CN110970231A - Semi-solid lithium ion capacitor and manufacturing method thereof - Google Patents
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- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a semi-solid lithium ion capacitor and a manufacturing method thereof, wherein a semi-solid positive electrode of the capacitor comprises porous carbon and/or lithium transition metal acid salt, a conductive agent and electrolyte, a semi-solid negative electrode comprises a negative electrode active substance, a conductive agent, electrolyte and pre-doped lithium, a non-porous current collector is adopted as the current collector, the semi-solid positive electrode and the semi-solid negative electrode are oppositely arranged, the middle part of the semi-solid positive electrode and the semi-solid negative electrode is separated by an ion permeable membrane, a lithium source electrode is oppositely arranged on one side of the semi-solid negative electrode, which is not close to the ion permeable membrane, and is separated by a. The invention has simple process, large electrode thickness, no binder, high active material ratio of the whole lithium ion capacitor, more stable, more efficient and uniform lithium ion pre-doping of the cathode, and obviously improved energy density of the lithium ion capacitor.
Description
Technical Field
The invention relates to a lithium ion capacitor, in particular to a semi-solid lithium ion capacitor and a manufacturing method thereof.
Background
Lithium ion batteries have received extensive research attention due to their high energy density, but the problems of low power density and poor cycle life limit their application in high power applications. In contrast, supercapacitors have high power density, long cycle life, but low energy density. The lithium ion capacitor is an energy storage device between the lithium ion battery and the double electric layer capacitor, and combines the advantages of high power density, long cycle life and high energy density of the lithium ion battery of the super capacitor.
Lithium ion capacitors generally use lithium battery electrode materials capable of releasing lithium as a negative electrode, mainly include lithium ion pre-doped carbon materials such as graphite, hard carbon, soft carbon, mesocarbon microbeads, lithium metal oxides and the like, and a positive electrode generally uses porous carbon materials with high specific surface area. However, the lithium ion capacitor introduces a certain proportion of capacitance carbon, so that the charge and discharge capacity and energy density of the device are reduced.
Patent CN106654177A discloses a method for preparing a composite electrode of a battery capacitor by a dry method, which comprises mixing an active material, a binder and a conductive agent, calcining, extruding to obtain a dry electrode film, adhering to a current collector, and rolling to obtain the dry composite electrode. Although the method improves the compaction density and the energy density to a certain extent, the problems of uneven compaction and overlarge local compaction still exist in the dry electrode rolling process, so that the rate capability is poor.
The potential of the negative electrode is greatly reduced by pre-doping the lithium ions in the negative electrode material, so that the energy density is improved. Patent CN105097293A discloses a method for pre-embedding lithium in a negative electrode of a lithium ion capacitor, in which after positive and negative electrode plates are stacked into an electrical core, a metal lithium electrode and the negative electrode are oppositely placed and separated by a diaphragm, and a constant voltage is applied between the metal lithium electrode and the negative electrode to pre-embed lithium in the negative electrode.
Disclosure of Invention
One of the main objects of the present invention is to improve the uniformity of the pre-doping.
The invention also aims to improve the energy density of the lithium ion capacitor.
In order to achieve the above object, the present invention provides a semi-solid lithium ion capacitor and a method for manufacturing the same, wherein the method for manufacturing the semi-solid lithium ion capacitor comprises the following steps:
step one, manufacturing a semi-solid positive plate and a semi-solid negative plate, comprising,
a. coating semi-solid positive electrode slurry on a positive electrode current collector to form a semi-solid positive electrode plate with the thickness of 100-1000 mu m, wherein the semi-solid positive electrode slurry contains 30-90% of positive electrode active substances, 0.5-20% of conductive agents, 10-50% of electrolyte and
b. coating semi-solid negative electrode slurry on a negative electrode current collector to form a semi-solid negative electrode sheet with the thickness of 100-1000 mu m, wherein the semi-solid negative electrode slurry contains 30-90% of negative electrode active substances, 0.5-20% of conductive agents and 10-50% of electrolyte,
step two, one side of the semi-solid positive pole slurry of the semi-solid positive pole piece is opposite to one side of the semi-solid negative pole slurry of the semi-solid negative pole piece and is separated by an ion permeable membrane, one side of the semi-solid negative pole piece, which is not close to the ion permeable membrane, is provided with a lithium source electrode, the electrodes of the semi-solid negative pole piece and the lithium source electrode are separated by a diaphragm, the semi-solid positive pole piece, the ion permeable membrane, the semi-solid negative pole piece, the diaphragm and the lithium source electrode,
step three, the lithium source carries out lithium ion pre-doping on the semi-solid negative electrode in a constant current mode,
step four, formation is carried out,
step five, removing the lithium source electrode,
and step five, sealing the shell.
