CN102956894A - Preparation method of lithium iron phosphate material anode sheet - Google Patents
Preparation method of lithium iron phosphate material anode sheet Download PDFInfo
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- CN102956894A CN102956894A CN2012104506206A CN201210450620A CN102956894A CN 102956894 A CN102956894 A CN 102956894A CN 2012104506206 A CN2012104506206 A CN 2012104506206A CN 201210450620 A CN201210450620 A CN 201210450620A CN 102956894 A CN102956894 A CN 102956894A
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Abstract
The invention relates to a coating method of a lithium iron phosphate material anode sheet, belonging to the technical field of preparation of a lithium ion battery. The invention aims to provide a preparation method of a superfine and nano lithium iron phosphate material anode sheet to improve an anode coating performance, improve a battery discharging performance and prolong the cycle life. The lithium iron phosphate material anode sheet prepared by the preparation method disclosed by the invention is coated uniformly; the surface of the lithium iron phosphate material anode sheet is smooth and has no grains; the surface density is obviously improved; and a discharging specific capacity of a prepared semi-battery under a 0.1 C multiplying power is more than 145 mAh/g and a discharging specific capacity under a 1C multiplying power is more than 135 mAh/g. According to the preparation method disclosed by the invention, the performance of a pole sheet can be improved through optimizing a slurry formula and adding an additive for increasing the bonding property; and the operation process is simple and the cost is low. The preparation method has the very great propelling effect on the actual application of superfine lithium iron phosphate and nano-scale lithium iron phosphate.
Description
Technical field
The invention belongs to the lithium ion battery preparing technical field, particularly a kind of preparation method of LiFePO 4 material positive plate.
Background technology
LiFePO 4 (LiFePO
4) battery be grew up in recent years a kind of, fail safe good, have extended cycle life, low-cost eco-friendly lithium ion battery.Various stand-by power supplies, electric tool and electric bicycle power supply have been widely used in, just in field Demonstration Application such as electric automobile, wind energy, solar energy and intelligent grids.
Yet as the ferric phosphate lithium cell of present commercial application, except the impact of LiFePO 4 material intrinsic performance on battery performance, battery preparation technique is also very large on the battery performance impact, especially the preparation technology of iron phosphate lithium positive pole sheet.In order to improve large multiplying power discharging property and the cryogenic property of battery, many researchers are devoted to LiFePO 4 material preparation technology's research, expectation improves the conductivity of LiFePO 4 material by the means such as fine, nanometer and carbon coating of LiFePO 4 material, with multiplying power discharging property and the low temperature properties of improving LiFePO 4 material.These researchs have obtained certain effect really, but new problem occurred, i.e. materials processing hydraulic performance decline, pole piece are difficult to coating, dry linting occurs, compacted density reduces, degradation problem under the battery specific energy.Simultaneously, cause the battery manufacture cost to increase, thereby also seriously restricted the large-scale production of ultra-fine and nano-scale lithium iron phosphate material and apply.Therefore, must solve the processing characteristics of ultra-fine and nano lithium iron phosphate material, especially be coated with problem.
Chinese patent 200610157460.0 improves Painting effect by processing the collector aluminium foil with alkaline solution; Patent 200810031763.7 is come the modification coating performance by the method for processing LiFePO 4 material with alkaline solution and add a small amount of alkaline matter in slurry; 200910213426.4 then be routine is prepared the LiFePO4 slurry all materials behind baking and ball milling under the inert atmosphere again solubilizer manufacture pole piece; Patent 200910311361.7 uses modified acacia as binding agent; 201010207504.2 the method that adopts the chemical corrosion collector and add organic conductive macromolecule; 201110253249.X adopt the different grain size LiFePO 4 material to prepare respectively the pole piece that slurry and gradation are coated with into double-layer structure; 201110403724.7 adopt three-dimensional foam structural metal original position to prepare the thinking novelty of integrated electrode; These methods have been improved the coating performance of LiFePO4 to a certain extent, but that some method may be not suitable for extensive preparation, some complicated process of preparation, some cost is higher.
