CN105261737A - Preparation method of ternary cathode material - Google Patents
Preparation method of ternary cathode material Download PDFInfo
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- CN105261737A CN105261737A CN201510677601.0A CN201510677601A CN105261737A CN 105261737 A CN105261737 A CN 105261737A CN 201510677601 A CN201510677601 A CN 201510677601A CN 105261737 A CN105261737 A CN 105261737A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M4/36—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
-
- 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
- H01M4/36—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
-
- 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
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
- 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 ternary cathode material. The method comprises the following steps of 1, uniformly mixing and integrating a salt ingredient and an alkali ingredient in a solution mode to form a mixture solution; 2, carrying out deposition on the mixture solution formed in the step 1 to form precursor grains, and controlling core formation and a crystal growth speed of co-precipitation reaction through parameter adjustment; 3, adding positive ions in a liquid phase to the precursor grains for doping modification after carrying out washing and filter pressing on the precursor grains formed in the step 2, and drying the precursor grains; and 4, adding lithium to the dried raw material, and carrying out calcination and surface coating modification to obtain a finished product of the ternary material. By the method, the product manufactured according to the method has technical effects of high tap density, high capacity and high cycle performance.
Description
Technical field
The present invention relates to ternary material preparation field, particularly relate to a kind of preparation method of tertiary cathode material.
Background technology
Conventional cell positive material is cobalt acid lithium LiCoO
2, ternary material is then nickle cobalt lithium manganate Li(NiCoMn) and O
2, ternary composite cathode material presoma product is with nickel salt, cobalt salt, manganese salt for raw material, and the ratio of the inside nickel cobalt manganese can adjust LiFePO4 capacity according to actual needs and play on the low side, is not suitable for the requirement pursuing high-capacity cell for mobile telephone set.
In recent years, owing to having, voltage is high, specific energy density is high, price comparatively LiCoO for LiNi0.7Co0.15Mn0.15O2 ternary material
2the advantage such as cheap, is considered to LiCoO always
2best alternate material.But nickelic LiNi0.7Co0.15Mn0.15O2 tertiary cathode material of the prior art, there is the technical problem that tap density is lower, capacity is lower, cycle performance is lower in product.
Summary of the invention
The invention provides a kind of preparation method of tertiary cathode material, solve nickelic LiNi0.7Co0.15Mn0.15O2 tertiary cathode material of the prior art, there is the technical problem that tap density is lower, capacity is lower, cycle performance is lower in product, achieves the technique effect adopting the product of this method manufacture to have high-tap density, high power capacity, high cycle performance.
For solving the problems of the technologies described above, the embodiment of the present application provides a kind of preparation method of LiNi0.7Co0.15Mn0.15O2 tertiary cathode material, and described method comprises:
Step 1: salt batching, alkali batching are mixed by solution mode and merges formation mixed liquor;
Step 2: the mixed liquor of step 1 is carried out precipitation and form presoma crystal grain, by nucleation and the rate of crystalline growth of adjustment state modulator coprecipitation reaction;
Step 3: after presoma crystal grain washing and filter pressing step 2 formed, liquid phase is added cation-bit and carried out doping vario-property, then carries out drying process;
Step 4: dried raw material is added lithium, then carries out roasting, then carries out surface coating modification, obtains ternary material finished product.
Further, described parameter comprises: the concentration of salt-mixture, mixeding liquid temperature, feed rate, pH value, stir speed (S.S.).
Further, described step 2 adds coagulation agent in the process of precipitation.
Further, described mutually add cation-bit carry out doping vario-property be specially adopt inactive Mg
2+, Ti
4+ion doping.
Further, carry out surface coating modification described in be specially: pass through Zn
oand Al
2o
3carry out surface coating modification.
The one or more technical schemes provided in the embodiment of the present application, at least have following technique effect or advantage:
Achieve the technique effect adopting the product of this method manufacture to have high-tap density, high power capacity, high cycle performance.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of tertiary cathode material in the embodiment of the present application.
