CN100438146C - Lithium ion cell, anode therefor and preparing method thereof - Google Patents
Lithium ion cell, anode therefor and preparing method thereof Download PDFInfo
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- CN100438146C CN100438146C CNB2005101125950A CN200510112595A CN100438146C CN 100438146 C CN100438146 C CN 100438146C CN B2005101125950 A CNB2005101125950 A CN B2005101125950A CN 200510112595 A CN200510112595 A CN 200510112595A CN 100438146 C CN100438146 C CN 100438146C
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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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- 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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Abstract
The invention is an Li ion battery anode, comprising collector and coated and/or filled anode material on the collector, where the anode material comprises anode active matter, conducting agent and adhesive, the adhesive contains charcoal black which has a specific surface area above 500m2/g obtained by nitrogen absorption, where the anode material also comprises dispersant. And a Li ion battery using the anode has good circulating performance and multiplying discharging performance.
Description
Technical field
The invention relates to the anodal of a kind of battery and battery and their preparation method, more specifically say so about the anodal of a kind of lithium ion battery and lithium ion battery and their preparation method.
Background technology
Lithium ion battery mainly comprises pole piece and nonaqueous electrolytic solution, described pole piece and nonaqueous electrolytic solution are sealed in the battery container, described pole piece comprises battery electrode and barrier film, described battery electrode comprises positive pole and negative pole, described battery electrode comprises collector body and coating and/or is filled in electrode material on the collector body that described positive electrode comprises positive active material, conductive agent and adhesive; Negative material comprises negative electrode active material and adhesive, can also comprise conductive agent.The preparation method of battery electrode comprises that the slurry that will contain electrode active material, adhesive, contain or not contain conductive agent and solvent applies and/or is filled on the collector body, and drying is rolled or do not rolled.
Lithium ion battery is as a kind of chemical power source, refers to respectively the secondary cell that constitutes as both positive and negative polarity with two compounds that can reversibly embed with the removal lithium embedded ion.When battery charge, lithium ion takes off embedding from positive pole, in negative pole, embed, otherwise during discharge.Lithium rechargeable battery exists the migration repeatedly of lithium ion in charge and discharge process repeatedly, and electrolyte is present in the lithium rechargeable battery as the transmission medium that lithium ion moves, and comprises in the space that is present in anodal and negative electrode active material.
Usually, negative active core-shell material is graphite or other material with carbon element, and this class material with carbon element generally all has conductivity preferably, and therefore, negative material can comprise conductive agent also can not comprise conductive agent.And be layer structure as the composite oxides of the lithium of positive active material, itself do not possess conductivity, therefore need in positive active material, add conductive agent, as: conductive black, acetylene black, electrically conductive graphite wait and improve anodal conductivity.
Except playing a part conduction, also has the effect of Electolyte-absorptive as the electric conducting material of conductive agent.Make conductive agent be dispersed in the electrode active material uniformly, can guarantee on the one hand in the electrolyte space that is present in pole piece as much as possible, particularly the repeated charge post consumption behind a large amount of electrolyte, also can guarantee to have a certain amount of electrolyte in the space of electrode active material, the even dispersion of conductive agent can guarantee that electrolyte is distributed in the space of electrode active material uniformly on the other hand, make after the repeated charge, battery still can keep higher capacity, is unlikely to cause in cyclic process the deterioration of battery to influence battery life.But, existing conductive agent, as carbon black, its grain diameter is bigger, causes specific area less, makes the conductive area of carbon black reduce, to such an extent as to conductance decline, thus cause the multiplying power discharging property of battery relatively poor.
In order to address the above problem, CN1516306A discloses a kind of secondary cell, and this secondary cell comprises: contain the positive pole of active material and electric conducting material, this active material is made of the transition metal oxide that contains lithium, negative pole and with anodal, the contacted electrolyte of negative pole;
Described electric conducting material comprises carbon black and acetylene black,
Described carbon black has graphite crystal and accumulates in its outside hollow shell structure, has the above DBP oil absorption of about 200 milliliters/100 grams, and the surface area that obtains with the nitrogen absorption process is 500 meters
2More than/the gram, and porosity is more than 35%,
It is characterized in that, the active material of per 100 weight portions, the ratio of described content of carbon black is in about 0.2 weight portion arrives the scope of about 1.0 weight portions; And
With respect to the described active material of per 100 weight portions, the ratio of described content of carbon black is that the content ratio of x weight portion, described acetylene black is under the situation of z weight portion, value (3x+z) about 1.1 in about 3.5 scope.
