CN104795562A - Preparation method of modified ternary cathode material - Google Patents
Preparation method of modified ternary cathode material Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- 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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- 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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a high-capacity modified ternary cathode material. The cathode material is formed by coating the surface of a ternary cathode with a nickel-plating layer. The preparation method comprises the steps of sequentially carrying out sensitization, activation and reduction treatment on the ternary cathode material in the existence of a dispersing agent, and plating the nickel-plating layer; carrying out thermal treatment on the ternary cathode material with the nickel-plating layer, and thus obtaining the nickel-coated modified ternary cathode material. The preparation method is simple to operate, moderate in process condition and low in cost; the prepared nickel-coated modified ternary cathode material is uniform in the coating of nickel-plating layer, stable in structure and capable of being used for preparing a lithium ion battery which is good in conductivity, high in specific capacity and high in power density.
Description
Technical field
The present invention relates to a kind of preparation method of modification tertiary cathode material, belong to field of lithium ion battery anode.
Background technology
Since nineteen ninety Sony corporation of Japan take the lead in succeeding in developing lithium ion battery and by its commercialization since, lithium ion battery obtains fast development.Nowadays lithium ion battery has been widely used in civilian and military every field.Along with the continuous progress of science and technology, the performance of people to battery proposes more higher requirements: the miniaturization of electronic equipment and individualized development, and the specific energy needing battery to have less volume and Geng Gao exports; Aero-Space energy requirements battery has cycle life, the security performance of better low temperature charge-discharge performance and Geng Gao; Electric automobile needs the battery of Large Copacity, low cost, high stability and security performance.
Along with the problem of environmental pollution using fossil energy to cause is day by day serious, green, free of contamination New Energy Industry more and more causes the attention of people.As one of the representative of New Energy Industry, lithium ion battery industry was obtaining swift and violent development in recent years.Energy density is high, operating voltage is high owing to having for lithium ion battery, have extended cycle life, memory-less effect and advantages of environment protection, has been widely used in the portable electric appts such as mobile phone, notebook computer, digital camera and electric automobile.In the composition of lithium ion battery, positive electrode is the key factor determining its chemical property, security performance and future thrust.So developing lithium-ion battery system of future generation and material becomes one of field that academia and industrial circle pay close attention to the most, and wherein, the exploitation of high specific energy positive electrode is undoubtedly the most important thing.
Positive electrode is one of the most key factor of the performance such as energy density, specific energy, life-span affecting lithium ion battery.In existing positive electrode, Layered Structural Positive Electrode Materials is still main flow.The electrochemical stability of first generation stratified material LiCoO2 is good, and cycle performance is excellent, but capacity is only 50% of its theoretical capacity, and there is the significant problem such as resource and fail safe; LiNiO2 specific capacity is the highest, but synthesis difficulty, and there is larger potential safety hazard; LiMnO2 good thermal stability and low price, but the obvious phase transformation in charge and discharge process causes its cyclical stability very poor.Polynary layered cathode material, as LiCo1/3Ni1/3Mn1/3 O2, LiNi0.8Al0.2O2, combine the advantage of existing layer structure material, reach the specific energy of 160 mAg/g, but high Co, Ni content in material still exists the problem such as cost, resource, fail safe, be also the shortcoming that this material is fatal.The LiMn2O44 of spinel-type, because high security, cheapness and the parent that is subject to electrokinetic cell hides, obtained business-like application, but relatively low specific energy or specific power becomes this two shortcomings that material is the most fatal, hinders the application of these two materials.
The reaction good reversibility of tertiary cathode material, large current discharging capability is strong, there are good cyclical stability and security performance, and when charging/discharging voltage scope is suitably widened, specific capacity can be promoted to more than 200mAh/g and there will not be the safety problem because overcharge causes or structural instability phenomenon, be considered to the positive electrode most possibly replacing LiCoO2, its commercialization has larger development space.