The preparation method also has the following optimized preparation steps.
The positive active material comprises porous carbon and/or lithium transition metal acid salt,
the negative active material is one or more of graphite, hard carbon, soft carbon, mesocarbon microbeads or graphene.
The lithium transition metal acid salt comprises LiFePO4、LiCO2、LiMn2O4、LiNiO2、LiNi0.5Mn1.5O4、LiNi0.8Co0.2O2、LiNi1/3Co1/3Mn1/3O2、LiNi0.5Co0.2Mn0.3O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.8Co0.1Mn0.1O2、LiNi0.8Co0.1Al0.1O2One or more of them.
And a non-porous current collector is adopted as the positive electrode current collector and/or the negative electrode current collector. The non-porous current collector is preferably a non-porous aluminum foil, a non-porous stainless steel foil, or a non-porous titanium foil.
The pre-doping is further characterized in that constant current with the size of 0.05C or less of the theoretical capacity of the semi-solid negative plate is applied between the semi-solid negative electrode and the lithium source, and the electric quantity is 15-50% of the theoretical capacity of the semi-solid negative plate.
The electrolyte includes a lithium saltSolutes, organic solvents and additives. The lithium salt is preferably LiPF6、LiClO4、LiBF4、LiBOB、LiAsF6、LiCF3SO3Or LiN (CF)3SO2) The organic solvent is preferably one or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methylethyl carbonate, methylpropyl carbonate, butylene carbonate, gamma-butyrolactone, ethyl acetate or acetonitrile, and the additive is preferably one or more of vinylene carbonate, ethylene sulfite, ethylene sulfate, methylene methyl disulfonate, fluoroethylene carbonate, 1, 3-propane sultone, propylene sultone, biphenyl, cyclohexylbenzene, coke tar, naphthalene, cyclohexane, cyclohexene, benzene, toluene, phenyladamantane, adamantane, 1,3, 5-tricyanobenzene, thianthrene or anthracene.
The preparation method of the semi-solid positive electrode slurry preferably comprises the following steps: mixing the positive active material and the conductive agent, mixing the mixture into the semi-solid positive slurry by using the electrolyte in a dry atmosphere,
the preparation method of the semi-solid negative electrode slurry preferably comprises the following steps: mixing the negative active material and the conductive agent, and mixing the mixture into the semi-solid negative slurry by using the electrolyte in a dry atmosphere.
According to the invention, the energy density of the lithium ion capacitor is improved by improving the thickness of the electrode, reducing the using amount of a current collector, not containing a binder, pre-doping lithium ions and the like, the lithium source electrode and the semi-solid negative plate are oppositely arranged and separated by the diaphragm, and the pre-doping lithium ions is carried out on the semi-solid negative electrode in a constant current mode.
The whole capacitor is simple in manufacturing process, the thickness of the electrode is improved, the using amount of the positive and negative current collectors is reduced, no binder is contained, the proportion of active substances of the whole lithium ion capacitor is improved, and the energy density of the lithium ion capacitor is obviously improved by combining a lithium ion pre-doping technology.
The pre-doped negative plate is in a semi-solid state form, so that the tortuosity of an electrode is reduced, and the electronic conductivity is improved, so that the uniformity of the lithium ion pre-doping of the negative electrode is effectively improved, meanwhile, the consistency of a lithium ion capacitor can be improved, and the assembly of a module and a system at the later stage is facilitated. The anode and the cathode are both made of non-porous current collectors, so that the preparation method is easy to obtain, low in cost, and low in process difficulty, and the semi-solid lithium ion capacitor is simple in manufacturing process and beneficial to industrial production of the lithium ion capacitor.