Embodiment
The invention provides a kind of preparation method of tertiary cathode material, solve nickelic LiNi0.7Co0.15Mn0.15O2 tertiary cathode material of the prior art, there is the technical problem that tap density is lower, capacity is lower, cycle performance is lower in product, achieves the technique effect adopting the product of this method manufacture to have high-tap density, high power capacity, high cycle performance.
In order to better understand technique scheme, below in conjunction with Figure of description and concrete execution mode, technique scheme is described in detail.
Below in conjunction with embodiment and accompanying drawing, to the detailed description further of the present invention's do, but embodiments of the present invention are not limited thereto.
Embodiment 1:
Please refer to Fig. 1, the application is on the basis of ternary material production existing 532, adopt the coprecipitation of independent research, mixed lithium and roasting synthesis technique, in liquid phase, carry out cation doping modification and material with carbon-coated surface technology produces nickelic LiNi0.7Co0.15Mn0.15O2 tertiary cathode material, product has the advantage of high-tap density, high power capacity, high cycle performance.
1, key technology and critical process
(1) coprecipitation technology prepares compact crystallization, and material particle size is moderate, and the nickel of narrow particle size distribution bores manganese ternary material precursor key technology;
(2) to carrying out cation doping modification preliminary treatment critical process after presoma washing and filter pressing;
(3) key technology of material structure and chemical property is controlled by adjustment product lithium content;
(4) surface coating modification improves transition metal ions stripping key technology.
2, concrete implementation content and technology path
The application adopts coprecipitation technology to prepare nickel and bores manganese ternary material precursor, by being reacted completely with controlling lithium content and adjusting suitable roasting system to precursor powder preliminary treatment, and the high-quality nickel brill manganese ternary material powder that component is homogeneous.
Concrete implementation content:
(1) the application adopts coprecipitation technology to prepare nickel and bores manganese ternary material precursor, by solution mode, various raw and auxiliary material and the corresponding auxiliary agent that adds are mixed, by nucleation and the rate of crystalline growth of the state modulator coprecipitation reaction such as concentration, mixeding liquid temperature, feed rate, pH value, stir speed (S.S.) of salt-mixture during adjustment co-precipitation.
The concentration of salt-mixture, mixeding liquid temperature, feed rate, pH value, stir speed (S.S.) all have obvious impact to the pattern of material and domain size distribution.This is because there are two balances in reaction system Ni2+-Co2+-Mn2+-NH4+-NH3-H2O: one is the complexation equilibrium of cation and NH3; One is cation and sedimentation equilibrium hydroxy.The factor such as concentration, temperature, pH of the salt of reaction system determines balanced sequence direction.Wherein pH value change has decisive action to balance.When pH value is lower, balances and move to complexing direction, the speed of growth of crystal grain is much larger than nucleation rate, and therefore crystallization is thick, and being reflected on particle diameter is exactly that the particle diameter of sample is large, but due to crystal growth too fast, material morphology is restive.Along with the increase of pH, balance and move to precipitation direction, M (OH) in reaction system
2degree of supersaturation increase, be conducive to the nucleation of crystal grain, the nucleation rate of crystal grain is much larger than the speed of growth, therefore crystal grain is difficult to grow up, and forms more granule, simultaneously due to the existence of too much OH-, occurring between granule reunites forms large aggregate, and particle size distribution range is broadened.When only having pH moderate, under the complexing of NH3, the speed of growth of crystal grain and nucleation rate are in more excellent state, and make crystal grain ordering growth, compact crystallization, material particle size is moderate, narrow particle size distribution.Therefore, the technological parameter by controlling coprecipitation reaction can obtain the precursor powder of needs.