At present, also there is the shortcoming of high temperature cyclic performance difference in tertiary cathode material.Active material material and electrolyte contacts, under the high temperature conditions, can by corrosion such as HF, destroy interfacial structure, and then cause W metal, Co, Al dissolving in the electrolytic solution, causes the decay of capacity.
Summary of the invention
Based on this, be necessary to provide a kind of modification ternary material that can improve cycle performance of lithium ion battery and preparation method thereof.The object of the invention is to be to provide a kind of nickel coating evenly coated, Stability Analysis of Structures, can be used for the modification tertiary cathode material preparing good conductivity, specific capacity is high, power density is large lithium ion battery.
The preparation method of nickel coated modification tertiary cathode material of the present invention comprises following concrete steps:
One, tertiary cathode material is placed in second alcohol and water by volume 1:2 ~ 3:1 composition mixed solvent, take mechanical agitation, mixing speed is 50 ~ 500 revs/min, temperature is 15 ~ 40 DEG C, be wash 1 ~ 30min under the ultrasonic wave added of 20 ~ 40kHz in frequency, centrifugation, water washing is for several times;
Two, gained tertiary cathode material is placed in the hydrochloric acid solution that temperature is the sub-tin of chloride containing of 15 ~ 40 DEG C, take mechanical agitation, stir 1 ~ 10min, centrifugation with the speed of 50 ~ 500 revs/min, water washing for several times again; The hydrochloric acid solution of the sub-tin of described chloride containing is composed of the following components: stannous chloride 2 ~ 8g/L, concentrated hydrochloric acid 2 ~ 6mL/L, dispersant 0.2 ~ 2mL/L, and solvent is water;
Three, then the tertiary cathode material after process is placed in the hydrochloric acid solution that temperature is the chloride containing palladium of 15 ~ 40 DEG C, takes mechanical agitation, stir carry out activation processing 1 ~ 10min, centrifugation with the speed of 50 ~ 500 revs/min, water washing for several times; The hydrochloric acid solution of described chloride containing palladium is composed of the following components: palladium bichloride 0.1 ~ 1g/L, concentrated hydrochloric acid 4 ~ 10mL/L, dispersant 0.2 ~ 2mL/L, and solvent is water;
Four, the tertiary cathode material after step 3 activation processing is placed in the ortho phosphorous acid sodium solution that temperature is 15 ~ 40 DEG C, takes mechanical agitation, stirs carry out reduction treatment 0.5 ~ 5min, centrifugation with the speed of 50 ~ 500 revs/min; Described ortho phosphorous acid sodium solution is composed of the following components: inferior sodium phosphate 1 ~ 5wt%, dispersant 0.2 ~ 2mL/L, and solvent is water;
Five, the tertiary cathode material after step 4 reduction treatment is placed in the plating solution that pH is 8 ~ 8.5, under 70 ~ 90 DEG C of temperature conditions, take mechanical agitation, stir with the speed of 50 ~ 500 revs/min and carry out chemical nickel plating 0.5 ~ 10min, centrifugation, water washing is for several times; Described plating solution is composed of the following components: nickelous sulfate 20 ~ 60g/L, inferior sodium phosphate 15 ~ 30g/L, natrium citricum 30 ~ 60g/L, ammonium chloride 30 ~ 70g/L, dispersant 0.2 ~ 2mL/L, and solvent is water;
Six, under the tertiary cathode material in step 5 after chemical nickel plating is placed in the temperature environment of 100 ~ 200 DEG C, is incubated 1 ~ 4 hour, obtains nickel coated modification tertiary cathode material.
Nickel coated of the present invention nickel coated of the present invention modification tertiary cathode material also comprises following preferred version: in preferred nickel coated modification tertiary cathode material, nickel coating thickness is 0.1 ~ 1.0 μm.
In preferred nickel coated modification tertiary cathode material, nickel coating is the nickel-phosphorus alloy of phosphorus mass percentage < 8%.
In preferred nickel coated modification tertiary cathode material, the ternary granulated average grain diameter D50 of modification is distributed between 5 ~ 30 μm.
