CN106252652A - The preparation method of a kind of positive electrode active materials, positive plate and lithium ion battery - Google Patents
The preparation method of a kind of positive electrode active materials, positive plate and lithium ion battery Download PDFInfo
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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
- H01M4/52—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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- 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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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Abstract
For overcoming the problem that in prior art, lithium ion cell positive energy density is low, the invention provides the preparation method of a kind of positive electrode active materials, it is characterised in that comprise the steps: that S1, acquisition molecular formula are Na3[CoMo6O24H6] precursor material, the mean diameter of described precursor material is more than 10 μm；S2, described precursor material is dissolved in the water, adds water soluble alcohols organic solvent under agitation, carry out recrystallization, after filtration, obtain described positive electrode active materials；Described water soluble alcohols organic solvent is 1 5:1 with the volume ratio of water.Meanwhile, the invention also discloses positive plate and the lithium ion battery of positive electrode active materials containing being prepared by said method.The positive electrode active materials mean particle size that the method that the present invention provides prepares is little, and effective gram volume is high, is beneficial to improve the energy density of lithium ion battery.
Description
Technical field
The present invention relates to field of lithium ion secondary, particularly relate to the preparation method of a kind of positive electrode active materials, positive plate and lithium ion battery.
Background technology
In current daily life, lithium rechargeable battery has been widely used in mobile phone, notebook computer and other digital products, is indispensable energy storage device.At present, the positive electrode being applied to lithium ion battery mainly uses lithium ion to insert embedding transition metal stratiform oxide, such as LiCoO2、LiMn2O4Deng.The charge and discharge process of such material depends on lithium ion inserting in order and deintercalation in its lattice structure, and the capacity of these materials and cyclical stability are mainly determined by the stability of its crystal structure.In charge and discharge process, once crystal structure is destroyed or loses restorability, and the capacity of battery will decay and cycle performance deterioration.
It addition, these traditional lithium ions insert embedding positive electrode mostly can only carry out one electron redox reaction in charge and discharge process, its obtainable specific capacity is caused to be usually less than 200mAhg-1So that the energy density of lithium ion battery is relatively low.Be currently based on these tradition positive electrodes lithium ion battery to those higher applications of energy density demand, such as hybrid electric vehicle, pure electric vehicle etc., show weak point.
Summary of the invention
The technical problem to be solved is the problem low for lithium ion battery energy density in prior art, it is provided that a kind of positive plate.
It is as follows that the present invention solves the technical scheme that above-mentioned technical problem used:
The preparation method of a kind of positive electrode active materials is provided, comprises the steps:
S1, acquisition molecular formula are Na3[CoMo6O24H6] precursor material, the mean diameter of described precursor material is more than 10 μm；
S2, described precursor material is dissolved in the water, adds water soluble alcohols organic solvent under agitation, carry out recrystallization, after filtration, obtain described positive electrode active materials；Described water soluble alcohols organic solvent is 1-5:1 with the volume ratio of water.
Meanwhile, present invention also offers a kind of positive plate, including plus plate current-collecting body and the positive electrode being positioned on plus plate current-collecting body, described positive electrode includes positive electrode active materials；Described positive electrode active materials is prepared by said method.
It addition, present invention also offers the lithium ion battery using above-mentioned positive plate, including battery container and the battery core that is arranged in battery container, described battery core includes winding or the positive plate of stacking, barrier film and negative plate；Described positive plate is foregoing positive plate.
In the present invention, it is Na by the mixed solution of water and water soluble alcohols organic solvent to molecular formula3[CoMo6O24H6] precursor material carry out recrystallization, the product mean diameter obtained has obtained obvious reduction, reach below 600nm, when using as positive electrode active materials, ionic conductivity can be effectively improved, the advantage making its high theoretical gram volume is fully used, thus is beneficial to be greatly improved lithium ion battery energy density.
Meanwhile, in said method, carrying out the organic solvent of interpolation during recrystallization is water soluble alcohols organic solvent, and its required addition is considerably less, is beneficial to reduce cost, reduces and pollutes.
Detailed description of the invention
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The preparation method of the positive electrode active materials that the present invention provides, comprises the steps:
S1, acquisition molecular formula are Na3[CoMo6O24H6] precursor material, the mean diameter of described precursor material is more than 10 μm；
S2, described precursor material is dissolved in the water, adds water soluble alcohols organic solvent under agitation, carry out recrystallization, after filtration, obtain described positive electrode active materials；Described water soluble alcohols organic solvent is 1-5:1 with the volume ratio of water.
