CN105336961A - Lithium battery anode and preparation method thereof - Google Patents
Lithium battery anode and preparation method thereof Download PDFInfo
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- CN105336961A CN105336961A CN201510857119.5A CN201510857119A CN105336961A CN 105336961 A CN105336961 A CN 105336961A CN 201510857119 A CN201510857119 A CN 201510857119A CN 105336961 A CN105336961 A CN 105336961A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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Abstract
The invention belongs to the field of cellulose and new energy lithium ion battery materials, and in particular relates to a lithium battery anode and a preparation method thereof. The lithium battery anode is prepared from the following raw materials in percentage by weight: 80 to 97 percent of an active substance, 1 to 4 percent of acetylene black, 0.5 to 10 percent of carboxymethyl cellulose lithium and 0 to 10 percent of other adhesives. The lithium battery anode is prepared by the following steps: dissolving carboxymethyl cellulose lithium into deionized water to prepare a carboxymethyl cellulose lithium solution with the mass percentage of 1 to 4 percent, adding the active substance, the acetylene black and other adhesives into the solution, uniformly mixing, obtaining mixed slurry, pouring the mixed slurry onto a current collector copper foil, drying and compacting, cutting the current collector copper foil into electrode slices according to an actual requirement, and obtaining the lithium battery anode. A lithium battery prepared from the lithium battery anode has the advantages of long service life and the like.
Description
Technical field
The invention belongs to cellulose and new forms of energy field of lithium ion battery material, be specifically related to a kind of Anode of lithium cell and preparation method thereof.
Background technology
Along with the fast development of field of lithium, the device demand of more portable, more frivolous, safer and high-octane lithium battery design is also increased thereupon.The electrode of lithium battery is formed at collection liquid surface through adhesive-coated by active material, conductive agent.Carrying out in charge and discharge process to lithium battery, because lithium ion interts back and forth at Yin/Yang interpolar, easily cause Yin/Yang pole active material to come off, be even separated with collector, capacity reduces to cause battery to occur, cycle life reduces, and directly has influence on battery performance.So binding agent is as the very important part of in lithium battery material, there is stronger adhesion strength, the manufacturing process of energy stable cell, and dispersiveness and the mechanical property of electrode can be increased, thus produce the lithium battery with excellent properties.In the binding agent of numerous lithium batteries, Kynoar (PVDF) oil-soluble binding agent using organic solvent 1-METHYLPYRROLIDONE (NMP) as dispersant is the most common, and PVDF lithium battery binder product molecular weight distribution is on the market wider, degree of crystallinity is generally about 40%, crystallization temperature is near 140 DEG C, degree of crystallinity is higher, ion is more difficult in migration, resistance internal resistance is easily caused to raise, it is easier that active material departs from from collector, causes capacity to be deteriorated.And there is more drawback as the dispersant of PVDF binding agent in NMP, such as poisonous, contaminated environment, recovery difficulty, cost are high, the high deficiency of operation technological requirement, increasing manufacturer brings into use aqueous binders to produce electrode of lithium cell.
Carboxymethyl cellulose-based material is widely applied in Anode of lithium cell material as aqueous lithium ion battery binding agent, mainly contain following feature: the carboxymethyl cellulose-based material one, containing hydroxyl and carboxymethyl structure, according to the difference of preparation technology can obtain different degree of etherification falling, different molecular weight, different quality product meet the requirement of the cohesive force of lithium battery binding agent; Two, the molecular structure property of ion can be ionized out, the requirement of the chemical property of lithium battery binding agent can be met; Three, take natural cellulosic materials as the product of raw material, can environmental protection be met, the requirement of convenient post-treatment; Four, take water as dispersant, cost is low, environmental friendliness, and manufacturing process is easy to operate.
