CN101210339B - Method for preparing battery electrode - Google Patents
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- CN101210339B CN101210339B CN200610167331XA CN200610167331A CN101210339B CN 101210339 B CN101210339 B CN 101210339B CN 200610167331X A CN200610167331X A CN 200610167331XA CN 200610167331 A CN200610167331 A CN 200610167331A CN 101210339 B CN101210339 B CN 101210339B
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
A battery electrode preparation method comprises the step of loading an electrode material on an electrode current collector, wherein the electrode material loading process comprises the following steps of disposing the electrode current collector in a suspension liquid containing an electrode material, connecting the electrode current collector with one electrode of a DC power supply, connecting the other electrode of the DC power supply with an inert electrode disposed in the suspension solution, switching on the DC power supply to electrophoretically deposit the electrode material on the electrode current collector. By electrophoretically depositing the electrode material on the electrode current collector, the battery electrode preparation method of the invention can improve the specific capacity and the cycle performance of the battery.
Description
Technical field
The invention relates to a kind of preparation method of battery electrode.
Background technology
Secondary cell like lithium ion battery, alkaline secondary cell, is widely used in 3C Product, also is in PC, mobile telephone and the individual radio electronics such as portable CD player, PDA.Secondary cell generally comprises shell, electrolytic solution, electrode and barrier film, and electrode comprises anode pole piece and cathode pole piece, and barrier film is between anode pole piece and cathode pole piece.Anode pole piece comprises plus plate current-collecting body and loads on the positive electrode material on the plus plate current-collecting body that cathode pole piece comprises negative current collector and loads on the negative material on the negative current collector.
In the making of conventional battery electrode, generally adopt the mode that applies.For example; The making method of anode pole piece generally comprises processes anode sizing agent with positive electrode material and solvent; Anode sizing agent is applied and/or is filled on the plus plate current-collecting body; Dry also compacting, the making method of cathode pole piece and the making method of anode pole piece are roughly the same, just use negative material to process cathode size earlier.Use in the process of above-mentioned cladding process manufacture batteries electrode; There is deviation in the homogeneity of dressing thickness; So just make thickness of electrode, uniformity of weight relatively poor; And in the process of preparation electrode, must use suitable sticker to accomplish the preparation of electrode, and so just having reduced the consumption of positive and negative electrode active substance, the specific storage of the battery that the electrode that is therefore made by the conventional battery method for making its electrode is formed is lower, cycle performance is relatively poor.
Summary of the invention
The objective of the invention is in order to overcome the shortcoming that specific storage is lower, cycle performance is relatively poor of the battery that the electrode that made by the conventional battery method for making its electrode forms; A kind of preparation method of battery electrode is provided, and the specific storage of the battery that electrode obtained by this method is formed is high, good cycle.
Contriver of the present invention finds; Electrode materials is dispersed in forms suspension-s in the dispersion medium; Electrode material granules in the suspension-s has electric charge; When the two poles of the earth of direct supply were contacted with suspension-s simultaneously, under the electrical forces effect, the electrode materials that has electric charge was moving to a Ghandler motion that has opposite charges of power supply.If the utmost point that has opposite charges of said power supply is linked to each other with electrode current collecting body and this electrode current collecting body is placed in the said suspension-s; Then can utilize principle of electrophoresis; Make the electrode materials that has electric charge move and be deposited on the collector, thereby make electrode to electrode current collecting body.
The invention provides a kind of preparation method of battery electrode, this method comprises electrode materials is loaded on the electrode current collecting body, wherein; Electrode materials the method on the electrode current collecting body of loading on comprised electrode current collecting body is placed in the suspension-s that contains electrode materials; Electrode current collecting body extremely links to each other with one of direct supply, and another utmost point of direct supply links to each other with noble electrode, and this noble electrode is placed in the said suspension-s; Connect direct supply, with the electrode materials electrophoretic deposition on electrode current collecting body.