Oil absorption uses phthalic acid fourth two fat oil absorptions (DBP oil absorption) to represent as the performance index of carbon black materials to the absorbency of electrolyte.The absorbent correspondence of this DBP oil absorption and electrolyte.Employed carbon black can be the Kai Tien carbon black among the CN1516306A, it has high DBP oil absorption, show that it has absorbent properties preferably to electrolyte, and compare with general carbon black, the specific area of this carbon black increases greatly, though this carbon black that has than bigger serface has higher oil absorption, theoretically, this carbon black is because have big relatively specific area, thereby can absorb a large amount of electrolyte, but find that the cycle performance and the multiplying power discharging property of battery are unsatisfactory adding to this carbon black in the electrode material and be prepared in the process of battery.
Summary of the invention
The objective of the invention is to solve the cycle performance and the relatively poor problem of multiplying power discharging property of the lithium ion battery of prior art, a kind of lithium ion battery with good circulation performance and multiplying power discharging property is provided, and the positive pole of this battery and their preparation method.
The present inventor has carried out careful analysis to adopting the carbon black among the CN1516306A as the cycle performance and the relatively poor reason of multiplying power discharging property of the lithium ion battery of conductive agent, discovery is compared with general carbon black, the Kai Tien carbon black is because have bigger specific area and higher DBP oil absorption, thereby has a performance of good Electolyte-absorptive, but in the process of preparation positive electrode, with active material, when conductive agent and adhesive and solvent form slurry, because the specific area of this conductive agent is excessive, grain graininess is little, the sucking action of interaction forces such as electrostatic force between the particle and Van der Waals force makes that this carbon black is very easy to reunite, make solvent make this carbon black be difficult in positive electrode, be uniformly dispersed to the dipping of Kai Tien carbon black pellet difficulty, thereby, though described have that fully Electolyte-absorptive but the electrolyte that is not easy to absorb are uniformly distributed between the pole piece and active material of electrode than the Kai Tien carbon black of bigger serface, thereby cause the deterioration of battery in cyclic process, influence the cycle performance and the multiplying power discharging property of battery to the greatest extent.
Lithium ion cell positive provided by the invention comprises collector body and coating and/or is filled in positive electrode on the collector body, described positive electrode contains positive active material, conductive agent and adhesive, described conductive agent contains carbon black, and described carbon black has 500 meters that obtain with the nitrogen absorption process
2The specific area that/gram is above, wherein, this positive electrode also contains dispersant.
The preparation method of lithium ion cell positive provided by the invention comprises that the slurry that will contain positive active material, described conductive agent and adhesive and solvent applies and/or is filled on the collector body, dry, roll or do not roll, described conductive agent contains carbon black, and described carbon black has 500 meters that obtain with the nitrogen absorption process
2The specific area that/gram is above wherein, also contains dispersant in described slurry.
Lithium ion battery provided by the invention comprises pole piece and nonaqueous electrolytic solution, described pole piece and nonaqueous electrolytic solution are sealed in the battery container, described pole piece comprises the electrode and the barrier film of battery, described anode comprises collector body and coating and/or is filled in positive electrode on the collector body, described positive electrode contains positive active material, conductive agent and adhesive, described conductive agent contains carbon black, and described carbon black has with the nitrogen absorption process and obtains 500 meters
2The specific area that/gram is above, wherein, this positive electrode also contains dispersant.
The preparation method of lithium ion battery provided by the invention comprises pole piece and electrolyte is sealed in the battery case, described pole piece comprises battery electrode and barrier film, the preparation method of described anode comprises that the slurry that will contain positive active material, conductive agent and adhesive and solvent applies and/or is filled on the collector body, dry, roll or do not roll, described conductive agent contains carbon black, and described carbon black has 500 meters that obtain with the nitrogen absorption process
2The specific area that/gram is above wherein, also contains dispersant in described slurries.
Because the specific area of described carbon black is big, grain diameter is little, electrostatic force between the particle and Van der Waals force make described carbon black pellet very easily reunite, in the dispersion process after in electrode slurry, adding dispersant, a dispersant part is adsorbed on the surface of conductive agent particle, and another part is diffused in the electrode slurry.After being adsorbed onto described conductive agent particle surface, dispersant molecule can form electric double layer, on the one hand, the sucking action that has Van der Waals force between the particle, on the other hand, owing to be adsorbed on the dispersant of conductive agent particle surface the repulsive force between the particle is increased, and make particle mutually near the time owing to the overlapping of electric double layer produces repulsive interaction, thereby stoped the reunion of carbon black pellet; That part of dispersant that enters electrode slurry can form the non-electrical steric restriction that particle is assembled in decentralized medium, the existence of steric restriction makes the stability of dispersion strengthen.Therefore, because the adding of described dispersant, and improved the dispersive property of described conductive agent in the slurry that contains positive active material, described conductive agent, adhesive and solvent, reduce the interfacial tension between solvent and the conductive agent, and guaranteed the stability of anode sizing agent by sterically hindered structure.