Summary of the invention
The present invention is intended to seek a kind of preparation method that can increase pole piece adhesive property, simple, the lower-cost LiFePO 4 material positive plate of technique.It is characterized in that the method carries out according to the following steps:
(1) according to LiFePO4: conductive agent: the weight ratio of binding agent is weighing in 90: 5: 5 and prepares LiFePO4, conductive agent and binder material; Wherein, the particle size range of described LiFePO 4 material is 50nm～10 μ m; Use solvent to configure respectively binding agent reinforcing agent solution and binding agent PVDF solution;
(2) at first that the good conductive agent dry mixed of weighing is even, add again a certain amount of solvent, the weight ratio of conductive agent and solvent is 1: 2～1: 6, add the binding agent reinforcing agent solution that has prepared, mix, then add lithium iron phosphate positive material and mix, add at last the binder solution that has prepared and mix, and adjust to 45%～60% solids content with solvent;
(3) slurry that step (2) is prepared at room temperature blade coating on the aluminium foil of clean dried;
(4) the coated pole piece of step (3) is placed in the vacuum drying oven, baking obtains electrode slice at a certain temperature.
Wherein, conductive agent preferably uses one or more the mixture in the following material: acetylene black, electrically conductive graphite, CNT (carbon nano-tube), carbon nano-fiber, Graphene, polypyrrole, polythiophene; Binding agent is preferably Kynoar (PVDF); Solvent is preferably 1-METHYLPYRROLIDONE (NMP).
In order further to improve adhesive property, can also the conductive agent dry mixed of above-mentioned steps 2 evenly after, add after the caking property reinforcing agent mix, add again afterwards the stirring solvent mixing; The caking property reinforcing agent is selected from one or more the mixture in the following material: sorbitan fatty acid ester (SPAN), tetraethoxysilane, butyl silicate, tetrabutyl titanate, polyoxyethylene, polyacrylonitrile, polypropylene alkene nitrile and methyl acrylate copolymer also preferably add to be dissolved in the caking property reinforcing agent solution form that is made in the solvent; The consumption of caking property reinforcing agent is preferably 0.1～1wt% of LiFePO4, conductive agent and binding agent total weight.
In coating and baking procedure, the thickness of preferred aluminium foil is 20 μ m, and coating thickness is: single face 20～150 μ m (not comprising aluminum foil thickness); Bake out temperature is 80～120 ℃, and drying time is 6～12 hours.
Characteristic of the present invention is: do not change existing coating process, just charging sequence is changed, in addition, add the caking property reinforcing agent, preparation technology is simple to operate, and pole piece caking property is improved.Because the general specific surface of conductive agent is larger, tap density is low, when directly adding solvent, conductive agent can waft on the surface, difficult mixing, so the different conductive agent dry mixed with two or more are even first, add a small amount of solvent wet-mixed again, the so at first reasonable mixing of finishing conductive agent; In the conductive agent solution that mixes, add the caking property reinforcing agent solution for preparing in advance, then, adding in batches lithium iron phosphate positive material mixes, this process mainly is that positive electrode and conductive agent are fully mixed, the good continuous phase that forms positive electrode and conductive agent distributes, and adds a certain amount of solvent at this blend step according to the deployment conditions of positive electrode and adjusts; On the basis that conductive agent and positive electrode mix, the binder solution that adding has prepared is in this scattered continuous phase, further mix, make binding agent more even, touch positive electrode and conductive agent more fully, form the slurry mixed system of conductive agent, positive electrode and binding agent three class material fine dispersion.The adjusting of solid content is very important for varigrained positive electrode, so, in conductive agent scatter stage, LiFePO 4 of anode material scatter stage and binding agent scatter stage and last solid content adjustment, the addition of solvent all has difference with the difference of conductive agent kind, the difference of LiFePO 4 of anode material granularity and the difference of binding agent reinforcing agent, and solid content can be adjusted to 45%～60% and not wait.