The preparation method of battery electrode provided by the invention on electrode current collecting body, can realize following advantage with the electrode materials electrophoretic deposition:
1, has enough bonding forces between the electrode material granules of electrophoretic deposition, need not sticker, improved the dressing amount of electrode active material, thereby improve the specific storage of battery;
2, through electrophoretic deposition can with the electrode materials uniform and delicate load on the electrode current collecting body, the uniform in thickness of the electrode plates that makes, thus improve the cycle performance of battery;
3, method of the present invention need not compressing tablet, and step is simple, save time, can be through control voltage of supply and the electrophoresis time thickness of the electrode material layer of control load on collector easily.
Embodiment
The preparation method of battery electrode provided by the invention comprises electrode materials is loaded on the electrode current collecting body; Wherein, electrode materials the method on the electrode current collecting body of loading on comprised electrode current collecting body is placed in the suspension-s that contains electrode materials that electrode current collecting body extremely links to each other with one of direct supply; Another utmost point of direct supply links to each other with noble electrode; This noble electrode is placed in the said suspension-s, connects direct supply, with the electrode materials electrophoretic deposition on electrode current collecting body.
Can regulate the voltage and the electrophoresis time of direct supply according to the amount of the electrode materials of want load.The voltage of said direct supply can lie prostrate for 10-3000, is preferably the 20-2000 volt.The electrophoretic time can be 5-60 minute, is preferably 10-30 minute.Electrophoretic temperature can be 25-80 ℃, is preferably 40-70 ℃.
In electrophoresis process, preferably make the voltage of direct supply keep constant, can make the electrode materials that is deposited on electrode current collecting body homogeneous more like this.Can use conventional various potentiostats to make the voltage of direct supply keep constant.Said potentiostat can be commercially available, for example 6800 model potentiostats of Taiwan Ai De Ces Co.,Ltd production.
Said noble electrode can be used noble electrode for the electrophoresis of routine, is preferably plate graphite electrode or platinum electrode.
The pole piece thickness of the electrode of the present invention's preparation can be preferably the 40-300 micron for its conventional thickness.
Said suspension-s contains electrode materials and dispersion medium, can make through electrode materials is joined in the dispersion medium.Dispersion medium with 100 weight parts is a benchmark, and the add-on of electrode materials can be the 0.1-50 weight part, is preferably the 2-35 weight part, more preferably the 5-20 weight part.In the process that forms suspension-s, can use ultra-sonic oscillation or magnetic agitation to make electrode materials more even dispersedly.The method of said ultra-sonic oscillation and magnetic agitation has been conventionally known to one of skill in the art, repeats no more at this.
The average particle diameter of said electrode materials can be preferably the 5-50 micron, more preferably the 5-20 micron for its conventional average particle diameter.
Said dispersion medium can disperse dispersion medium wherein with electrode materials for any, and for example, said dispersion medium can be selected from one or more in water, alcohol, nitrile, furans, aldehyde, organic carboxylic ester and the ketone.Said alcohol can be the alcohol of 1-10 for carbonatoms, is preferably the alcohol that carbonatoms is 1-6.Said alcohol can be monohydroxy-alcohol or polyvalent alcohol.In the present invention, the example of said alcohol includes but not limited to methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, amylalcohol, neopentyl alcohol, hexanol, hexalin, terepthaloyl moietie and USP Kosher.Said furans is preferably THF.Said nitrile is preferably acetonitrile.Said aldehyde can be the aldehyde of 2-10 for carbonatoms, is preferably the aldehyde that carbonatoms is 2-6.Said organic carboxylic ester can be the organic carboxyl acid of 2-10 for carbonatoms, is preferably the organic carboxyl acid that carbonatoms is 2-6.Said ketone can be ketone or the N-Methyl pyrrolidone (NMP) of 3-10 for carbonatoms, is preferably ketone or NMP that carbonatoms is 3-6.Said dispersion medium is preferably one or more among water, Virahol, ethanol and the NMP.
After the electrophoresis, can also counter electrode washing and dry.The method of washing can be washed electrode for water, till washing fluid is neutrality.Said drying can be the drying means of routine, and is like seasoning, heat drying, forced air drying or vacuum-drying, preferably dry down, more preferably dry down at 80-180 ℃ at 50-200 ℃.