In the present invention, molecular formula is Na3[CoMo6O24H6] material be material known in prior art, can be prepared, such as by the Na of 7.23g (29.88mmol) by conventional method2MoO4·2H2O is dissolved in 100ml deionized water, after it all dissolves, adds the CoSO of 2.256g (8.58mmol)4·6H2O solid, the Na of 0.977g (4.102mmol)2S2O8Solid, is then added dropwise over concentrated sulphuric acid, and adjusting solution ph is 3.5, then solution temperature is transferred to 60-80 DEG C, evaporates solution, until occurring precipitation in solution, stops heating, allows solution natural cooling.
Molecular formula of the prior art is Na3[CoMo6O24H6] precursor material particle size the biggest, usually more than 10 μm.
Inventor finds in an experiment, and molecular formula is Na3[CoMo6O24H6] precursor material there is the highest theoretical gram volume, when being used as the positive electrode active materials of lithium ion battery, be beneficial to improve lithium ion battery energy density.But, molecular formula is Na3[CoMo6O24H6] the low shortcoming of precursor material village electrical conductivity, constrain the performance of its chemical property greatly.
In the present invention, it is first Na by the molecular formula that above-mentioned mean diameter is more than 10 μm3[CoMo6O24H6] precursor material be dissolved in the water, the most under agitation add water soluble alcohols organic solvent, carry out recrystallization.I.e. available required positive electrode active materials after final filtration.
The mean diameter of the positive electrode active materials prepared by said method is nanoscale, reaches below 600nm, and under preferable case, the mean diameter of described positive electrode active materials is 100-600nm, more preferably 100-500nm, and uniform particle sizes.Nano level above-mentioned positive electrode active materials can shorten lithium ion transmission range in the electrodes, thus improves ionic conductivity to a certain extent.
According to the present invention, in above-mentioned steps S2, precursor material can be dissolved by the amount of water, and under preferable case, described precursor material is 0.01-0.05:1 with the mass ratio of described water, and the most described precursor material is 0.025-0.05:1 with the mass ratio of described water.
When the precursor material being dissolved in the water is carried out recrystallization, the water soluble alcohols organic solvent of interpolation and the volume ratio of water are 1-5:1, preferably 1-2:1.When using said method to carry out recrystallization, add a small amount of water soluble alcohols organic solvent and i.e. can reach the purpose of the recrystallization nano level positive electrode active materials of precipitation.
Water soluble alcohols organic solvent employed in above-mentioned steps can use the water soluble alcohols organic solvent of routine, the most specifically can be selected from one or more in methanol, ethanol, propanol, butanol or isopropanol.
Meanwhile, present invention also offers a kind of positive plate, including plus plate current-collecting body and the positive electrode being positioned on plus plate current-collecting body, described positive electrode includes the positive electrode active materials that method as described before prepares.
Similar with existing positive plate, in the present invention, the kind of described plus plate current-collecting body is the most known to those skilled in the art, such as, can be selected from aluminium foil, Copper Foil, Punching steel strip.
According to the present invention, in positive electrode, the content of positive electrode active materials is 20-99wt%, preferably 20-90wt%, more preferably 30-60wt%.In the present invention, under preferable case, in positive electrode, the mean diameter of positive electrode active materials is below 600nm, further preferably in the case of, the mean diameter of described positive electrode active materials is 100-600nm, more preferably 100-500nm.Now, it is beneficial to improve further the electric conductivity of positive electrode active materials, improves its charge/discharge capacity, beneficially improve the energy density of the lithium ion battery prepared by this positive electrode active materials.
In described positive electrode in addition to above-mentioned positive electrode active materials, the most also include the positive conductive agent that positive electrode binder and selectivity contain.
Positive electrode binder is had no particular limits by positive electrode of the present invention, can use the various positive electrode binder that can be used for lithium rechargeable battery known in the art, for example, it is possible to be one or more in Kynoar, politef or LA132.In described positive electrode, the content of described positive electrode binder is 0.5-10wt%, preferably 3-10wt%, more preferably 5-10wt%.
The positive electrode that the present invention provides can also optionally contain positive conductive agent the most contained in prior art positive electrode.Owing to positive conductive agent is for increasing the electric conductivity of electrode, reducing the internal resistance of battery, therefore the present invention preferably comprises positive conductive agent.Described positive conductive agent kind is known to those skilled in the art, and such as, described positive conductive agent can be selected from one or more in the positive conductive agent such as conductive carbon black, acetylene black, furnace black, CNT.