Compare with traditional slurry preparation section, such as patent CN200710115518 elder generation's hybrid adhesive and solvent, join again conductive agent and mix, add at last LiFePO4.Because the conductive agent specific surface is large, directly in binding agent, disperse and may reunite, after LiFePO4 added, the dispersion of conductive agent and LiFePO4 also can be affected in the slurry.Patent CN200910191894 joins conductive agent in the solvent first, adds binding agent again, adds afterwards LiFePO4 again.When in being dispersed with the solvent of conductive agent, adding binding agent, because the solution solid content is very low, the binding agent molecule has larger suction-operated to the conductive agent molecule, binding agent may disperse inequality, conductive agent also can be gathered near the binding agent molecule in a large number, so the conductivity of this slurry system and caking property can descend.Patent CN201010253824 is first with LiFePO4, and conductive agent and a small amount of dispersant ground and mixed add binder solution afterwards again.This dispersion process is fairly simple, add dispersant favourable to the dispersion of positive electrode and conductive agent, but because conductive agent content is less, strengthen dispersed although this process has added dispersant, but may can be not clearly to the dispersion effect of conductive agent, if mixed effect may be better after both were disperseed separately.Solution and conductive agent that patent CN200910064193x will contain first dispersant mix, and add LiFePO4 again, add at last binding agent.This patent and the present invention have similar part, but the present invention has selected several different binding agent reinforcing agents, and this reinforcing agent plays good effect to dispersion and the caking property of slurry, and this also is the innovation of this patent.Patent CN200910306489 mixes part binding agent and water first, adds conductive agent and stirs, and adds LiFePO4 again, add at last remaining binding agent, and water is adjusted viscosity.This patent is used aqueous binders, and the present invention is different with it, in addition, the conductive agent adding is contained in the aqueous solution of a certain amount of binding agent, has equally similar patent CN200710115518 conductive agent to mix inhomogeneous problem.
The adding of caking property reinforcing agent of the present invention can be played following three aspects: effect: the surface property that 1) improves aluminium foil; 2) slurry is played peptizaiton; 3) strengthen adhesive property.The chemical property that adds as seen from Figure 3 the battery that pole piece is done of SPAN and tetrabutyl titanate is better than the not chemical property of additivated basic components, at room temperature 0.1C multiplying power discharging specific capacity is greater than 145mAh/g, 1C multiplying power discharging specific capacity is greater than 130mAh/g, and cyclicity is good.This preparation method is easy to large-scale continuous production.
Description of drawings
Fig. 1 is the stereoscan photograph of the iron phosphate lithium positive pole sheet that is coated with of embodiment one (not using the caking property reinforcing agent).
Fig. 2 is the stereoscan photograph of the iron phosphate lithium positive pole sheet that is coated with of embodiment two (use SPAN80 caking property reinforcing agent).
Fig. 3 is the discharge performance curve of the battery for preparing of embodiment one (not using the caking property reinforcing agent), embodiment two (use SPAN80 caking property reinforcing agent), embodiment five (using the prescription of tetrabutyl titanate caking property reinforcing agent) the institute pole piece that is coated with.(BASE: be embodiment one basic components; SPAN80: for embodiment two adds SPAN80; TZD: for embodiment five adds tetrabutyl titanate)
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further, following examples do not produce restriction to the present invention.
Embodiment one:
Prepare step ultra-fine and nano-scale lithium iron phosphate material positive plate as follows:
(1) according to mass ratio LiFePO4: acetylene black: electrically conductive graphite: PVDF=90: 2.5: 2.5: 5, accurately the good 90g particle mean size of weighing was approximately LiFePO4 positive electrode, 2.5g acetylene black, 2.5g electrically conductive graphite and the 5g PVDF of 2～3 μ m; 5g PVDF is mixed with the solution for later use of 45ml 10% with NMP.
(2) at first load weighted 2.5g acetylene black and 2.5g electrically conductive graphite are mixed the there-necked flask that the band of the sealing that places 250ml stirs in the glassware of drying, speed with 80 rev/mins stirs, add gradually 20ml NMP, continued dispersed with stirring 20 minutes, gradation adds the 90g LiFePO 4 material again, stirs 30 minutes, adds gradually 10% PVDF solution, add again 35ml NMP and make solid content be about 50%, stir and stopped in 30 minutes.