Battery electrode preparation method provided by the invention is applicable to the electrode of the various batteries of preparation; For example; The positive and negative electrode of lithium ion battery, the positive and negative electrode of alkaline secondary cell only need to form said suspension-s and use the corresponding electrode collector to get final product with the corresponding electrode material.
For example, during the preparation lithium ion cell positive, said electrode materials is the positive electrode material of lithium ion battery, and this positive electrode material comprises positive active material.The kind of said lithium ion anode active substance has been conventionally known to one of skill in the art, and for example, said positive active material can be in cobalt acid lithium, lithium manganate, iron lithium phosphate and the lithium nickelate one or more.Said positive electrode material can also comprise static eliminator, and the amount of static eliminator is the 0-15 weight % of positive active material, is preferably 1-10 weight %.The kind of static eliminator has been conventionally known to one of skill in the art, for example, can be in conductive carbon black, superconduction carbon black, electrically conductive graphite and the acetylene black one or more.
Said positive electrode material joined form suspension-s in the dispersion medium.The pH value of said suspension-s is preferably 0.3-6.5, more preferably 0.5-2.Method that can be through routine transfers to above-mentioned scope with the pH value of suspension-s, for example, in suspension-s, adds hydrochloric acid.
Said electrode current collecting body is the lithium ion cell positive collector, and said lithium ion cell positive collector has been conventionally known to one of skill in the art.Among the present invention, said lithium ion cell positive collector is preferably Copper Foil or aluminium foil, more preferably aluminium foil.The lithium ion cell positive collector is put into said suspension-s and linked to each other with the negative pole of direct supply, and the positive pole of direct supply links to each other with noble electrode.
The voltage of said direct supply is preferably the 10-400 volt, more preferably the 20-300 volt.The pole piece thickness of the lithium ion cell positive that makes is preferably the 70-300 micron, more preferably the 70-100 micron.
During the preparation lithium ion battery negative, said electrode materials is the negative material of lithium ion battery, and this negative material comprises negative electrode active material.The kind of said lithium ion negative electrode active material has been conventionally known to one of skill in the art; For example; Said negative electrode active material can be in natural graphite, synthetic graphite, refinery coke, organic cracking carbon, carbonaceous mesophase spherules, thomel, tin alloy, the silicon alloy one or more, preferred electrographite.Said negative material can also comprise static eliminator, and the amount of static eliminator is the 0-15 weight % of negative electrode active material, is preferably 1-10 weight %.The kind of static eliminator has been conventionally known to one of skill in the art, for example, can be in conductive carbon black, superconduction carbon black, electrically conductive graphite and the acetylene black one or more.
Said negative material joined form suspension-s in the dispersion medium.The pH value of said suspension-s is preferably 0.5-6.5, more preferably 3-4.Method that can be through routine transfers to above-mentioned scope with the pH value of suspension-s, for example, in suspension-s, adds hydrochloric acid.
Said electrode current collecting body is the lithium ion battery negative collector, and said lithium ion battery negative collector has been conventionally known to one of skill in the art.Among the present invention, said lithium ion battery negative collector is preferably Copper Foil or aluminium foil, more preferably Copper Foil.The lithium ion battery negative collector is put into said suspension-s and linked to each other with the positive pole of direct supply, and the negative pole of direct supply links to each other with noble electrode.
The voltage of said direct supply is preferably the 400-3000 volt, more preferably the 500-2000 volt.The pole piece thickness of the lithium ion cell positive that makes is preferably the 40-70 micron.
Come to describe in more detail the present invention through embodiment below.
Embodiment 1
This embodiment is used to explain the preparation method of battery electrode provided by the invention.
With 15 weight part LiCoO
2Powder (average particle diameter is 8 microns) joins in the 100 weight part Virahols, with 2000 rev/mins of stirrings 30 minutes, forms suspension-s, and dripping hydrochloric acid transfers to 1 with the pH value of suspension-s.