Japanese Patent Publication No.JP5-74461 discloses sodium carboxymethylcellulose (CMC-Na or CMC) and butadiene-styrene rubber (SBR) binding agent as lithium battery to improve the performance of anode, is realized by the etherificate or the degree of polymerization regulating CMC-Na.Korea S's Samsung is applied for a patent bulletin CN100457848C and is disclosed a kind of Anode of lithium cell containing carboxymethyl cellulose-based binder and use the lithium battery of this carboxymethyl cellulose-based binder, but refer in particular in this patent, the cation of carboxymethyl cellulose binding agent is by Na
+or NH
4 +the binding agent of the carboxymethyl cellulose-based structure that salt replaces.Along with the application of sodium carboxymethylcellulose (CMC-Na) in lithium battery gets more and more, also more and more higher to the requirement of CMC-Na, have data to show, using CMC-Na as binding agent, under long-term discharge scenario, battery efficiency and cycle characteristics decline very fast; The sodium ion ionized out may with the lithium ion generation exchange reaction of carbon anode surface, reduce the deintercalation efficiency of lithium ion, after reacting with the lithium ion in electrolyte, easily promote the decomposition of electrolyte solution.Meanwhile, the advantages such as sodium salt electrical efficiency is relatively lower, little for lithium battery volume, light weight, and energy is high can not fully demonstrate.And the insufficient infiltration of electrolyte in active particle easily causes the interface resistance of electrode to increase and battery internal resistance increases, and under the environment that temperature is lower, what easily appearance was serious analyses lithium phenomenon, impacts the security performance of battery.
Summary of the invention
For existing Problems existing, goal of the invention of the present invention is to provide a kind of carboxymethyl cellulose lithium as the application of binding agent on Anode of lithium cell.This carboxymethyl cellulose lithium binding agent has better water-soluble than sodium carboxymethylcellulose binding agent, carboxymethyl cellulose lithium binding agent slurry has better dispersed and cohesive force.
First technical problem to be solved by this invention is to provide carboxymethyl cellulose lithium and is preparing the purposes on Anode of lithium cell.
Second technical problem to be solved by this invention is to provide a kind of Anode of lithium cell.This Anode of lithium cell is characterised in that using carboxymethyl cellulose lithium and prepares as binding agent.
Preferably, in above-mentioned Anode of lithium cell, described binding agent also comprises other binding agent except carboxymethyl cellulose lithium.
Preferably, above-mentioned Anode of lithium cell, is prepared from by the raw material of following percentage by weight: active material 80 ~ 97%, acetylene black 1 ~ 4%, carboxymethyl cellulose lithium 0.5 ~ 10%, other binding agent 0 ~ 10%.
Preferably, above-mentioned Anode of lithium cell, is prepared from by the raw material of following percentage by weight: active material is 90 ~ 97%, acetylene black 1 ~ 3%, carboxymethyl cellulose lithium 1 ~ 5%, other binding agent 0 ~ 3%.
Preferably, in above-mentioned Anode of lithium cell, described active material is: graphite material, at least one in the compound be made up of at least one element in Al, Si, Sn, Bi, Zn, Ge, Ti, Ag, Mg, In, Pb, at least one in the alloy formed by least one element and lithium in Al, Si, Sn, Bi, Zn, Ge, Ti, Ag, Mg, In, Pb, lithium nitride.
Further, in above-mentioned Anode of lithium cell, the compound that described graphite material is native graphite, coke, Delanium, carbon fiber or material with carbon element are formed.
Further, in above-mentioned Anode of lithium cell, other described binding agent is: butadiene-styrene rubber, LA132/133/135 or sodium carboxymethylcellulose.
3rd technical problem to be solved by this invention is to provide a kind of preparation method of Anode of lithium cell.The method comprises the following steps: carboxymethyl cellulose lithium is mixed with the carboxymethyl cellulose lithium solution that mass fraction is 1 ~ 4%, after adding active material, acetylene black, other binding agent more wherein, mixing obtains mixed slurry, mixed slurry is cast on copper foil of affluxion body, compacting after dry, be cut into electrode slice by actual requirement, obtain Anode of lithium cell.
Preferably, in the preparation method of above-mentioned Anode of lithium cell, described drying for be dried to constant weight at 92 ~ 105 DEG C.
The present invention's carboxymethyl cellulose lithium salts replaces sanlose, can provide lithium ion to extraly whole lithium battery, add the total number of lithium ion; Simultaneously, carboxymethyl cellulose lithium is as Ionomer, itself also can in conjunction with and ionize out lithium ion, Lithium-ion embeding and the quantity of deviating between raising both positive and negative polarity that can be extra, improve the specific capacity of battery, the cycle efficieny of battery can be improved again, shorten the path of lithium ion motion between both positive and negative polarity, lithium ion radius is little, conductivity and conductivity high.Carrying out under 2C multiplying power discharging state, specific capacity at least can be more used than present lithium battery sodium carboxymethylcellulose improve more than 5%, the internal resistance of cell sodium carboxymethylcellulose more used than present lithium battery improves more than at least 10%, under same loop, capacity loss is lower, cycle efficieny is higher, longer service life.