On the other hand, owing to preparing the demand of high-tap density powder, in coprecipitation process, the appearance due to part gelatinous precipitate have impact on the tap density of powder.Therefore, add suitable coagulation agent, it is spherical that the network structure utilizing coagulation agent to be formed makes gelatinous precipitate be agglomerated into rapidly, and molecule is combined closely, and hydrone is extruded, and reaches coagulation effect.Because the molecule of coagulation agent is made up of linear molecule, when the amount once adding coagulation agent in sample is too many, because coagulation agent molecule itself can cohere reunion, so linear molecule can not launch completely, network structure can not be formed preferably, and during rapid stirring, the initial network structure formed can be destroyed, so coagulation effect is bad, thus make the tap density of sample not high.Therefore coagulation agent by a small amount of repeatedly and adjustment mixing speed, the linear molecule of coagulation agent can well launch completely, and also well can form network structure between molecule, makes the coagulation effect of coagulation agent best, improves the tap density of product.By effectively controlling presoma crystallite dimension, sphericity and the dispersed precursor powder obtaining high-tap density.
(2) the application adopts and adds cation-bit to liquid phase after presoma washing and filter pressing and carry out doping vario-property, improves the chemical property of material, ensure that powder is in the homogeneity of production process and stability simultaneously.First, inactive Mg is adopted
2+, Ti
4+plasma doping can prevent Ni
2+at Li
+during the discharge and recharge of position, ionic radius changes and causes material structure to cave in improving the stability of material main structure, and is conducive to the raising of material cyclical stability under high voltage, high magnification.Secondly, because the content of Co is lower, cause the electronic conductivity of material lower, therefore the high rate performance of material is poor, can improve the electronics of material and the diffusion rate of Li+, and then improve cycle performance, the high rate performance of material by the mode of doping.
(3) by adjustment product lithium content and in conjunction with sintering temperature system, the crystal structure controlling synthetic material reaches the object improving material electrochemical performance.Because lithium ion (0.076nm) is close with nickel ion (0.069nm) radius, under the condition meeting stoichiometric proportion, also there is the mixing of lithium ion and nickel ion, affect the chemical property of material.Cause material lithium to lack because lithium in the process of synthesizing in roasting exists part volatilization, make the Li being originally in 3a position
+by Ni
2+substitute.Needs due to charge balance cause more lithium room to produce, and cause the local collapse of material structure, affect the performance of material capacity.And lithium content is too high, the gap that lithium ion enters material structure in a large number causes oxonium ion to increase along the distortion of C axle, material is departed from telephony performance that layer structure also can affect material.Therefore, by control raw material join lithium amount to combine with suitable roasting system the mixing that reduces lithium ion and nickel ion with ensure that the layer structure stability of material is conducive to obtaining high performance product.
(4) the circulation cycle performance of material is improved by surface modification.Due to a series of side reactions that electrolyte and electrode surface occur, form surperficial SEI film at electrode surface, mainly comprise Li salt in SEI film, the bath deposition materials such as polymerizable compound.On the one hand because the formation of SEI film suppresses the continuation of electrolyte side reaction to occur to too increase Li simultaneously
+ion diffusivity; so it serves the effect of certain guard electrode material in electrochemical process; but for positive electrode, this electrode material surface SEI film unavoidably makes the irreversible capacity loss of material, efficiency for charge-discharge and cycle life are deteriorated.Especially in overcharge situation due to pyrolysis, SEI film will produce waste heat and fuel gas, thus have a strong impact on battery safety.Meanwhile, also easy in interface generation HF in charge and discharge cycles process, cause metal Co, the dissolving of Ni, Mn.Consequent accessory substance can make product very large in the increase of cyclic process middle impedance, worsens the chemical property of electrode material, causes material capacity to decay.Therefore Zn is passed through
oand Al
2o
3the method of carrying out surface coating modification can change the surface nature of active material to reduce the interfacial reaction of active material and electrolyte, impel and form excellent SEI film, lithium ion is allowed freely to embed and the dissolving of transition metal ions in suppression material while deviating from, then be expected to solve transition metal ions stripping phenomenon, the stability of material can be kept in high voltage cyclic process, thus improve the cycle life of product.
Technical scheme in above-mentioned the embodiment of the present application, at least has following technique effect or advantage:
Achieve the technique effect adopting the product of this method manufacture to have high-tap density, high power capacity, high cycle performance.