Because the adding of dispersant has improved described conductive agent and has contained positive active material, described conductive agent, dispersive property in the slurry of adhesive and solvent, thereby make that the dispersion of described conductive agent in anode sizing agent is more even, thereby can give full play of the big advantage of described carbon black specific surface, and Electolyte-absorptive more fully, and the electrolyte that absorbs is uniformly distributed between anode pole piece and the active material, can guarantee on the one hand in the electrolyte space that is present in anode pole piece as much as possible, particularly the repeated charge post consumption also can guarantee under the situation of a large amount of electrolyte to have a certain amount of electrolyte in the space of positive active material, the even dispersion of conductive agent can guarantee that electrolyte is distributed in the space of positive active material uniformly on the other hand, thereby improves and improve the cycle performance and the multiplying power discharging property of battery.
Embodiment
According to the present invention, described dispersant is preferably one or more in polyisobutene succinimide, polyacrylamide, polyvinylpyrrolidone (PVP), poly(ethylene oxide) ether, hydroxyethylcellulose, polyacrylate, dodecyl poly(ethylene oxide) ester, fatty acid polyglycol oxirane ester, polycaprolactone, alkyl acid, alkyl dioxane, alkyl dioxolanes, the alkyl dioxepin.More preferably polyacrylamide and/or polyvinylpyrrolidone (PVP).Wherein, the number-average molecular weight of described polyisobutene succinimide, polyacrylamide, polyvinylpyrrolidone (PVP), poly(ethylene oxide) ether, hydroxyethylcellulose, polyacrylate, dodecyl poly(ethylene oxide) ester, fatty acid polyglycol oxirane ester, polycaprolactone is preferably 500-50000.
(1) molecular structure of alkyl acid is as follows:
(2) molecular structure of alkyl dioxane is as follows:
(3) molecular structure of alkyl dioxolanes is as follows:
(4) molecular structure of alkyl dioxepin is as follows:
(5) structure of polyvinylpyrrolidone is as follows:
Above-mentioned dispersant can be commercially available.The model that provides as Shanghai dimension ketone Materials Co., Ltd is that the number-average molecular weight of the polyvinylpyrrolidone of PVP K17 is 8000, and model is that the number-average molecular weight of the polyvinylpyrrolidone of PVP K25 is 34000.
According to the present invention, just can improve the dispersive property of described carbon black in the slurry that contains electrode active material, described conductive agent, adhesive and solvent as long as add described dispersant, under the preferable case, weight with described conductive agent is benchmark, the content of described dispersant is 0.5-15 weight %, is preferably 1-10 weight %.
Disperse more uniform carbon black to have the performance of better Electolyte-absorptive in positive electrode after making the described dispersant of adding, described carbon black is except having 500 meters that obtain with the nitrogen absorption process
2More than/the gram, be preferably 500 meters
2-1500 meters of/grams
2Beyond the specific area of/gram, under the preferable case, the DBP oil absorption of described carbon black is more than 300 milliliters/100 grams, is preferably 300 milliliters/100 grams-600 milliliters/100 grams, and has graphite crystal and accumulate in its outside hollow shell structure.The carbon black that preferably adopts as the present invention is Kai Tien carbon black ECP, and the DBP oil absorption is 360 milliliters/100 grams, and the specific area that obtains with the nitrogen absorption process is 800 meters
2/ gram; Kai Tien carbon black ECP600JD, the DBP oil absorption is 500 milliliters/100 grams, the specific area that obtains with the nitrogen absorption process is 1400 meters
2/ gram, Te Migao carbon black ENSACO350G, the DBP oil absorption is 300 milliliters/100 grams, the specific area that obtains with the nitrogen absorption process is 770 meters
2/ gram.Above-mentioned carbon black can be commercially available, and also can prepare according to method known in those skilled in the art.
Dispersant provided by the invention can well be scattered in the positive electrode by described conductive agent particle diameter is little, that specific area is big, thereby improve the dispersive property of described conductive agent in anode sizing agent, make described conductive agent Electolyte-absorptive and the electrolyte that absorbs is uniformly distributed between electrode plates and the active material fully.According to a specific embodiments of the present invention, with described carbon black is example, and through screening, the present inventor also is surprised to find that, described dispersant can be the 0.01-0.5 micron with particle diameter especially, is preferably more uniform being scattered in the positive electrode of described carbon black of 0.01-0.1 micron.Adopting particle diameter is the 0.01-0.5 micron, is preferably the lithium ion battery of the described carbon black of 0.01-0.1 micron and the positive electrode preparation that described dispersant prepares, and has better cycle performance and multiplying power discharging property.