Inventor is found surprisingly that in test, in the present invention, on the basis of the positive electrode active materials that positive electrode active materials provides for the present invention, when positive conductive agent uses conductive carbon black, more preferable conductive effect can be realized, make positive electrode active materials give play to higher gram volume, thus more obviously improve the energy density of lithium ion battery.
In described positive electrode, the content of described positive conductive agent is 0.5-70wt%, preferably 30-60wt%.Now, on the basis of positive electrode active materials prepared by the method using the present invention to provide, in the case of above-mentioned positive conductive agent addition, it is beneficial to improve the gram volume of positive electrode active materials.
According to the present invention, the preparation method of above-mentioned positive plate is known, and such as, the preparation method of positive plate is included on plus plate current-collecting body the slurry of the positive conductive agent that coating contains containing positive electrode active materials, positive electrode binder and selectivity, dry, roll-in, i.e. obtains positive plate after cut-parts.Described dry generally at 50-160 DEG C, carry out at preferably 80-150 DEG C.Described roll-in and cut-parts are known to the skilled person, and after roll-in completes, cut according to the positive pole size of prepared battery request, obtain positive plate.
Described coating step forms the positive electrode material layer that thickness is 0.01-1mm on plus plate current-collecting body.
According to the present invention, can be selected from conventional solvent for preparing the solvent of anode sizing agent, as N-Methyl pyrrolidone (NMP), N can be selected from, one or more of dinethylformamide (DMF), N, N-diethylformamide (DEF), dimethyl sulfoxide (DMSO), oxolane (THF) and alcohol apoplexy due to endogenous wind.The consumption of solvent enables described slurry to be coated on described collector.
Meanwhile, present invention also offers a kind of lithium ion battery using above-mentioned positive plate, including battery container and the battery core that is arranged in battery container, described battery core includes positive plate, barrier film and the negative plate set gradually；Described positive plate is foregoing positive plate.
According to the present invention, in above-mentioned lithium ion battery, the remaining part beyond positive plate, such as battery container, barrier film, negative plate etc. all can use existing conventional structure and material.
Such as, like the prior art, described negative pole consist of known to one of skill in the art.The negative electrode active material comprised in negative pole includes to react the material forming lithium-containing compound, and lithium alloy with lithium ion.Under preferable case, use metal lithium sheet as negative pole.
In the present invention, as existing, barrier film is arranged between positive plate and negative plate, has electrical insulation capability and liquid retainability energy.Described barrier film can be selected from various barrier films used in lithium rechargeable battery, and under preferable case, described barrier film is selected from polyethylene diagrams, polypropylene diaphragm or polypropylene, polyethylene/polypropylene composite film.The position of described barrier film, character and kind are known to those skilled in the art.
Above-mentioned positive plate, barrier film, negative plate are set gradually, and prepares formation battery core by the way of conventional.Above-mentioned battery core is positioned in battery container, and by positive pole ear, positive plate is welded with the positive pole of battery, make positive plate be connected with the positive electrical of battery, by negative lug, negative plate is welded with the negative pole of battery, make negative plate be connected with the negative electricity of battery.
As known to those skilled in the art, after battery core being placed in battery case, also need to inject electrolyte in battery case, make battery core be immersed in electrolyte, eventually pass plasticizing and chemical conversion i.e. can get the lithium rechargeable battery that the present invention provides.
Electrolyte is not particularly limited by the present invention, can use the various of routine, and such as, as known to those skilled in the art, described electrolyte is by nonaqueous solvent and is dissolved in the electrolyte of nonaqueous solvent and forms.Above-mentioned nonaqueous solvent is not particularly limited, and can use nonaqueous solvent up to now.Described nonaqueous solvent can make various high boiling solvent of the prior art, low boiling point solvent or their mixture.Such as, gamma-butyrolacton can be selected from, ethylene carbonate, Ethyl methyl carbonate, dimethyl carbonate, diethyl carbonate, methyl propyl carbonate, ethyl propyl carbonic acid ester, Allyl carbonate, vinylene carbonate, diphenyl carbonate, methyl acetate, ethyl acetate, methyl propionate, ethyl propionate, dimethoxy-ethane, diethoxyethane, sultone and other are fluorine-containing, sulfur-bearing or the ring-type organosilane ester containing unsaturated bond, organic acid anhydride, N-Methyl pyrrolidone, N-METHYLFORMAMIDE, N-methylacetamide, N, dinethylformamide, sulfolane, acetonitrile, at least one in dimethyl sulfoxide.