Suspension-s is transferred in the electrolyzer, and bath temperature is controlled at 50 ℃, and Graphite Electrodes and aluminium foil (length is 89.0 millimeters, and width is 38.5 millimeters, and thickness is 0.016 millimeter) are put into the electrolyzer that suspension-s is housed respectively.Graphite Electrodes is linked to each other with the positive pole of direct supply, and aluminium foil links to each other with the negative pole of direct supply, makes power source voltage be stabilized in 200 volts, and energized begins electrophoresis.Behind the electrophoresis 10 minutes, taking out load has LiCoO
2Aluminium foil, be washed with water to washings and be neutral, 80 ℃ of oven dry down, obtain anodal A1 then, the pole piece thickness of anodal A1 is 0.090 millimeter.Anodal A1 contains 1.220 gram LiCoO
2
Embodiment 2
This embodiment is used to explain the preparation method of battery electrode provided by the invention.
With 5 weight part LiCoO
2Powder (average particle diameter is 10 microns) joins in the 100 weight part acetonitriles, with 2000 rev/mins of stirrings 30 minutes, forms suspension-s, and dripping hydrochloric acid transfers to 0.5 with the pH value of suspension-s.
Suspension-s is transferred in the electrolyzer, and bath temperature is controlled at 40 ℃, and platinum electrode and aluminium foil (length is 89.0 millimeters, and width is 38.5 millimeters, and thickness is 0.016 millimeter) are put into the electrolyzer that suspension-s is housed respectively.With just linking to each other of platinum electrode and direct supply, aluminium foil links to each other with the negative pole of direct supply, makes power source voltage be stabilized in 50 volts, and energized begins electrophoresis.Behind the electrophoresis 30 minutes, taking out load has LiCoO
2Aluminium foil, be washed with water to washings and be neutral, 80 ℃ of oven dry down, obtain anodal A2 then, the pole piece thickness of anodal A2 is 0.085 millimeter.Anodal A2 contains 1.125 gram LiCoO
2
Embodiment 3
This embodiment is used to explain the preparation method of battery electrode provided by the invention.
10 weight part powdered graphites (average particle diameter is 25 microns) are joined among the 100 weight part NMP, with 2000 rev/mins of stirrings 30 minutes, form suspension-s, dripping hydrochloric acid transfers to 3 with the pH value of suspension-s.
Suspension-s is transferred in the electrolyzer, and bath temperature is controlled at 80 ℃, and Graphite Electrodes and Copper Foil (length is 91.0 millimeters, and width is 40.5 millimeters, and thickness is 0.010 millimeter) are put into the electrolyzer that suspension-s is housed respectively.Graphite Electrodes is linked to each other with the negative pole of direct supply, and Copper Foil links to each other with the positive pole of direct supply, makes power source voltage be stabilized in 500 volts, and energized begins electrophoresis.Behind the electrophoresis 10 minutes, take out the Copper Foil that load has graphite, be washed with water to washings and be neutral, 80 ℃ of oven dry down, obtain negative pole B1 then, the pole piece thickness of negative pole B1 is 0.105 millimeter.Negative pole B1 contains 0.630 gram graphite.
Embodiment 4
This embodiment is used to explain the preparation method of battery electrode provided by the invention.
4 weight part graphite (average particle diameter is 25 microns) are joined in the mixture of 50 parts by weight of ethanol and 50 weight parts waters, with 2000 rev/mins of stirrings 30 minutes, form suspension-s, dripping hydrochloric acid transfers to 4 with the pH value of suspension-s.
Suspension-s is transferred in the electrolyzer, and bath temperature is controlled at 70 ℃, and platinum electrode and Copper Foil (length is 91.0 millimeters, and width is 40.5 millimeters, and thickness is 0.010 millimeter) are put into the electrolyzer that suspension-s is housed respectively.Platinum electrode is linked to each other with the negative pole of direct supply, and Copper Foil links to each other with the positive pole of direct supply, makes power source voltage be stabilized in 1000 volts, and energized begins electrophoresis.Behind the electrophoresis 15 minutes, take out the Copper Foil that load has graphite, be washed with water to washings and be neutral, 80 ℃ of oven dry down, obtain negative pole B2 then, the pole piece thickness of negative pole B2 is 0.095 millimeter.Negative pole B2 contains 0.565 gram graphite.
