃, and the freezing time is 24-48 h.
3. The integrated preparation method of the cathode-gel polymer electrolyte as claimed in claim 2, wherein:
in step 2, preparing the modified gelatin into a 3-8% solution in a water bath at 40 ℃;
the mass ratio of the modified gelatin to the polyethylene glycol diacrylate is 5: 1-1: 1;
the photoinitiator is I2959, and the proportion of the photoinitiator in the positive electrode binder solution is 0.05-0.5 wt%.
4. The integrated preparation method of the cathode-gel polymer electrolyte as claimed in claim 3, wherein: in the step 3, the positive electrode material is lithium iron phosphate, the conductive agent is KB carbon, the mass ratio of the positive electrode material to the conductive agent to the binder in terms of solid content is 8:1:1, and the mixing and grinding time is 5-10 min.
5. The integrated preparation method of the cathode-gel polymer electrolyte as claimed in claim 4, wherein:
in the step 4, 5-10% of modified gelatin is prepared into a solution in a water bath at 40 ℃, the mass ratio of the modified gelatin to the polyethylene glycol diacrylate is 1:1, the photoinitiator is I2959, and the proportion of the photoinitiator in the polymer precursor solution is 0.05-0.5 wt%.
6. The integrated preparation method of the cathode-gel polymer electrolyte as claimed in claim 5, wherein: in the step 5, the current collector is an aluminum foil, the curing time is 60-120s, and the drying condition is drying in a blast oven at 80 ℃ for 3-5 h; the secondary curing time is 60-120s, the secondary drying condition is drying in a forced air oven at 80 ℃ for 3-5h, and the drying condition is storing in a vacuum drying oven at 110 ℃ for 24-36 h.
7. The integrated preparation method of the cathode-gel polymer electrolyte as claimed in claim 6, wherein in the step 5, the soaking time is 12h, the electrolyte is lithium hexafluorophosphate, the solvent is one-to-one by volume of ethyl carbonate and dimethyl carbonate, and the concentration of the lithium hexafluorophosphate in the electrolyte is 1 mol/L.
8. An integrated pole piece of positive electrode-gel polymer electrolyte prepared by the method of any one of claims 1 to 7.
9. A lithium ion battery comprising the cathode-gel polymer electrolyte integrated pole piece of claim 8.
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