Accompanying drawing explanation
The AC impedance figure of Fig. 1 embodiment 1 and comparative example 1
The cycle life curve chart of Fig. 2 embodiment and comparative example
Embodiment
In field of lithium, Kynoar (PVDF) oil-soluble binding agent using organic solvent 1-METHYLPYRROLIDONE (NMP) as dispersant is the most common, and PVDF molecular weight distribution is wider, degree of crystallinity is generally about 40%, and crystallization temperature is near 140 DEG C, and degree of crystallinity is higher, ion is more difficult in migration, easily cause resistance internal resistance to raise, it is easier that active material departs from from collector, causes capacity to be deteriorated.And there is more drawback as the dispersant of PVDF binding agent in NMP, such as poisonous, contaminated environment, recovery difficulty, cost are high, the high deficiency of operation technological requirement, increasing manufacturer brings into use aqueous binders to produce electrode of lithium cell.
In view of the above problems, this area starts again to adopt sodium carboxymethylcellulose (CMC-Na or CMC) as the binding agent of lithium battery to improve the performance of anode.But using CMC-Na as binding agent, under long-term discharge scenario, battery efficiency and cycle characteristics decline very fast; The sodium ion ionized out may with the lithium ion generation exchange reaction of carbon anode surface, reduce the deintercalation efficiency of lithium ion, after reacting with the lithium ion in electrolyte, easily promote the decomposition of electrolyte solution.Meanwhile, the advantages such as sodium salt electrical efficiency is relatively lower, little for lithium battery volume, light weight, and energy is high can not fully demonstrate.And the insufficient infiltration of electrolyte in active particle easily causes the interface resistance of electrode to increase and battery internal resistance increases, and under the environment that temperature is lower, what easily appearance was serious analyses lithium phenomenon, impacts the security performance of battery.
The present invention is in the application providing carboxymethyl cellulose lithium for the deficiencies in the prior art on Anode of lithium cell.This lithium salts replaces sodium salt, and whole lithium battery of giving that can be extra provides lithium ion, and add the total number of the lithium ion in whole lithium battery system, CMC-Li is as Ionomer simultaneously, itself also has the ability combining and ionize out lithium ion.So, carboxymethyl cellulose lithium can be extra raising both positive and negative polarity between Lithium-ion embeding and the quantity of deviating from, improve the specific capacity of battery, the cycle efficieny of battery can be improved again, shorten the path of lithium ion motion between both positive and negative polarity, have conductivity and conductivity is higher, electrolyte permeability is advantage more fully.
Meanwhile, the inventive method additionally provides the method utilizing carboxymethyl cellulose lithium to prepare Anode of lithium cell.The method comprises the following steps: raw material is made up of the material of following percentage by weight, active material 80 ~ 97%, acetylene black 1 ~ 4%, carboxymethyl cellulose lithium 0.5 ~ 10%, other binding agent 0 ~ 10%; Carboxymethyl cellulose lithium is dissolved and is mixed with the carboxymethyl cellulose lithium solution that mass fraction is 1 ~ 4% in deionized water, add active material more wherein, acetylene black, binding agent mix to obtain mixed slurry, mixed slurry is cast on copper foil of affluxion body, compacting after dry, be cut into electrode slice by actual requirement, obtain Anode of lithium cell.
The present invention prepares in the raw material of Anode of lithium cell, and described active material and other binding agent are the conventional substances prepared Anode of lithium cell and adopt.Such as: described active material is: a, graphite material, graphite material comprises again the compound etc. that native graphite, coke, Delanium, carbon fiber or material with carbon element are formed; At least one in b, the compound that is made up of at least one element in Al, Si, Sn, Bi, Zn, Ge, Ti, Ag, Mg, In, Pb; Or at least one in the alloy to be formed by least one element and lithium in Al, Si, Sn, Bi, Zn, Ge, Ti, Ag, Mg, In, Pb; C, lithium nitride.Other described binding agent is: butadiene-styrene rubber, LA132/133/135 or sodium carboxymethylcellulose.