Comparative Examples 1
This Comparative Examples is used to explain the preparation method of conventional battery electrode.
With positive electrode material (100 weight part positive active material LiCoO
2, 4 weight part caking agent PVDF, 4 weight part static eliminator acetylene blacks) and 40 parts by weight solvent NMP mix; Make anode sizing agent; This anode sizing agent is uniformly coated on aluminium foil (length is 89.0 millimeters, and width is 38.5 millimeters, and thickness is 0.016 millimeter) surface; Dry, compressing tablet obtain anode pole piece CA1.Wherein this anode pole piece contains 1.342 gram positive active material LiCoO
2
Comparative Examples 2
This Comparative Examples is used to explain the preparation method of conventional battery electrode.
With negative material (100 weight part graphite; 5 weight part tackiness agent tetrafluoroethylene) and 40 parts by weight solvent NMP mix, make cathode size, this cathode size is uniformly coated on Copper Foil, and (length is 91.0 millimeters; Width is 40.5 millimeters; Thickness is 0.010 millimeter) surface, dry, compressing tablet obtain cathode pole piece CB1.Wherein this cathode pole piece contains 0.670 gram graphite.
Embodiment 5-8
Embodiment 5-8 is respectively applied for the performance of the lithium ion battery of the negative pole assembling that positive pole that explanation makes by embodiment 1 and 2 and embodiment 3 and 4 make.
According to following method, the negative pole that positive pole that use embodiment 1 and 2 makes and embodiment 3 and 4 make is assembled into lithium ion battery D1 to D4 respectively:
Anodal, negative pole and polypropylene screen are wound into the pole piece of a square lithium ion battery, then nonaqueous electrolytic solution are injected battery case with the amount of 3.8g/Ah, seal, process lithium ion battery.This electrolytic solution contains 1 mol LiPF6, and solvent is that weight ratio is 30: 34: 11: the mixture of 12 NSC 11801, Methyl ethyl carbonate, diethyl carbonate and methylcarbonate.
Go up specific storage and the cycle performance of measuring the above-mentioned battery D1 to D4 that obtains according to following method at BK-6016AR cabinet (Guangzhou Lanqi Electronic Industrial Co., Ltd.).
Specific storage: the ratio of quality that is discharged to loading capacity and positive active material or the negative electrode active material of 3.0V with the electric current of 0.1C from 4.2V first;
Cycle performance: under 25 ℃; With 10 milliamperes continuous currents battery charge to 2.5 is lied prostrate; With 10 milliamperes continuous current battery discharge to 0.005 is lied prostrate then; Record cycle charge-discharge n time is the capacity of battery afterwards, representes the cycle performance of battery with the percent value of this capacity and battery initial capacity as the capacity surplus ratio, and the cycle performance of the high more explanation battery of capacity surplus ratio is made an appointment.
Mensuration result is as shown in table 1.
Comparative Examples 3
This Comparative Examples is used to explain the performance of the lithium ion battery of the negative pole assembling that the positive pole that made by Comparative Examples 1 and Comparative Examples 2 make.
According to the method identical, the positive pole of Comparative Examples 1 and the negative pole of Comparative Examples 2 are assembled into lithium ion battery CD1 with embodiment 5-8.
Measure specific storage and the cycle performance of lithium ion battery CD1 according to the method identical with embodiment 5-8.The result is as shown in table 1.
Table 1
Can find out from the mensuration result shown in the table 1; The specific storage of the battery D1-4 of embodiment 5-8 is apparently higher than the battery CD1 of Comparative Examples 3; Capacity surplus ratio after the battery D1-4 circulation 50 times and 300 times is also apparently higher than battery CD1, explains that specific storage that electrode that battery electrode preparation method provided by the invention obtains can significantly improve battery also significantly improves the cycle performance of battery.