The electrolyte dissolved in described nonaqueous solvent, the present invention, also without particularly limiting, can use the electrolyte being generally used for Lithium Secondary Battery Of Nonaqueous Electrolyte.Such as lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), hexafluoroarsenate lithium (LiSbF6), lithium perchlorate (LiClO4), fluorohydrocarbon base Sulfonic Lithium (LiCF3SO3)、Li(CF3SO2)2N、LiC4F9SO3, high lithium aluminate (LiAlO4)、LiN(CxF2x+1SO2)(CyF2y+1SO2) (in formula, x and y is the natural number of 1-10), one or more in lithium chloride (LiCl) and lithium iodide (LiI).In nonaqueous electrolytic solution, the concentration of electrolyte is generally 0.1-2.0mol/L, preferably 0.7-1.6mol/L.
By the following examples the present invention is further detailed.
Embodiment 1
The present embodiment is used for positive electrode active materials disclosed by the invention and preparation method thereof is described.
1, precursor material synthesis
Na by 7.23g (29.88mmol)2MoO4·2H2O is dissolved in 100ml deionized water, after it all dissolves, adds the CoSO of 2.256g (8.58mmol)4·6H2O solid, the Na of 0.977g (4.102mmol)2S2O8Solid, is then added dropwise over concentrated sulphuric acid, and adjusting solution ph is 3.5, then solution temperature is transferred to 60-80 DEG C, evaporates solution, until occurring precipitation in solution, stops heating, allows solution natural cooling.Obtain the precursor material that mean diameter is 12 μm.
2, prepared by positive electrode active materials
Under room temperature, above-mentioned for 2g precursor material is dissolved in 50ml distilled water, stirring and dissolving, adds 50ml ethanol under agitation, after separating out product, filter, it is thus achieved that positive electrode active materials, its mean diameter is 480nm.
3, the preparation of positive plate
By positive electrode active materials: conductive carbon black: positive electrode binder (PVDF) by the mass percent of 30%:60%:10% carry out slurry prepare, be coated with, dry, roll-in, cut-parts, obtain positive plate.
4, the preparation of lithium ion battery
Using above-mentioned positive plate (diameter 14mm), metal lithium sheet is negative plate, EC:DEC=3:7 (the volume ratio) (LiPF containing 1mol/L6) it is electrolyte, make 2032 type button cell S1.
Embodiment 2
The present embodiment is for illustrating the preparation method of positive electrode active materials disclosed by the invention, positive plate and lithium ion battery.
1, prepared by positive electrode active materials
Under room temperature, the precursor material of synthesis in 0.5g embodiment 1 is dissolved in 50ml distilled water, stirring and dissolving, adds 150ml ethanol under agitation, after separating out product, filter, it is thus achieved that positive electrode active materials, its mean diameter is 460nm.
2, the preparation of positive plate
By positive electrode active materials: conductive carbon black: positive electrode binder (PVDF) by the mass percent of 40%:55%:5% carry out slurry prepare, be coated with, dry, roll-in, cut-parts, obtain positive plate.
3, the preparation of lithium ion battery
Using above-mentioned positive plate (diameter 14mm), metal lithium sheet is negative plate, EC:DEC=3:7 (the volume ratio) (LiPF containing 1mol/L6) it is electrolyte, make 2032 type button cell S2.
Embodiment 3
The present embodiment is for illustrating the preparation method of positive electrode active materials disclosed by the invention, positive plate and lithium ion battery.
1, prepared by positive electrode active materials
Under room temperature, the precursor material of synthesis in 1.25g embodiment 1 is dissolved in 50ml distilled water, stirring and dissolving, adds 250ml ethanol under agitation, after separating out product, filter, it is thus achieved that positive electrode active materials, its mean diameter is 450nm.
2, the preparation of positive plate
By positive electrode active materials: conductive carbon black: positive electrode binder (PVDF) by the mass percent of 55%:42%:3% carry out slurry prepare, be coated with, dry, roll-in, cut-parts, obtain positive plate.
3, the preparation of lithium ion battery
Using above-mentioned positive plate (diameter 14mm), metal lithium sheet is negative plate, EC:DEC=3:7 (the volume ratio) (LiPF containing 1mol/L6) it is electrolyte, make 2032 type button cell S3.