Described anodal conductive agent has 500 meters that obtain with the nitrogen absorption process except containing
2More than/the gram, be preferably 500 meters
2-1500 meters of/grams
2Beyond the carbon black of the specific area of/gram, as Kai Tien carbon black ECP, Kai Tien carbon black ECP600JD, Te Migao carbon black ENSACO350G can also contain conventional electric conducting material, as graphite, acetylene black, furnace black, carbon fiber etc., the content of described conductive agent is the content of this area routine, weight with described positive active material is benchmark, and the content of described conductive agent is 0.2-2.5 weight %, is preferably 0.3-2.0 weight %.
According to the positive pole of lithium ion battery provided by the invention, described positive active material is not particularly limited, and can be selected from the active material that embedding of this area routine disengaged lithium.One or more in the preferred following material of positive active material: Li wherein
xNi
1-yCoO
2(wherein, 0.9≤x≤1.1,0≤y≤1.0), Li
1+aM
bMn
2-bO
4(wherein ,-0.1≤a≤0.2,0≤b≤1.0, M is a kind of in lithium, boron, magnesium, aluminium, titanium, chromium, iron, cobalt, nickel, copper, zinc, gallium, yttrium, fluorine, iodine, the element sulphur), Li
mMn
2-nB
nO
2(wherein, B is a transition metal, 0.9≤m≤1.1,0≤n≤1.0).
The kind of described anodal adhesive and content are conventionally known to one of skill in the art, for example one or more in fluorine resin and polyolefin compound such as polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), the butadiene-styrene rubber (SBR).In general, according to the difference of used anodal adhesive kind, be benchmark with the weight of positive active material, the content of anodal adhesive is 2-10 weight %, is preferably 2-5 weight %.
Positive electrode collector can be positive electrode collector conventional in the lithium ion battery, uses aluminium foil as positive electrode collector in specific embodiments of the present invention.
Preparation method according to positive pole provided by the invention, electrode active material, described conductive agent and adhesive are joined in the solvent, be mixed and made into slurry, the slurry that will be mixed with dispersant then applies and/or is filled on the collector body, dry, roll or do not roll, wherein, with electrode active material, described conductive agent and adhesive and solvent the time, also add dispersant.Described dispersant can add arbitrarily the time, as can with electrode active material, as described in conductive agent and adhesive add before joining solvent, can add simultaneously with electrode active material, conductive agent and adhesive or add later in that in electrode active material, conductive agent and the adhesive one or more are joined solvent; Described dispersant can add separately also can mix the back adding with conductive agent.Under the preferable case, after joining adhesive in the solvent, with described dispersant with join the above-mentioned solvent that contains adhesive after described conductive agent mixes, add positive active material at last.Wherein, described solvent can be selected from one or more in N-methyl pyrrolidone (NMP), dimethyl formamide (DMF), diethylformamide (DEF), dimethyl sulfoxide (DMSO) (DMSO), oxolane (THF) and water and the alcohols.The consumption of solvent can make described slurry be coated on the described collector body and get final product.In general, be benchmark with the weight of described positive active material, the consumption of described solvent is 5-70 weight %, is preferably 15-50 weight %.Wherein, described slurry applied and/or be filled in the method on the described collector body, drying, the method for calendering and condition are conventionally known to one of skill in the art.
Lithium ion battery provided by the present invention comprises pole piece and nonaqueous electrolytic solution, and described pole piece and nonaqueous electrolytic solution are sealed in the battery container, and described pole piece comprises positive pole, negative pole and barrier film.Except using, can use conventional negative pole, barrier film, nonaqueous electrolytic solution by the positive pole provided by the invention.
Described barrier film is arranged between positive pole and the negative pole, and it has electrical insulation capability and liquid retainability energy, and described pole piece and nonaqueous electrolytic solution are contained in the battery case together.Described barrier film can be selected from various barrier films used in the lithium ion battery, as polyolefin micro porous polyolefin membrane.The position of described barrier film, character and kind are conventionally known to one of skill in the art.
Consisting of of described negative pole is conventionally known to one of skill in the art.In general, negative pole comprises collector body and coating and/or is filled in negative material on the collector body that described negative material comprises negative electrode active material and negative pole adhesive.
The negative electrode active material of described negative pole is not particularly limited, can use embedding of this area routine to disengage the negative electrode active material of lithium, such as in native graphite, Delanium, petroleum coke, organic cracking carbon, carbonaceous mesophase spherules, carbon fiber, ashbury metal, the silicon alloy one or more, preferred electrographite.
Described negative pole adhesive can adopt adhesive used in the positive pole.The content of adhesive is conventionally known to one of skill in the art, is generally the 1-10 weight % of negative electrode active material, is preferably 1-5 weight %.
Negative pole of the present invention can also contain conductive agent, described conductive agent is not particularly limited, can be the cathode conductive agent of this area routine, at least a such as in acetylene black, conductive carbon black and the electrically conductive graphite, weight with negative electrode active material is benchmark, the content of described conductive agent is 1-15 weight %, is preferably 2-10 weight %.