Claims (6)
1. the preparation method of a battery electrode, this method comprise electrode materials are loaded on the electrode current collecting body, it is characterized in that; Electrode materials the method on the electrode current collecting body of loading on comprised electrode current collecting body is placed in the suspension-s that contains electrode materials that electrode current collecting body extremely links to each other with one of direct supply, another utmost point of direct supply links to each other with noble electrode; This noble electrode is placed in the said suspension-s, connects direct supply, with the electrode materials electrophoretic deposition on electrode current collecting body; The electrophoretic time is 10-30 minute; The voltage of said direct supply is the 10-3000 volt, and electrophoretic temperature is 25-80 ℃, and said suspension-s is made up of electrode materials and dispersion medium; Said dispersion medium is selected from one or more in water, alcohol, nitrile, furans, aldehyde, organic carboxylic ester and the ketone; Dispersion medium with 100 weight parts is a benchmark, and the content of electrode materials is the 0.1-50 weight part
This method also comprise following the two one of:
(1) said electrode materials is the positive electrode material of lithium ion battery; The static eliminator that the positive electrode material of said lithium ion battery is contained by lithium ion anode active substance and selectivity and forming; Said electrode current collecting body is the lithium ion cell positive collector, and the lithium ion cell positive collector links to each other with the negative pole of said direct supply, and the positive pole of direct supply links to each other with said noble electrode; Said lithium ion cell positive collector is Copper Foil or aluminium foil, and the pH value of said suspension-s is 0.3-6.5;
(2) said electrode materials is the negative material of lithium ion battery; The static eliminator that the negative material of said lithium ion battery is contained by lithium ion negative electrode active material and selectivity and forming; Said electrode current collecting body is the lithium ion battery negative collector; The lithium ion battery negative collector links to each other with the positive pole of said direct supply, and the negative pole of direct supply links to each other with said noble electrode, and the pH value of said suspension-s is 0.5-6.5.
2. method according to claim 1, wherein, the voltage of said direct supply is the 20-2000 volt, electrophoretic temperature is 40-70 ℃.
3. method according to claim 1, wherein, the average particle diameter of said electrode materials is the 5-50 micron.
4. method according to claim 1, wherein, said dispersion medium is one or more in water, Virahol, ethanol and the N-Methyl pyrrolidone.
5. method according to claim 1, wherein, the voltage of said direct supply is the 10-400 volt, and the pH value of said suspension-s is 0.5-2, and said lithium ion cell positive collector is an aluminium foil.
6. method according to claim 1, wherein, the voltage of said direct supply is the 400-3000 volt, and the pH value of said suspension-s is 3-4, and said lithium ion battery negative collector is a Copper Foil.
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| CN102956872B (en) * | 2011-08-29 | 2015-06-03 | 海洋王照明科技股份有限公司 | Preparation method and application of compound electrode slice |
| CN103035878B (en) * | 2011-10-09 | 2015-11-25 | 海洋王照明科技股份有限公司 | Graphene/tin-oxide compound electric pole piece and preparation method thereof |
| CN105161694A (en) * | 2015-06-12 | 2015-12-16 | 南通彩都新能源科技有限公司 | Preparation method for silicon-carbon-graphene composite negative electrode for lithium ion battery |
| CN108598451B (en) * | 2017-12-12 | 2020-11-06 | 湖北工业大学 | Sodium ion battery red phosphorus negative pole piece and preparation method thereof |
| CN112981499B (en) * | 2021-02-05 | 2022-03-18 | 太原科技大学 | Method and apparatus for electrodepositing active material particles on electrode current collector |
| CN114843451A (en) * | 2022-05-16 | 2022-08-02 | 中山大学 | Preparation method of nontoxic and economical positive pole piece of sodium-ion battery |
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| CN1763261A (en) * | 2005-09-27 | 2006-04-26 | 清华大学 | Titanium dioxide nano material film and preparation method thereof |
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