(3) the slurry blade coating that step (2) is prepared is on the aluminium foil of clean dried, and control single face coating thickness is at 50 μ m;
(4) the coated pole piece of step (3) is placed in the vacuum drying oven, baking is 8 hours under 120 ℃ of temperature.
(5) it is the disk of 8mm that the pole piece trimming that step (4) is prepared becomes diameter, take lithium as to electrode, prepares button cell in being full of the glove box of argon gas.
(6) button cell of step (5) preparation is tested at electrochemical test.Carry out charge-discharge test with constant current, charging/discharging voltage is 2.5-4.2V, under the room temperature, tests respectively the discharge performance under 0.1C, 0.2C, 0.5C and the 1C multiplying power.
Embodiment two:
Prepare step ultra-fine and nano-scale lithium iron phosphate material positive plate as follows:
(1) according to mass ratio LiFePO4: carbon nano-tube: electrically conductive graphite: PVDF=90: 0.2: 4.8: 5, accurately the good 90g granularity of weighing was approximately LiFePO4 positive electrode, 0.2g carbon nano-tube, 4.8g electrically conductive graphite and the 5g PVDF of 2～3 μ m; 5g PVDF is mixed with the solution for later use of 45ml 10% with NMP; With 5mlNMP 0.5g sorbitan fatty acid ester (SPAN80) is mixed with solution for later use in advance.
(2) at first load weighted 0.2g carbon nano-tube and 4.8g electrically conductive graphite are mixed the there-necked flask that the band of the sealing that places 250ml stirs in the glassware of drying, add the 25ml nmp solvent, speed with 80 rev/mins stirs, stir the nmp solution of the 5ml SPAN80 that adding (1) prepares after 20 minutes, continue to stir 20 minutes, add again 10ml NMP, dispersed with stirring 30 minutes, add gradually the 90g LiFePO 4 material, stirred 30 minutes, 10% the PVDF solution that adds that (1) prepare adds 37ml NMP again and makes solid content be about 45%, stirs to stop in 30 minutes.
(3) the slurry blade coating that step (2) is prepared is on the aluminium foil of clean dried, and control single face coating thickness is at 100 μ m;
(4) the coated pole piece of step (3) is placed in the vacuum drying oven, baking is 12 hours under 100 ℃ of temperature.
(5) it is the disk of 8mm that the pole piece trimming that step (4) is prepared becomes diameter, take lithium as to electrode, prepares button cell in being full of the glove box of argon gas.
(6) button cell of step (5) preparation is tested at electrochemical test.Carry out charge-discharge test with constant current, charging/discharging voltage is 2.5-4.2V, under the room temperature, tests respectively the discharge performance under 0.1C, 0.2C, 0.5C and the 1C multiplying power.
Embodiment three
Prepare step ultra-fine and nano-scale lithium iron phosphate material positive plate as follows:
(1) according to mass ratio LiFePO4: acetylene black: electrically conductive graphite: PVDF=90: 1.5: 3.5: 5, accurately the good 90g granularity of weighing was approximately LiFePO4 positive electrode, 1.5g acetylene black, 3.5g electrically conductive graphite and the 5g PVDF of 100nm～200nm; 5g PVDF is mixed with the solution for later use of 45ml 10% with NMP; With the 10ml dimethyl formamide 0.1g polyacrylonitrile is mixed with solution for later use in advance.
(2) at first load weighted 1.5g acetylene black and 3.5g electrically conductive graphite are mixed the there-necked flask that the band of the sealing that places 250ml stirs in the glassware of drying, add the 10ml nmp solvent, speed with 80 rev/mins stirs, stir the dimethyl formamide solution that adds the 10ml polyacrylonitrile after 20 minutes, continue to stir 20 minutes, add again 10ml NMP, dispersed with stirring 30 minutes, add gradually the 90g LiFePO 4 material, stirred 30 minutes, the PVDF solution of adding 35ml 10% makes solid content be about 60%, stirs to stop in 30 minutes.