Embodiment 1
1) minus plate is prepared: cathode activity electrode (the such as LiFePO of mixing 95 % by weight
4), the binding agent Kynoar (PVDF) of 3 % by weight and the carbon conductor (such as acetylene black) of 2 % by weight, obtain mixture.Mixture is put into together with 1-METHYLPYRROLIDONE (NMP) and glass marble mixing to fill with, then mix more than 10h.With the preparing device of 200 microns or 250 micron pitch, obtained mixture is coated on the aluminium foil of 15 micron thickness uniformly, putting in vacuum drying oven to dry about 100 DEG C time allows NMP vapor away completely in about 12 hours, the electrode slice that compacting obtains, is cut into required predetermined size thus obtains the minus plate with 95 micron thickness.
2) prepare positive plate: respectively weigh 90 % by weight powdered graphite, conductive agent 4 % by weight acetylene black, as the carboxymethyl cellulose lithium of binding agent 3 % by weight and the butadiene-styrene rubber (SBR) of 3 % by weight.First, at non-iron ware with under stirring, be mixed with soluble in water for carboxymethyl cellulose lithium the carboxymethyl cellulose lithium solution that mass fraction is 1%, then powdered graphite before adding wherein, acetylene black, butadiene-styrene rubber mix.Distilled water and glass marble are added in mixing filling, then more than 10 hours are mixed, with the preparing device of 250 microns or 300 micron pitch, obtained mixture is coated on the Copper Foil of 12 micron thickness uniformly, putting in vacuum drying oven to dry about 90 DEG C time allows moisture vapor away completely in about 10 hours, the electrode slice that compacting obtains, is cut into required predetermined size thus obtains the positive plate with 120 micron thickness.
3) barrier film is prepared: by the polyethylene of 20 micron thickness or polypropylene porous septum (being used in Celgard, U.S.A) as barrier film.Porous septum is used for carrying out between positive plate and minus plate separately and can be wound into difformity being rolled into electrode assemblie, among the battery container putting into required not homomorphs, injects non-aqueous electrolytic solution and also carries out sealing formation lithium secondary battery.
4) electrolyte is prepared: the ethyl methyl carbonate (EMC) mixed with volume ratio 50 ︰ 30 ︰ 10 ︰ 10, ethylene carbonate, fluorobenzene (FB) and propylene carbonate (PC) have also dissolved 1.1MLiPF
6oRGANIC SOLVENT MIXTURES.And prepare example 2-4 according to this comprise carboxymethyl cellulose lithium in the anode as in the lithium battery of binding agent.
Embodiment 2
Difference from Example 1 is: carboxymethyl cellulose lithium salts as binding agent, raw material weigh respectively 92 % by weight powdered graphite, conductive agent 4 % by weight acetylene black, as the carboxymethyl cellulose lithium of binding agent 3 % by weight and the butadiene-styrene rubber of 1 % by weight.Other is identical with embodiment 1.
Embodiment 3
Difference from Example 1 is: carboxymethyl cellulose lithium salts is as binding agent, and raw material weighs powdered graphite, the acetylene black of conductive agent 4 % by weight, the carboxymethyl cellulose lithium as binding agent 3 % by weight of 93 % by weight respectively.Other is identical with embodiment 1.
Embodiment 4
Difference from Example 1 is: carboxymethyl cellulose lithium salts as binding agent, raw material weigh respectively 90 % by weight powdered graphite, conductive agent 4 % by weight acetylene black, as the carboxymethyl cellulose lithium of binding agent 5 % by weight and the butadiene-styrene rubber of 1 % by weight.Other is identical with embodiment 1.
Embodiment 5
Difference from Example 1 is: carboxymethyl cellulose lithium salts as binding agent, raw material weigh respectively 87 % by weight powdered graphite, conductive agent 4 % by weight acetylene black, as the carboxymethyl cellulose lithium of binding agent 8 % by weight and the butadiene-styrene rubber of 1 % by weight.Other is identical with embodiment 1.
Comparative example 1
Except carboxymethyl cellulose lithium (CMC-Li) binding agent using conventional sodium carboxymethylcellulose CMC-Na binding agent to replace in embodiment, all the other are used in mode identical described in embodiment 1 and provide electrode.
In order to detect binding agent carboxymethyl cellulose lithium described in lithium ion battery of the present invention and conventional CMC-Na Binder Properties, adopt conventional method of testing test cohesive force situation and membrane resistance after the electrode slice of the different binding agents that embodiment and comparative example obtain is colded pressing, and again cohesive force is tested to the pole piece after 60 DEG C of electrolyte soak 96 hours.And the levels suspension settlement solid content of anode slurry after 60 hours is tested, test result is in table 1.