Although describe the preferred embodiments of the present invention, those skilled in the art once obtain the basic creative concept of cicada, then can make other change and amendment to these embodiments.So claims are intended to be interpreted as comprising preferred embodiment and falling into all changes and the amendment of the scope of the invention.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (5)
1. a preparation method for tertiary cathode material, is characterized in that, described method comprises:
Step 1: salt batching, alkali batching are mixed by solution mode and merges formation mixed liquor;
Step 2: the mixed liquor of step 1 is carried out precipitation and form presoma crystal grain, by nucleation and the rate of crystalline growth of adjustment state modulator coprecipitation reaction;
Step 3: after presoma crystal grain washing and filter pressing step 2 formed, liquid phase is added cation-bit and carried out doping vario-property, then carries out drying process;
Step 4: dried raw material is added lithium, then carries out roasting, then carries out surface coating modification, obtains ternary material finished product.
2. preparation method according to claim 1, is characterized in that, described parameter comprises: the concentration of salt-mixture, mixeding liquid temperature, feed rate, pH value, stir speed (S.S.).
3. preparation method according to claim 1, is characterized in that, described step 2 adds coagulation agent in the process of precipitation.
4. preparation method according to claim 1, is characterized in that, the described cation-bit of interpolation mutually carries out doping vario-property and is specially the inactive Mg of employing
2+, Ti
4+ion doping.
5. preparation method according to claim 1, is characterized in that, described in carry out surface coating modification and be specially: pass through Zn
oand Al
2o
3carry out surface coating modification.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107644997A (en) * | 2016-07-20 | 2018-01-30 | 三星环新（西安）动力电池有限公司 | A kind of positive electrode surface coating modification method based on sodium carboxymethylcellulose |
| CN109524662A (en) * | 2018-11-09 | 2019-03-26 | 浙江德升新能源科技有限公司 | A kind of preparation method of the good nickel-cobalt lithium manganate cathode material of crystallinity |
| CN110534694A (en) * | 2019-07-12 | 2019-12-03 | 乳源东阳光磁性材料有限公司 | A kind of ternary precursor production method of automatic blending method and its application |
| CN112378177A (en) * | 2020-10-20 | 2021-02-19 | 常州百利锂电智慧工厂有限公司 | Washing system, processing system and processing technology of lithium battery ternary material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103117380A (en) * | 2013-01-31 | 2013-05-22 | 中信大锰矿业有限责任公司 | Preparation method of manganese Li-NiCoMn ternary material for lithium ion battery |
| CN103825016A (en) * | 2014-02-13 | 2014-05-28 | 宁波金和新材料股份有限公司 | Nickelic cathode material rich in lithium and preparation method thereof |
-
2015
- 2015-10-20 CN CN201510677601.0A patent/CN105261737A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103117380A (en) * | 2013-01-31 | 2013-05-22 | 中信大锰矿业有限责任公司 | Preparation method of manganese Li-NiCoMn ternary material for lithium ion battery |
| CN103825016A (en) * | 2014-02-13 | 2014-05-28 | 宁波金和新材料股份有限公司 | Nickelic cathode material rich in lithium and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107644997A (en) * | 2016-07-20 | 2018-01-30 | 三星环新（西安）动力电池有限公司 | A kind of positive electrode surface coating modification method based on sodium carboxymethylcellulose |
| CN109524662A (en) * | 2018-11-09 | 2019-03-26 | 浙江德升新能源科技有限公司 | A kind of preparation method of the good nickel-cobalt lithium manganate cathode material of crystallinity |
| CN110534694A (en) * | 2019-07-12 | 2019-12-03 | 乳源东阳光磁性材料有限公司 | A kind of ternary precursor production method of automatic blending method and its application |
| CN110534694B (en) * | 2019-07-12 | 2021-10-01 | 乳源东阳光磁性材料有限公司 | Automatic batching method and ternary precursor production method applied by same |
| CN112378177A (en) * | 2020-10-20 | 2021-02-19 | 常州百利锂电智慧工厂有限公司 | Washing system, processing system and processing technology of lithium battery ternary material |
| CN112378177B (en) * | 2020-10-20 | 2022-05-13 | 常州百利锂电智慧工厂有限公司 | Processing system and processing technology suitable for lithium battery ternary material |
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Application publication date: 20160120 |