(3) the slurry blade coating that step (2) is prepared is on the aluminium foil of clean dried, and control single face coating thickness is at 150 μ m;
(4) the coated pole piece of step (3) is placed in the vacuum drying oven, baking is 12 hours under 120 ℃ of temperature.
(5) it is the disk of 8mm that the pole piece trimming that step (4) is prepared becomes diameter, take lithium as to electrode, prepares button cell in being full of the glove box of argon gas.
(6) button cell of step (5) preparation is tested at electrochemical test.Carry out charge-discharge test with constant current, charging/discharging voltage is 2.5-4.2V, under the room temperature, tests respectively the discharge performance under 0.1C, 0.2C, 0.5C and the 1C multiplying power.
Embodiment four
Prepare step ultra-fine and nano-scale lithium iron phosphate material positive plate as follows:
(1) according to mass ratio LiFePO4: polypyrrole: electrically conductive graphite: PVDF=90: 2.0: 3.0: 5, accurately the good 90g granularity of weighing was approximately LiFePO4 positive electrode, 2.0g polypyrrole, 3.0g electrically conductive graphite and the 5g PVDF of 5～6um; 5g PVDF is mixed with the solution for later use of 45ml 10% with NMP; With 10mlNMP the tetraethoxysilane of 0.1g is mixed with solution for later use in advance.
(2) at first load weighted 2.0g polypyrrole and 3.0g electrically conductive graphite are mixed the there-necked flask that the band of the sealing that places 250ml stirs in the glassware of drying, add the 15ml nmp solvent, speed with 80 rev/mins stirs, stir the nmp solution that adds the 10ml tetraethoxysilane after 20 minutes, continue to stir 20 minutes, add again 20ml NMP, dispersed with stirring 30 minutes, add gradually the 90g LiFePO 4 material, stirred 30 minutes, the PVDF solution of adding 45ml 10% adds 2ml NMP again and makes solid content be about 52%, stirs to stop in 30 minutes.
(3) the slurry blade coating that step (2) is prepared is on the aluminium foil of clean dried, and control single face coating thickness is at 20 μ m;
(4) the coated pole piece of step (3) is placed in the vacuum drying oven, baking is 10 hours under 80 ℃ of temperature.
(5) it is the disk of 2cm that the pole piece trimming that step (4) is prepared becomes diameter, take lithium as to electrode, prepares button cell in being full of the glove box of argon gas.
(6) button cell of step (5) preparation is tested at electrochemical test.Carry out charge-discharge test with constant current, charging/discharging voltage is 2.5-4.2V, under the room temperature, tests respectively the discharge performance under 0.1C, 0.2C, 0.5C and the 1C multiplying power.
Embodiment five
Prepare step ultra-fine and nano-scale lithium iron phosphate material positive plate as follows:
(1) according to mass ratio LiFePO4: acetylene black: polythiophene: PVDF=90: 3.5: 1.5: 5, accurately the good 90g granularity of weighing was approximately LiFePO4 positive electrode, 3.5g acetylene black, 1.5g polythiophene and the 5g PVDF of 2～3 μ m; 5g PVDF is mixed with the solution for later use of 45ml 10% with NMP; With 10ml NMP the 1g tetrabutyl titanate is mixed with solution for later use in advance.
(2) at first load weighted 3.5g acetylene black and 1.5g polythiophene are mixed the there-necked flask that the band of the sealing that places 250ml stirs in the glassware of drying, add the 30ml nmp solvent, speed with 80 rev/mins stirs, stir the nmp solution that adds the 10ml tetrabutyl titanate after 20 minutes, continue to stir 20 minutes, add again 10ml NMP, dispersed with stirring 30 minutes, add gradually the 90g LiFePO 4 material, stirred 30 minutes, the PVDF solution of adding 10% adds 13ml NMP again and makes solid content be about 48%, stirs to stop in 30 minutes.