The preparation method of nickel coated modification tertiary cathode material of the present invention, by after ternary granulated for modification employing alcohol water mixed solvent washing, carry out sensitization, activation and reduction pretreatment successively, ternary granulated being dispersed under dispersant effect in the mixing plating solution of sulfur acid nickel, inferior sodium phosphate, natrium citricum and ammonium chloride of pretreated modification carries out chemical nickel plating coating; Heat-treat ternary granulated for the modification of plating nickel coating again, to obtain final product.
Beneficial effect of the present invention: it is good that the present invention adopts nickel coated modification ternary to obtain a kind of conductivity performance first, constitutionally stable nickel coated modification tertiary cathode material, can be used for the lithium ion battery preparing height ratio capacity and high power density.The advantage that technical solution of the present invention is outstanding is:
1, the present invention is to the coated nickel of modification ternary powder particle surface, can improve the conductivity of positive electrode on the one hand, be beneficial to electron transmission, fast reaction speed, effectively improves the discharge power of lithium ion battery; On the other hand can the amphipathic property of reinforcing material, be conducive to material surface solution and exchange and ion transport, reduce electrode polarization, promote cell discharge voltage platform, improve cell power conversion efficiency;
2, nickel coated modification ternary powder particle material conductivity obtained after the present invention adopts nickel coated modification ternary improves greatly, when making lithium ion cell electrode, can reduce and uses or do not use carbonaceous conductive agent;
3, preparation method of the present invention, all use dispersant in whole preparation technology, can be effectively dispersed in solution by ternary granulated for modification, more be conducive to sensitization, activation, reduction and nickel process, so that it is evenly coated to obtain coating, constitutionally stable nickel coated modification tertiary cathode material;
4, preparation technology of the present invention is simple to operate, and process conditions are gentle, and production cost is low, meets suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, preferably embodiment of the present invention is described in further detail:
Embodiment 1
Get tertiary cathode material 5g, be 8.53 μm, carry out chemical nickel plating process sized by average grain diameter D50, the technique of chemical nickel plating is:
1, above-mentioned tertiary cathode material is added alcohol and water volume ratio is 1:1, cumulative volume is in the alcohol water blend of 1L.Temperature is 25 DEG C, mixing speed 200 rpms, ultrasonic oscillation, and concussion frequency 30kHz, the time is 5min.
By tertiary cathode material centrifugation, and with deionized water rinsing repeatedly.
2, the tertiary cathode material after cleaning being added composition is stannous chloride (SnCl22H2O) 4g/L, 37%HCl 4mL/L, OP-101mL/L, and solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed 200 rpms, and the time is 2min.By tertiary cathode material centrifugation, and be 7 with deionized water rinsing to pH.
3, the tertiary cathode material after sensitization being added composition is palladium bichloride (PdCl2) 0.4g/L, 37%HCl 8mL/L, OP-101mL/L, and solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed 200 rpms, and the time is 2min.By tertiary cathode material centrifugation, and be 7 with deionized water rinsing to pH.
4, the tertiary cathode material after activation being added composition is inferior sodium phosphate (NaH2PO2H2O) 3% mass fraction, and OP-101mL/L, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed 200 rpms, and the time is 1min.By tertiary cathode material centrifugation.
5, the modification ternary after reduction being added composition is nickelous sulfate (NiSO46H2O) 35g/L, inferior sodium phosphate (NaH2PO2H2O) 20g/L, natrium citricum (C6H5Na3O72H2O) 45g/L, ammonium chloride (NH4Cl) 50g/L, surfactant 1mL/L, solvent is deionized water, and volume is in the solution of 1L.Be adjusted to pH 8 ~ 8.5 with ammoniacal liquor or citric acid, temperature is 85 DEG C, mixing speed 200 rpms, and the time is 3min.
6, the modification ternary after chemical nickel plating is put into the baking oven of 150 DEG C, be incubated 2 hours.