Negative electrode collector can be for negative electrode collector conventional in the lithium ion battery, as stamped metal, and metal forming, net metal, foamed metal uses Copper Foil as negative electrode collector in specific embodiments of the present invention.
The preparation method of described negative pole comprises that the slurry that will contain negative electrode active material and adhesive and solvent applies and/or is filled on the collector body, and drying is rolled or do not rolled.Wherein, described solvent can be selected from one or more in N-methyl pyrrolidone (NMP), dimethyl formamide (DMF), diethylformamide (DEF), dimethyl sulfoxide (DMSO) (DMSO), oxolane (THF) and water and the alcohols.The consumption of described solvent can make described pastel have viscosity and flowability, can be coated on the described collector body to get final product.In general, be benchmark with the weight of negative electrode active material, the consumption of described solvent is 50-150%.Wherein, described slurry applied and/or be filled in the method on the described collector body, drying, the method for calendering and condition are conventionally known to one of skill in the art.
Described nonaqueous electrolytic solution is the mixed solution of electrolyte lithium salt and nonaqueous solvents, and it is not particularly limited, and can use the nonaqueous electrolytic solution of this area routine.Be selected from lithium hexafluoro phosphate (LiPF such as electrolyte lithium salt
6), in lithium perchlorate, LiBF4, hexafluoroarsenate lithium, lithium halide, chlorine lithium aluminate and the fluorocarbon based sulfonic acid lithium one or more.Organic solvent is selected chain acid esters and ring-type acid esters mixed solution for use, wherein the chain acid esters can be dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), carbonic acid first propyl ester (MPC), dipropyl carbonate (DPC) and other are fluorine-containing, sulfur-bearing or contain at least a in the chain organosilane ester of unsaturated bond, the ring-type acid esters can be ethylene carbonate (EC), propene carbonate (PC), vinylene carbonate (VC), gamma-butyrolacton (γ-BL), sultone and other are fluorine-containing, sulfur-bearing or contain at least a in the ring-type organosilane ester of unsaturated bond.
According to the preparation method of lithium ion battery provided by the invention, except described positive pole prepared according to method provided by the invention, other step was conventionally known to one of skill in the art.In general, the described positive pole for preparing, negative pole and membrane coil around constituting a pole piece, are contained in this pole piece in the battery container, inject electrolyte, then that battery container is airtight, can obtain lithium ion battery provided by the invention.
The following examples will the present invention will be further described.
Embodiment 1
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
90 gram polyvinylidene fluoride are dissolved among the 1350 gram NMP, add then 30 gram carbon blacks (the triumphant benefactor of carrying department commodity, trade mark is called ECP600JD, the carbon black pellet diameter is 0.03 micron, 1400 meters of specific areas
2/ restrain DBP oil absorption 500 milliliters/100 grams) restrain anodal active component LiCoO with 1.5 mixtures and 3000 that restrain polyvinylpyrrolidones (Shanghai dimension ketone Materials Co., Ltd, PVP K25, number-average molecular weight 34000)
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, then in 125 ℃ of following oven dry, roll-in, cut to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A1 is made in sealing.
Embodiment 2
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
90 gram polyvinylidene fluoride are dissolved among the 1350 gram NMP, add then 9 gram carbon blacks (the triumphant benefactor of carrying department commodity, trade mark is called ECP, the carbon black pellet diameter is 0.04 micron, 800 meters of specific areas
2/ restrain DBP oil absorption 360 milliliters/100 grams) restrain anodal active component LiCoO with 0.45 mixture and 3000 that restrains polyvinylpyrrolidone (Shanghai dimension ketone Materials Co., Ltd, PVP K17, number-average molecular weight 8000)
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, 125 ℃ of following oven dry, roll-ins then, cuts to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A2 is made in sealing.
Embodiment 3
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
90 gram polyvinylidene fluoride are dissolved among the 1350 gram NMP, add then 60 gram carbon blacks (the triumphant benefactor of carrying department commodity, trade mark is called ECP600JD, the carbon black pellet diameter is 0.03 micron, 1400 meters of specific areas
2/ gram, DBP oil absorption 500 milliliters/100 grams) with 3 gram dispersants (polyacrylamide (number-average molecular weight 20000): polyvinylpyrrolidone (Shanghai dimension ketone Materials Co., Ltd, PVP K17, number-average molecular weight 8000)=1: 1) mixture and the anodal active component LiCoO of 3000 grams
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, then in 125 ℃ of following oven dry, roll-in, cut to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A3 is made in sealing.