Drawings
Fig. 1 is a schematic structural diagram of a lithium ion capacitor in the embodiment when performing lithium ion pre-doping.
FIG. 2 is a graph showing the change with time of the lithium intercalation voltage in example 1.
Wherein: 100-a semi-solid lithium ion capacitor, 10-a positive electrode current collector, 20-semi-solid positive electrode slurry, 30-an ion permeable membrane, 40-semi-solid negative electrode slurry, 50-a negative electrode current collector, 60-a diaphragm, 70-a lithium source electrode and 80-a shell.
Detailed Description
The invention will be further described with reference to the following examples and figures, which are given for illustration only and are not intended to limit the scope of the invention.
Example 1
Manufacturing a semi-solid positive plate: mixing activated carbon and a Super P conductive agent according to a mass ratio of 55: 3, then adding an electrolyte into the dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 42: and 55, preparing slurry, and coating the slurry on an aluminum foil to prepare a semi-solid positive plate with the thickness of 500 mu m.
Manufacturing a semi-solid negative plate: mixing hard carbon and a Super P conductive agent according to a mass ratio of 55: 3, then adding an electrolyte into the dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 42: and 55, preparing slurry, and coating the slurry on copper foil to prepare the semi-solid negative plate with the thickness of 400 mu m.
Wherein the electrolyte is LiPF of 1 mol per liter6The solvent is prepared from the following components in a volume ratio of 1: 1 ethylene carbonate and dimethyl carbonate, and the additive is vinylene carbonate with the volume fraction of 2%.
The semi-solid positive plate and the semi-solid negative plate are oppositely arranged, the middle of the semi-solid positive plate and the middle of the semi-solid negative plate are separated by an ion permeable membrane, a lithium plate is oppositely arranged on one side of the semi-solid negative plate, which is not close to the ion permeable membrane, the semi-solid negative plate and the middle of the lithium plate are separated by a cellulose diaphragm and are placed in a shell, constant current is applied between the semi-solid negative plate and the lithium plate to pre-dope lithium ions on the negative electrode, the current is 0.02C of the theoretical capacity of hard carbon, the electric quantity is 30% of the theoretical capacity of the hard carbon, then formation is carried out, the. As can be seen from fig. 2, the potential of the negative electrode gradually decreases after lithium ion doping. The energy density of the lithium ion capacitor is 30Wh/kg by testing in a voltage interval of 2.2-3.8V.
Example 2
Manufacturing a semi-solid positive plate: mixing activated carbon and a Super P conductive agent according to a mass ratio of 57: 3, mixing, and then adding an electrolyte into a dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 40: 57, preparing the mixture into slurry, and then coating the slurry on an aluminum foil to prepare a semi-solid positive plate with the thickness of 400 mu m.
Manufacturing a semi-solid negative plate: mixing hard carbon and a Super P conductive agent according to a mass ratio of 60: 3, then adding an electrolyte into the dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 37: 60, preparing slurry, and then coating the slurry on copper foil to prepare the semi-solid negative plate with the thickness of 320 mu m.
Wherein the electrolyte is LiPF of 1 mol per liter6The solvent is prepared from the following components in a volume ratio of 1: 3: 1 ethylene carbonate, dimethyl carbonate and propylene carbonate, and the additive is vinylene carbonate with the volume fraction of 2%.
The semi-solid positive plate and the semi-solid negative plate are oppositely arranged, the middle of the semi-solid positive plate and the middle of the semi-solid negative plate are separated by an ion permeable membrane, a lithium plate is oppositely arranged on one side of the semi-solid negative plate, which is not close to the ion permeable membrane, the semi-solid negative plate and the middle of the lithium plate are separated by a polyester diaphragm and are placed in a shell, constant current is applied between the semi-solid negative plate and the lithium plate to pre-dope lithium ions on the negative electrode, the current is 0.05C of the theoretical capacity of hard carbon, the electric quantity is 20% of the theoretical capacity of the hard carbon, then formation is carried out. The energy density of the lithium ion capacitor is 24Wh/kg by testing in a voltage interval of 2.2-3.8V.