Embodiment 2
Get tertiary cathode material 20g, average grain diameter D50 size is 13.72 μm, carries out chemical nickel plating process, and the technique of chemical nickel plating is:
1, above-mentioned tertiary cathode material is added alcohol and water volume ratio is 1:2, cumulative volume is in the alcohol water blend of 1L.Temperature is 25 DEG C, mixing speed 200 rpms, ultrasonic oscillation, and concussion frequency 35kHz, the time is 8min.By ternary centrifugation, and with deionized water rinsing repeatedly.
2, the tertiary cathode material after cleaning being added composition is stannous chloride (SnCl22H2O) 7g/L, 37%HCl 5mL/L, and sucrose ester and each 0.5mL/L of OP-10, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed 400 rpms, and the time is 2min.By tertiary cathode material centrifugation, and be 7 with deionized water rinsing to pH.
3, tertiary cathode material being added composition is palladium bichloride (PdCl2) 0.8g/L, 37 %HCl 4mL/L, sucrose ester and each 0.5mL/L of OP-10, and solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed 200 rpms, and the time is 2min.By tertiary cathode material centrifugation, and be 7 with deionized water rinsing to pH.
4, the modification ternary after activation being added composition is inferior sodium phosphate (NaH2PO2H2O) 4 % mass fraction, and sucrose ester and each 0.5mL/L of OP-10, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed 200 rpms, and the time is 1min.By ternary material centrifugation.
5, the tertiary cathode material after reduction being added composition is nickelous sulfate (NiSO46H2O) 50g/L, inferior sodium phosphate (NaH2PO2H2O) 25g/L, natrium citricum (C6H5Na3O72H2O) 30g/L, ammonium chloride (NH4Cl) 60g/L, sucrose ester and each 0.5mL/L of OP-10, solvent is deionized water, and volume is in the solution of 1L.Be adjusted to pH 8 ~ 8.5 with ammoniacal liquor or citric acid, temperature is 80 DEG C, mixing speed 200 rpms, and the time is 3min.
6, the modification ternary after chemical nickel plating is put into the baking oven of 200 DEG C, be incubated 1 hour.
Performance measurement
For the performance of positive electrode prepared by inspection the inventive method, test by half-cell method of testing, with above embodiment 1 and embodiment 2 and the tertiary cathode pole material without nickel coated: acetylene black: PVDF(Kynoar)=93:3:4(weight ratio), add appropriate NMP(N-methyl pyrrolidone) furnishing pulpous state, coat on aluminium foil, within 8 hours, make positive plate through vacuum 110 DEG C of dryings; Be to electrode with metal lithium sheet, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1:1:1, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 0 ~ 2.0V, and charge-discharge velocity is 0.2C, and carry out testing to battery performance, test result sees the following form.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (5)
1. a preparation method for high power capacity modification tertiary cathode material, specifically comprises the following steps:
One, tertiary cathode material is placed in second alcohol and water by volume 1:2 ~ 3:1 composition mixed solvent, take mechanical agitation, mixing speed is 50 ~ 500 revs/min, temperature is 15 ~ 40 DEG C, be wash 1 ~ 30min under the ultrasonic wave added of 20 ~ 40kHz in frequency, centrifugation, water washing is for several times;
Two, gained tertiary cathode material in step one is placed in the hydrochloric acid solution that temperature is the sub-tin of chloride containing of 15 ~ 40 DEG C, take mechanical agitation, stir 1 ~ 10min, centrifugation with the speed of 50 ~ 500 revs/min, water washing for several times again;
Three, then the tertiary cathode material after process in step 2 is placed in the hydrochloric acid solution that temperature is the chloride containing palladium of 15 ~ 40 DEG C, take mechanical agitation, stir with the speed of 50 ~ 500 revs/min and carry out activation processing 1 ~ 10min, centrifugation, water washing for several times;
Four, the tertiary cathode material after step 3 activation processing is placed in the ortho phosphorous acid sodium solution that temperature is 15 ~ 40 DEG C, takes mechanical agitation, stir with the speed of 50 ~ 500 revs/min and carry out reduction treatment 0.5 ~ 5min, centrifugation;
Five, again the tertiary cathode material after step 4 reduction treatment is placed in the plating solution that pH is 8 ~ 8.5, under 70 ~ 90 DEG C of temperature conditions, take mechanical agitation, stir with the speed of 50 ~ 500 revs/min and carry out chemical nickel plating 0.5 ~ 10min, centrifugation, water washing is for several times;
Six, under finally the tertiary cathode material after chemical nickel plating in step 5 being placed in the temperature environment of 100 ~ 200 DEG C, being incubated 1 ~ 4 hour, obtaining nickel coated modification tertiary cathode material.