Embodiment 4
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
With 90 the gram polyvinylidene fluoride be dissolved in 1350 the gram NMP in, add then 30 the gram carbon blacks (the Te Migao carbon black, trade mark is called ENSACO350G, the carbon black pellet diameter is 0.03 micron, 770 meters of specific areas
2/ restrain DBP oil absorption 300 milliliters/100 grams) restrain anodal active component LiCoO with 0.3 mixture and 3000 that restrains polyvinylpyrrolidone (Shanghai dimension ketone Materials Co., Ltd, PVP K25, number-average molecular weight 34000)
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, then in 125 ℃ of following oven dry, roll-in, cut to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A4 is made in sealing.
Embodiment 5
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
With 90 the gram polyvinylidene fluoride be dissolved in 1350 the gram NMP in, add then 30 the gram carbon blacks (the Te Migao carbon black, trade mark is called ENSACO350G, the carbon black pellet diameter is 0.03 micron, 770 meters of specific areas
2/ restrain DBP oil absorption 300 milliliters/100 grams) restrain anodal active component LiCoO with 3 mixtures and 3000 that restrain polyvinylpyrrolidones (Shanghai dimension ketone Materials Co., Ltd, PVP K25, number-average molecular weight 34000)
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, then in 125 ℃ of following oven dry, roll-in, cut to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A5 is made in sealing.
Embodiment 6
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
With 90 the gram polyvinylidene fluoride be dissolved in 1350 the gram NMP in, add then 30 the gram carbon blacks (the Te Migao carbon black, trade mark is called ENSACO350G, the carbon black pellet diameter is 0.03 micron, 770 meters of specific areas
2/ gram, DBP oil absorption 300 milliliters/100 grams) with 3 gram dispersants (polymethyl acrylate (number-average molecular weight 50000): dodecyl poly(ethylene oxide) ester (number-average molecular weight 10000): polyvinylpyrrolidone (Shanghai dimension ketone Materials Co., Ltd, PVP K25, number-average molecular weight 34000): polyacrylamide (number-average molecular weight 15000)=1: 1: 2: mixture 1) and the anodal active component LiCoO of 3000 grams
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, then in 125 ℃ of following oven dry, roll-in, cut to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A6 is made in sealing.
Comparative Examples 1
This Comparative Examples illustrates that reference is anodal and contains this anodal lithium ion battery and their preparation method.
Adopt the method identical with embodiment 1, except positive pole did not contain dispersant, other various compositions and consumption were all identical.Prepare reference lithium ion battery AC1.
Embodiment 7
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
90 gram polyvinylidene fluoride are dissolved among the 1350 gram NMP, add then 30 gram carbon blacks (the triumphant benefactor of carrying department commodity, trade mark is called ECP600JD, the carbon black pellet diameter is 0.03 micron, 1400 meters of specific areas
2/ gram, DBP oil absorption 500 milliliters/100 grams), 30 gram acetylene blacks and 3 gram dispersants (myristyl dioxolanes: polyvinylpyrrolidone (Shanghai dimension ketone Materials Co., Ltd, PVP K25, number-average molecular weight 34000): mixture octadecyl dioxane=1: 2: 1) and the anodal active component LiCoO of 3000 grams
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, then in 125 ℃ of following oven dry, roll-in, cut to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A7 is made in sealing.
Embodiment 8
Present embodiment illustrates lithium ion battery provided by the invention and positive pole and their preparation method.
(1) Zheng Ji preparation
With 90 the gram polyvinylidene fluoride be dissolved in 1350 the gram NMP in, add then 15 the gram carbon blacks (the Te Migao carbon black, trade mark is called ENSACO350G, the carbon black pellet diameter is 0.03 micron, 770 meters of specific areas
2/ gram, DBP oil absorption 300 milliliters/100 grams), 30 gram acetylene blacks and 0.75 gram dispersant (polyacrylamide (number-average molecular weight 20000): polyvinylpyrrolidone (Shanghai dimension ketone Materials Co., Ltd, PVPK17, number-average molecular weight 8000)=1: 2) mixture and the anodal active component LiCoO of 3000 grams
2, and in mixer, stir the uniform anode sizing agent of formation.
This slurry is coated on the aluminium foil equably, then in 125 ℃ of following oven dry, roll-in, cut to make and be of a size of 375 * 43.5 millimeters positive pole, wherein contain the anodal material of 6.1 grams.
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 4 gram bonding agent Kynoar are joined among the 100 gram NMP, in mixer, stir then and form uniform cathode size.
This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 340 * 44.5 millimeters negative pole, wherein contain 2.6 gram negative pole material.
(3) assembling of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery, subsequently with LiPF
6Concentration by 1 mol is dissolved in EC/DMC=1: form nonaqueous electrolytic solution in 1 the mixed solvent, this electrolyte is injected battery case with the amount of 3.8g/Ah, lithium ion battery A8 is made in sealing.