The pole piece cohesive force of the different embodiment of table 1 and comparative example and resistance and anti-suspension situation
As can be seen from Table 1, adopt carboxymethyl cellulose lithium for the preparation of Anode of lithium cell, there is the cohesive force more excellent than comparative example, and pole piece resistance is little; And the cohesive force of pole piece after carrying out electrolyte immersion under the same conditions is obviously better than comparative example 1; And the anti-suspending power of carboxymethyl cellulose lithium can better prevent sedimentation, and the slurry solid content of levels does not have notable difference, and active material distribution is more even.
Meanwhile, the lithium battery assembled respectively embodiment 1 and comparative example 1 has carried out ac impedance spectroscopy (EIS) to be tested, and embodiment 1 impedance is starkly lower than comparative example 1, sees Fig. 1.
Further, lithium battery prepared by the present invention charges with 0.8 multiplying power through low temperature 10 DEG C, and 0.5 multiplying power discharging circulates after 20 times, and fully charged state takes battery apart, and anode pole piece does not separate out lithium; But under the same terms, use CMC-Na and SBR as the lithium battery prepared by anode binder in comparative example 1, occurred analysing lithium phenomenon.
The full battery of embodiment 1, embodiment 2, embodiment 3 and embodiment 4 preparation is charged with 0.7 multiplying power at 45 DEG C, 1 multiplying power discharging circulates after 700 times, battery capacity keeps still 88%, and comparative example 1 is 83%, improve 1% all unusual difficulty in such cases charge and discharge cycles 700 times, the present invention can improve about 5% than comparative example 1, and this is unexpected, there is unforeseeable technique effect, as shown in Figure 2.
Claims (10)
1. carboxymethyl cellulose lithium is preparing the purposes on Anode of lithium cell.
2. an Anode of lithium cell, is characterized in that: prepare using carboxymethyl cellulose lithium as binding agent.
3. Anode of lithium cell according to claim 2, is characterized in that: described binding agent also comprises other binding agent except carboxymethyl cellulose lithium.
4. the Anode of lithium cell according to Claims 2 or 3, is characterized in that: be prepared from by the raw material of following percentage by weight: active material 80 ~ 97%, acetylene black 1 ~ 4%, carboxymethyl cellulose lithium 0.5 ~ 10%, other binding agent 0 ~ 10%.
5. Anode of lithium cell according to claim 4, is characterized in that: be prepared from by the raw material of following percentage by weight: active material is 90 ~ 97%, acetylene black 1 ~ 3%, carboxymethyl cellulose lithium 1 ~ 5%, other binding agent 0 ~ 3%.
6. in Anode of lithium cell according to claim 3, it is characterized in that: other described binding agent is: butadiene-styrene rubber, LA132/133/135 or sodium carboxymethylcellulose.
7. in Anode of lithium cell according to claim 4, it is characterized in that: described active material is: graphite material, at least one in the compound be made up of at least one element in Al, Si, Sn, Bi, Zn, Ge, Ti, Ag, Mg, In, Pb, at least one in the alloy formed by least one element and lithium in Al, Si, Sn, Bi, Zn, Ge, Ti, Ag, Mg, In, Pb or lithium nitride.
8. in Anode of lithium cell according to claim 7, it is characterized in that: the compound that described graphite material is native graphite, coke, Delanium, carbon fiber or material with carbon element are formed.
9. the preparation method of the Anode of lithium cell described in any one of claim 2 ~ 8, it is characterized in that: carboxymethyl cellulose lithium is mixed with the carboxymethyl cellulose lithium solution that mass fraction is 1 ~ 4%, after adding active material, acetylene black, other binding agent more wherein, mixing obtains mixed slurry, mixed slurry is cast on copper foil of affluxion body, compacting after dry, be cut into electrode slice by actual requirement, obtain Anode of lithium cell.
10. the preparation method of Anode of lithium cell according to claim 9, is characterized in that: described drying for be dried to constant weight at 92 ~ 105 DEG C.
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| CN109309232A (en) * | 2018-09-13 | 2019-02-05 | 深圳市电科电源股份有限公司 | A kind of preparation method of lithium ion battery with high energy density |
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