Embodiment 4
The present embodiment is for illustrating the preparation method of positive electrode active materials disclosed by the invention, positive plate and lithium ion battery.
The preparation method of positive plate is substantially the same manner as Example 1, and difference is to use acetylene black to replace conductive carbon black, makes positive plate.
Use above-mentioned positive plate, prepare 2032 type button cell S4 according to the method for embodiment 1.
Comparative example 1
This comparative example is for preparation method, positive plate and the lithium ion battery of comparative illustration positive electrode active materials disclosed by the invention.
The method using embodiment 1 prepares lithium ion battery, except for the difference that, directly uses the precursor material in embodiment 1 to prepare positive plate and lithium ion battery as positive electrode active materials.
Obtain lithium ion battery D1.
Comparative example 2
This comparative example is for preparation method, positive plate and the lithium ion battery of comparative illustration positive electrode active materials disclosed by the invention.
The method using embodiment 1 prepares lithium ion battery, and except for the difference that, directly the precursor material in employing embodiment 1 is as positive electrode active materials, and uses acetylene black replacement conductive carbon black to prepare positive plate and lithium ion battery.
Obtain lithium ion battery D2.
Performance test
Above-mentioned lithium ion battery S1-S4 and D1, the D2 prepared is tested as follows:
Under 25 DEG C of environment, to battery voltage range be 1.5-4.2V, electric current density be 17mA/g under conditions of carry out constant current charge-discharge circulation.
The test result obtained is shown in Table 1.
Table 1
| Sample | Discharge capacity (mAh/g) first |
| S1 | 400 |
| S2 | 381 |
| S3 | 360 |
| S4 | 283 |
| D1 | 240 |
| D2 | 200 |
From the test result of table 1 it can be seen that the particle diameter of positive active material for preparing of the method using the present invention to provide is little, time on positive plate, it is beneficial to improve its electric conductivity.
The test result of comparative example 1 and embodiment 4 understands, and when the positive electrode active materials using conductive carbon black and the inventive method to prepare is used in conjunction with, can preferably improve electric conductivity and the specific capacity of battery.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (11)
1. the preparation method of a positive electrode active materials, it is characterised in that comprise the steps:
S1, acquisition molecular formula are Na3[CoMo6O24H6] precursor material, the mean diameter of described precursor material
It is more than 10 μm；
S2, described precursor material is dissolved in the water, adds water soluble alcohols organic solvent under agitation,
Carry out recrystallization, after filtration, obtain described positive electrode active materials；Described water soluble alcohols organic solvent and water
Volume ratio is 1-5:1.
Preparation method the most according to claim 1, it is characterised in that described precursor material and described water
Mass ratio be 0.01-0.05:1.
Preparation method the most according to claim 1, it is characterised in that described water soluble alcohols is organic molten
One or more in methanol, ethanol, propanol, butanol or isopropanol of agent.
4. according to the preparation method described in any one in claim 1-3, it is characterised in that described positive pole
The mean diameter of active material is 100-600nm.
5. a positive plate, it is characterised in that include plus plate current-collecting body and the positive pole being positioned on plus plate current-collecting body
Material, described positive electrode includes positive electrode active materials；Described positive electrode active materials passes through claim 1-4
Method described in middle any one prepares.
Positive plate the most according to claim 5, it is characterised in that described positive electrode include described just
Pole active material, positive electrode binder and positive conductive agent；Described positive conductive agent is conductive carbon black.
Positive plate the most according to claim 6, it is characterised in that described positive electrode binder is selected from poly-inclined
One or more in fluorothene, politef；
In described positive electrode, the content of described positive electrode active materials is 20-99wt%, described positive electrode binder
Content be 0.5-10wt%, the content of described positive conductive agent is 0.5-70wt%.
8. according to the positive plate described in any one in claim 5-7, it is characterised in that described positive pole collection
Positive electrode on fluid is stratiform, and its thickness is 0.01-1mm.
9. a lithium ion battery, it is characterised in that include battery container and be arranged in battery container
Battery core, described battery core includes positive plate, barrier film and the negative plate set gradually；
Described positive plate is the positive plate in claim 5-8 described in any one.
Lithium ion battery the most according to claim 9, it is characterised in that described negative plate is metal
Lithium sheet.
11. according to the lithium ion battery described in claim 9 or 10, it is characterised in that described barrier film is selected from
Polyethylene diagrams, polypropylene diaphragm or polypropylene, polyethylene/polypropylene composite film.
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