Comparative Examples 2
This Comparative Examples illustrates that reference is anodal and contains this anodal lithium ion battery and their preparation method.
Adopt the method identical with embodiment 7, except positive pole did not contain dispersant, other various compositions and consumption were all identical.Prepare reference lithium ion battery AC2.
Embodiment 9-16
The following example is measured battery capacity and multiplying power discharging property and the cycle performance of lithium ion battery A1, A2, A3, A4, A5, A6, A7 and A8 that embodiment 1-8 makes respectively.
Battery capacity test: to 4.2V, with constant-potential charge, is 25mA by electric current with the constant current charge of 800mA after voltage rises to 4.2V; With the constant current discharge of 800mA, be 3.0V then, measure the capacity of battery by voltage.
C
2C/ C
0.2C: the electric current with 2C is discharged to the discharge capacity of 3.0V and the ratio that is discharged to the discharge capacity of 3.0V with the electric current of 0.2C from 4.2V from 4.2V.
Cycle performance: under 23 ℃ of conditions, with battery respectively with the 1C current charges to 4.2V, with constant-potential charge, cut-off current is 0.05C after voltage rises to 4.2V, shelves 10 minutes; Battery, was shelved 5 minutes to 3.0V with the 1C current discharge.Capacity with first charge-discharge is the initial capacity of this battery, the cycle-index when record circulation back battery capacity is initial capacity 80%.
Measurement result is as shown in table 1.
Comparative Examples 3-4
Reference lithium ion battery AC1 that this Comparative Examples mensuration Comparative Examples 1,2 makes and battery capacity, multiplying power discharging property and the cycle performance of AC2.
Adopt with embodiment 9-16 in identical method measure, the battery of mensuration that different is is reference lithium ion battery AC1 and AC2.
The result is as shown in table 1.
Table 1
| The embodiment numbering | The battery numbering | Initial capacity | C 2C/C 0.2CMultiplying power (%) | Cycle-index |
| Embodiment 9 | A1 | 814 | 96.7 | 453 |
| Embodiment 10 | A2 | 836 | 94.3 | 438 |
| Embodiment 11 | A3 | 809 | 97.2 | 459 |
| Embodiment 12 | A4 | 812 | 96.5 | 441 |
| Embodiment 13 | A5 | 818 | 96.7 | 469 |
| Embodiment 14 | A6 | 818 | 95.1 | 404 |
| Comparative Examples 3 | AC1 | 788 | 89.3 | 265 |
| Embodiment 15 | A7 | 805 | 96.8 | 452 |
| Embodiment 16 | A8 | 807 | 95.3 | 431 |
| Comparative Examples 4 | AC2 | 801 | 92.5 | 283 |
From the result shown in the table 1 as can be seen, compare with reference cell, lithium ion battery provided by the invention has excellent cycle performance and multiplying power discharging property.
Claims (13)
1, a kind of positive pole of lithium ion battery, this positive pole comprises collector body and coating and/or is filled in positive electrode on the collector body, described positive electrode contains positive active material, conductive agent and adhesive, and described conductive agent contains carbon black, and described carbon black has 500 meters that obtain with the nitrogen absorption process
2The specific area that/gram is above, wherein, this positive electrode also contains dispersant, and the particle diameter of described carbon black is the 0.01-0.5 micron.
2, positive pole according to claim 1, wherein, described dispersant is selected from one or more in polyisobutene succinimide, polyacrylamide, polyvinylpyrrolidone, poly(ethylene oxide) ether, hydroxyethylcellulose, polyacrylate, dodecyl poly(ethylene oxide) ester, fatty acid polyglycol oxirane ester, polycaprolactone, alkyl acid, alkyl dioxane, alkyl dioxolanes, the alkyl dioxepin.
3, positive pole according to claim 2, wherein, described dispersant is polyacrylamide and/or polyvinylpyrrolidone.
4, positive pole according to claim 1, wherein, the DBP oil absorption of described carbon black is more than 300 milliliters/100 grams.
5, positive pole according to claim 1, wherein, described carbon black has graphite crystal and accumulates in its outside hollow shell structure.
6, positive pole according to claim 1 wherein, is a benchmark with the weight of the conductive agent in the described positive electrode, and the content of described dispersant is 0.5-15 weight %.
7, positive pole according to claim 6 wherein, is a benchmark with the weight of the conductive agent in the described positive electrode, and the content of described dispersant is 1-10 weight %.
8, the preparation method of the described positive pole of claim 1, this method comprises that the slurry that will contain positive active material, conductive agent and adhesive and solvent applies and/or is filled on the collector body, dry, roll or do not roll, described conductive agent contains carbon black, and described carbon black has 500 meters that obtain with the nitrogen absorption process
2The specific area that/gram is above wherein, also contains dispersant in described slurry, the particle diameter of described carbon black is the 0.01-0.5 micron.