2. the preparation method of a high power capacity modification tertiary cathode material, it is characterized in that: the hydrochloric acid solution of the sub-tin of the chloride containing described in claim 1 step 2 is composed of the following components: stannous chloride 2 ~ 8g/L, concentrated hydrochloric acid 2 ~ 6mL/L, dispersant 0.2 ~ 2mL/L, solvent is water.
3. the preparation method of a high power capacity modification tertiary cathode material, it is characterized in that: the hydrochloric acid solution of the chloride containing palladium described in claim 1 step 3 is composed of the following components: palladium bichloride 0.1 ~ 1g/L, concentrated hydrochloric acid 4 ~ 10mL/L, dispersant 0.2 ~ 2mL/L, solvent is water.
4. a preparation method for high power capacity modification tertiary cathode material, is characterized in that: the ortho phosphorous acid sodium solution described in claim 1 step 4 is composed of the following components: inferior sodium phosphate 1 ~ 5wt%, dispersant 0.2 ~ 2mL/L, and solvent is water.
5. the preparation method of a high power capacity modification tertiary cathode material, it is characterized in that: the plating solution described in claim 1 step 5 is composed of the following components: nickelous sulfate 20 ~ 60g/L, inferior sodium phosphate 15 ~ 30g/L, natrium citricum 30 ~ 60g/L, ammonium chloride 30 ~ 70g/L, dispersant 0.2 ~ 2mL/L, solvent is water.
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| CN109860590A (en) * | 2018-11-15 | 2019-06-07 | 广东邦普循环科技有限公司 | A kind of preparation method and application of 55 type nickel-cobalt lithium manganate material of nickel |
| CN111868975A (en) * | 2018-03-20 | 2020-10-30 | 株式会社田中化学研究所 | Compound for positive electrode |
| CN112599735A (en) * | 2020-12-11 | 2021-04-02 | 合肥国轩高科动力能源有限公司 | Modified NCM622 ternary cathode material and preparation method thereof |
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| CN104538604A (en) * | 2015-01-20 | 2015-04-22 | 河北工业大学 | Surface modifying method for lithium nickel manganese oxide positive electrode material |
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| CN1417875A (en) * | 2002-12-06 | 2003-05-14 | 北京理工大学 | Acive material for cell electrode and electrode plate surface modifying techuology |
| CN102747344A (en) * | 2011-12-08 | 2012-10-24 | 广西师范大学 | Chemical nickel plating solution and preparation method thereof, method for carrying out nickel plating on nano-LiFePO4/C composite material by using chemical nickel plating solution, and resulting product thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111868975A (en) * | 2018-03-20 | 2020-10-30 | 株式会社田中化学研究所 | Compound for positive electrode |
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| CN112599735A (en) * | 2020-12-11 | 2021-04-02 | 合肥国轩高科动力能源有限公司 | Modified NCM622 ternary cathode material and preparation method thereof |
| CN112599735B (en) * | 2020-12-11 | 2022-02-18 | 合肥国轩高科动力能源有限公司 | Modified NCM622 ternary cathode material and preparation method thereof |
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Application publication date: 20150722 |