(3) the slurry blade coating that step (2) is prepared is on the aluminium foil of clean dried, and control single face coating thickness is at 60 μ m;
(4) the coated pole piece of step (3) is placed in the vacuum drying oven, baking is 10 hours under 100 ℃ of temperature.
(5) it is the disk of 8mm that the pole piece trimming that step (4) is prepared becomes diameter, take lithium as to electrode, prepares button cell in being full of the glove box of argon gas.
(6) button cell of step (5) preparation is tested at electrochemical test.Carry out charge-discharge test with constant current, charging/discharging voltage is 2.5-4.2V, under the room temperature, tests respectively the discharge performance under 0.1C, 0.2C, 0.5C and the 1C multiplying power.
Claims (9)
1. a lithium ion battery is with the preparation method of iron phosphate lithium positive pole sheet, it is characterized in that the method carries out according to the following steps:
(1) according to LiFePO4: conductive agent: the weight ratio of binding agent is weighing in 90: 5: 5 and prepares LiFePO4, conductive agent and binder material; Wherein, the particle size range of described LiFePO 4 material is 50nm～10 μ m; Use solvent to configure respectively binding agent reinforcing agent solution and binding agent PVDF solution;
(2) at first that the good conductive agent dry mixed of weighing is even, add again a certain amount of solvent, the weight ratio of conductive agent and solvent is 1: 2～1: 6, add the binding agent reinforcing agent solution that has prepared, mix, then add lithium iron phosphate positive material and mix, add at last the binder solution that has prepared and mix, and adjust to 45%～60% solids content with solvent;
(3) slurry that step (2) is prepared at room temperature blade coating on the aluminium foil of clean dried;
(4) the coated pole piece of step (3) is placed in the vacuum drying oven, baking obtains electrode slice at a certain temperature.
2. the preparation method of a kind of lithium-ion battery lithium iron phosphate positive plate according to claim 1 is characterized in that described conductive agent is selected from one or more the mixture in the following material: acetylene black, electrically conductive graphite, CNT (carbon nano-tube), carbon nano-fiber, Graphene, polypyrrole, polythiophene.
3. a kind of lithium ion battery according to claim 1 is characterized in that with the preparation method of iron phosphate lithium positive pole sheet described binding agent is Kynoar (PVDF).
4. a kind of lithium ion battery according to claim 1 is with preparation method ultra-fine and the nano-grade lithium iron phosphate positive plate, it is characterized in that the conductive agent dry mixed of described step 2 evenly after, after adding caking property reinforcing agent mixes, add again afterwards stirring solvent and mix; Described caking property reinforcing agent is selected from one or more the mixture in the following material: sorbitan fatty acid ester (SPAN), tetraethoxysilane, butyl silicate, tetrabutyl titanate, polyoxyethylene, polyacrylonitrile, polypropylene alkene nitrile and methyl acrylate copolymer; Described caking property reinforcing agent adds to be dissolved in the caking property reinforcing agent solution form that is made in the solvent.
5. a kind of lithium ion battery according to claim 1 is characterized in that with the preparation method of iron phosphate lithium positive pole sheet described solvent is 1-METHYLPYRROLIDONE (NMP).
6. a kind of lithium ion battery according to claim 4 is with the preparation method of iron phosphate lithium positive pole sheet, and the consumption that it is characterized in that described caking property reinforcing agent is 0.1～1wt% of LiFePO4, conductive agent and binding agent total weight.
7. a kind of lithium ion battery according to claim 1 is characterized in that with the preparation method of iron phosphate lithium positive pole sheet described aluminum foil thickness is 20 μ m, and coating thickness is: single face 20～150 μ m (not comprising aluminum foil thickness).
8. a kind of lithium ion battery according to claim 1 is characterized in that with the preparation method of iron phosphate lithium positive pole sheet described pole piece bake out temperature is 80～120 ℃, and drying time is 6～12 hours.
9. the preparation method of a battery is characterized in that pole piece trimming being of a size of the disk of diameter 8mm, as the positive pole of button cell according to appointing the described preparation method of * claim to prepare electrode slice among the claim 1-8.
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