Example 3
Manufacturing a semi-solid positive plate: mixing activated carbon and a Super P conductive agent according to a mass ratio of 45: 2, then adding electrolyte into the dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 53: 45, preparing slurry, and then coating the slurry on an aluminum foil to prepare a semisolid positive plate with the thickness of 750 mu m.
Manufacturing a semi-solid negative plate: mixing graphite and a Super P conductive agent according to a mass ratio of 48: 2, then adding electrolyte into the dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 50: and 48, preparing slurry, and coating the slurry on copper foil to prepare the semi-solid negative plate with the thickness of 500 mu m.
Wherein the electrolyte is LiPF of 1 mol per liter6The solvent is prepared from the following components in a volume ratio of 1: 1 ethylene carbonate and dimethyl carbonate, and the additive is vinylene carbonate with the volume fraction of 2 percent and ethylene sulfite with the volume fraction of 1 percent.
The semi-solid positive plate and the semi-solid negative plate are oppositely arranged, the middle of the semi-solid positive plate and the middle of the semi-solid negative plate are separated by an ion permeable membrane, a lithium plate is oppositely arranged on one side of the semi-solid negative plate, which is not close to the ion permeable membrane, the semi-solid negative plate and the middle of the lithium plate are separated by a polyethylene/ceramic composite membrane and are placed into a shell, constant current is applied between the semi-solid negative plate and the lithium plate to pre-dope lithium ions on the negative electrode, the current is 0.03C of the theoretical capacity of hard carbon, the electric quantity is 15% of the theoretical capacity of the hard carbon, then formation is carried out. The energy density of the lithium ion capacitor is 29Wh/kg when the voltage interval is tested at 2.2-3.8V.
Example 4
Manufacturing a semi-solid positive plate: mixing activated carbon and a Super P conductive agent according to a mass ratio of 70: 2, then adding an electrolyte into the dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 28: 70, preparing slurry, and then coating the slurry on an aluminum foil to prepare a semi-solid positive plate with the thickness of 570 mu m.
Manufacturing a semi-solid negative plate: mixing hard carbon and a Super P conductive agent according to a mass ratio of 68: 2, then adding electrolyte into the dry atmosphere, wherein the mass ratio of the electrolyte to the activated carbon is 30: and 68, preparing slurry, and coating the slurry on copper foil to prepare the semi-solid negative plate with the thickness of 450 mu m.
Wherein the electrolyte is LiPF of 1 mol per liter6The solvent is prepared from the following components in a volume ratio of 1: 1: 1 ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate, and the additive is vinylene carbonate with the volume fraction of 2%.
The semi-solid positive plate and the semi-solid negative plate are oppositely arranged, the middle of the semi-solid positive plate and the middle of the semi-solid negative plate are separated by an ion permeable membrane, a lithium plate is oppositely arranged on one side of the semi-solid negative plate, which is not close to the ion permeable membrane, the semi-solid negative plate and the middle of the lithium plate are separated by a polyester/ceramic composite membrane and are placed into a shell, constant current is applied between the semi-solid negative plate and the lithium plate to pre-dope the lithium ions of the negative electrode, the current is 0.04C of the theoretical capacity of hard carbon, the electric quantity is 25% of the theoretical capacity of the hard carbon, then formation is carried. The energy density of the lithium ion capacitor is 31Wh/kg when the voltage interval is tested at 2.2-3.8V.
The electrochemical properties of the lithium ion capacitor prepared according to the present invention were measured as shown in table 1.
TABLE 1
The embodiments described in the specification are only preferred embodiments of the present invention, and the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit the present invention. Those skilled in the art can obtain technical solutions through logical analysis, reasoning or limited experiments according to the concepts of the present invention, and all such technical solutions are within the scope of the present invention.