9, method according to claim 8, wherein, described dispersant is selected from one or more in polyisobutene succinimide, polyacrylamide, polyvinylpyrrolidone, poly(ethylene oxide) ether, hydroxyethylcellulose, polyacrylate, dodecyl poly(ethylene oxide) ester, fatty acid polyglycol oxirane ester, polycaprolactone, alkyl acid, alkyl dioxane, alkyl dioxolanes, the alkyl dioxepin.
10, a kind of lithium ion battery, this battery comprises pole piece and nonaqueous electrolytic solution, described pole piece and nonaqueous electrolytic solution are sealed in the battery container, described pole piece comprises positive pole, negative pole and the barrier film of battery, described anode comprises collector body and coating and/or is filled in positive electrode on the collector body, described positive electrode contains positive active material, conductive agent and adhesive, and described conductive agent contains carbon black, and described carbon black has 500 meters that obtain with the nitrogen absorption process
2The specific area that/gram is above, wherein, positive electrode also contains dispersant, and the particle diameter of described carbon black is the 0.01-0.5 micron.
11, battery according to claim 10, wherein, described dispersant is selected from one or more in polyisobutene succinimide, polyacrylamide, polyvinylpyrrolidone, poly(ethylene oxide) ether, hydroxyethylcellulose, polyacrylate, dodecyl poly(ethylene oxide) ester, fatty acid polyglycol oxirane ester, polycaprolactone, alkyl acid, alkyl dioxane, alkyl dioxolanes, the alkyl dioxepin.
12, the preparation method of the described battery of claim 10, this method comprises pole piece and electrolyte is sealed in the battery case, described pole piece comprises anode, negative pole and barrier film, the preparation method of described anode comprises that the slurry that will contain positive active material, conductive agent and adhesive and solvent applies and/or is filled on the collector body, dry, roll or do not roll, described conductive agent contains carbon black, and described carbon black has 500 meters that obtain with the nitrogen absorption process
2The specific area that/gram is above wherein, also contains dispersant in described slurry, the particle diameter of described carbon black is the 0.01-0.5 micron.
13, method according to claim 12, wherein, described dispersant is selected from one or more in polyisobutene succinimide, polyacrylamide, polyvinylpyrrolidone, poly(ethylene oxide) ether, hydroxyethylcellulose, polyacrylate, dodecyl poly(ethylene oxide) ester, fatty acid polyglycol oxirane ester, polycaprolactone, alkyl acid, alkyl dioxane, alkyl dioxolanes, the alkyl dioxepin.
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| CN102099947A (en) * | 2008-06-04 | 2011-06-15 | 东洋油墨制造股份有限公司 | Composition for battery |
| JP5471598B2 (en) * | 2010-03-02 | 2014-04-16 | ソニー株式会社 | Non-aqueous electrolyte battery |
| CN106165041A (en) | 2014-04-08 | 2016-11-23 | 麦斯韦尔技术股份有限公司 | Energy storage device, its negative pole and the method manufacturing energy storage device |
| CN104332591B (en) * | 2014-09-05 | 2016-08-24 | 济宁市无界科技有限公司 | A kind of lithium ion battery anode glue size and preparation technology thereof |
| KR20160139240A (en) | 2015-05-27 | 2016-12-07 | 주식회사 엘지화학 | Electrode mixture, preparation method thereof and secondary battery comprising the same |
| JP6994157B2 (en) * | 2018-02-09 | 2022-01-14 | トヨタ自動車株式会社 | Non-aqueous electrolyte secondary battery and battery assembly |
| JP7107382B2 (en) * | 2018-09-19 | 2022-07-27 | 株式会社村田製作所 | secondary battery |
| JP7466211B2 (en) * | 2019-04-10 | 2024-04-12 | パナソニックＩｐマネジメント株式会社 | Positive electrode for non-aqueous electrolyte secondary battery and non-aqueous electrolyte secondary battery |
| KR20210097528A (en) * | 2020-01-30 | 2021-08-09 | 주식회사 엘지화학 | Method for preparing positive electrode active material for lithium secondary battery and positive electrode active material prepared thereby |
| CN112864395B (en) * | 2021-03-10 | 2022-11-04 | 合肥国轩高科动力能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| WO2022198401A1 (en) * | 2021-03-22 | 2022-09-29 | 宁德新能源科技有限公司 | Electrochemical device and electronic device |
| CN113725497A (en) * | 2021-09-03 | 2021-11-30 | 天能帅福得能源股份有限公司 | Preparation method of low-cost high-performance lithium ion battery using dispersing agent |
| CN115611285B (en) * | 2022-10-13 | 2023-06-23 | 焦作市和兴化学工业有限公司 | Slurry, preparation method and equipment thereof |
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