Claims (10)
1. A manufacturing method of a semi-solid lithium ion capacitor is characterized by comprising the following steps:
step one, manufacturing a semi-solid positive plate and a semi-solid negative plate, comprising,
a. coating semi-solid positive electrode slurry on a positive electrode current collector to form a semi-solid positive electrode plate with the thickness of 100-1000 mu m, wherein the semi-solid positive electrode slurry contains 30-90% of positive electrode active substances, 0.5-20% of conductive agents, 10-50% of electrolyte and
b. coating semi-solid negative electrode slurry on a negative electrode current collector to form a semi-solid negative electrode sheet with the thickness of 100-1000 mu m, wherein the semi-solid negative electrode slurry contains 30-90% of negative electrode active substances, 0.5-20% of conductive agents and 10-50% of electrolyte,
step two, one side of the semi-solid positive pole slurry of the semi-solid positive pole piece is opposite to one side of the semi-solid negative pole slurry of the semi-solid negative pole piece and is separated by an ion permeable membrane, one side of the semi-solid negative pole piece, which is not close to the ion permeable membrane, is provided with a lithium source electrode, the electrodes of the semi-solid negative pole piece and the lithium source electrode are separated by a diaphragm, the semi-solid positive pole piece, the ion permeable membrane, the semi-solid negative pole piece, the diaphragm and the lithium source electrode,
step three, the lithium source carries out lithium ion pre-doping on the semi-solid negative electrode in a constant current mode,
step four, formation is carried out,
step five, removing the lithium source electrode,
and step five, sealing the shell.
2. The method for manufacturing a semi-solid lithium ion capacitor according to claim 1, wherein:
the positive active material includes porous carbon and/or lithium transition metal acid salt,
the negative active material is one or more of graphite, hard carbon, soft carbon, mesocarbon microbeads or graphene.
3. The method for manufacturing a semi-solid lithium ion capacitor according to claim 2, wherein:
the lithium transition metal acid salt comprises LiFePO4、LiCO2、LiMn2O4、LiNiO2、LiNi0.5Mn1.5O4、LiNi0.8Co0.2O2、LiNi1/3Co1/3Mn1/3O2、LiNi0.5Co0.2Mn0.3O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.8Co0.1Mn0.1O2、LiNi0.8Co0.1Al0.1O2One or more of them.
4. The method for manufacturing a semi-solid lithium ion capacitor according to claim 1, wherein the positive electrode current collector and/or the negative electrode current collector is a non-porous current collector.
5. The method of manufacturing a semi-solid lithium ion capacitor according to claim 4, wherein the non-porous current collector is a non-porous aluminum foil, a non-porous stainless steel foil or a non-porous titanium foil.
6. The method for manufacturing a semi-solid lithium ion capacitor according to claim 1, wherein the pre-doping is performed by applying a constant current between the semi-solid negative electrode and the lithium source, the constant current having a magnitude of 0.05C or less of the theoretical capacity of the semi-solid negative electrode sheet, and the electric quantity is 15-50% of the theoretical capacity of the semi-solid negative electrode sheet.
7. The method of manufacturing a semi-solid lithium ion capacitor according to claim 1, wherein the electrolyte comprises a solute including a lithium salt, an organic solvent, and an additive.
8. The method for manufacturing a semi-solid lithium ion capacitor according to claim 7, wherein:
the lithium salt is LiPF6、LiClO4、LiBF4、LiBOB、LiAsF6、LiCF3SO3Or LiN (CF)3SO2) One or more of the components (A) and (B),
the organic solvent is one or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, butylene carbonate, gamma-butyrolactone, ethyl acetate or acetonitrile,
the additive is one or more of vinylene carbonate, vinyl sulfite, vinyl sulfate, methyl disulfonate, fluoroethylene carbonate, 1, 3-propane sultone, propylene sultone, biphenyl, cyclohexylbenzene, coke acid ester, naphthalene, cyclohexane, cyclohexene, benzene, toluene, phenyl adamantane, 1,3, 5-tricyanobenzene, thianthrene or anthracene.
9. The method for manufacturing a semi-solid lithium ion capacitor according to claim 1, wherein:
mixing the positive active material and the conductive agent, mixing the mixture into the semi-solid positive slurry by using the electrolyte in a dry atmosphere,
mixing the negative active material and the conductive agent, and mixing the mixture into the semi-solid negative slurry by using the electrolyte in a dry atmosphere.
10. A semi-solid lithium ion capacitor manufactured by the manufacturing method of any one of claims 1 to 9.
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