CN106486664A - Positive electrode material precursor preparation method and sintering method and lithium ion battery - Google Patents
Positive electrode material precursor preparation method and sintering method and lithium ion battery Download PDFInfo
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- CN106486664A CN106486664A CN201610834477.9A CN201610834477A CN106486664A CN 106486664 A CN106486664 A CN 106486664A CN 201610834477 A CN201610834477 A CN 201610834477A CN 106486664 A CN106486664 A CN 106486664A
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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
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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
- H01M4/36—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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- 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
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Abstract
Positive electrode material precursor preparation method of the present invention, comprises the steps：1a) configure mixed solution A：By Ni：Mn=1:3 configure soluble nickel source compounds and manganese source compound and obtain mixed solution A；1b) configure mixed solution B；1c) mixed solution A and mixed solution B are added dropwise in reaction vessel and are sufficiently stirred for；1d) well-beaten mixed solution A and mixed solution B are carried out still aging, after carry out filtering and washing；1e) dry, and finally give high magnification nickel lithium manganate cathode material presoma.The present invention utilizes oxalates series precipitant, effectively simplify the building-up process of co-precipitation nickel manganese presoma, and the technique of material microwave Fast Sintering is so as to manufacturing cycle greatly shortens, obtain the nickel ion doped material of bigger serface, effectively raise the high rate charge-discharge performance of electrode material.
Description
Technical field
The invention belongs to being applied to field of lithium ion battery, the Fast back-projection algorithm technology of more particularly, to nickel ion doped material is led
Domain, specifically, it provides a kind of positive electrode material precursor preparation method and sintering method and lithium ion battery.
Background technology
Since twentieth century, with the continuous development of human society, growing to the demand of the energy, the shortage of the energy is very
Become the bottleneck that the mankind continue development to exhaustion, it is high that people's exigence finds a kind of new, cheap, energy storage efficiency
, environment amenable battery material；
Since the seventies energy crisis, history is climbed up with lithium and the novel battery as energy storage material for the transistion metal compound
Stage, compared with the secondary cell in past, it is prominent that lithium rechargeable battery has high, energy big, good cycle of force density of voltage etc.
Go out advantage, and the performance of lithium ion battery is largely more dependent upon positive electrode；
Especially Sony issued first item commercial Li-ion battery in 1992, and it is with stratiform cobalt acid lithium as positive pole
Material；
But cobalt acid lithium material has high cost, environment is unfriendly, heat stability difference the shortcomings of, therefore improving cobalt acid
While lithium anode material, Olivine-type Cathode Material in Li-ion Batteries is also required to be constantly brought forth new ideas；
The ternary layered material coming different from cobalt acid lithium Materials and the LiFePO 4 material of olivine, with manganese
Sour lithium is the spinel-type positive electrode of representative, has three-dimensional ionic transport passages, therefore has outstanding chemical property；
In spinel, LiMn2O4 structural instability, it is susceptible to crystal transition, lead to capacity attenuation too fast, follow
Ring poor performance, the shortcomings of energy density is high.Nickel ion doped material is on the basis of lithium manganate material, and part manganese nickel is taken
In generation, make nickel, in charge and discharge cycles, variation of valence occur, and manganese plays skeleton function in the material, rock-steady structure；Nickel ion doped material
Material reversible capacity reaches 147mAh/g, and voltage flat rubber belting is 4.7V.
At present, the preparation method preparing spinel-type nickel ion doped material mainly has solid-phase ball milling method, sol-gal process, is total to
The sedimentation method, high temperature hydro-thermal, spray drying etc..Gao et al. [Controlled Preparation and
Characterization of Spherical LiNi0.5Mn1.5O4Cathode Material for Lithium-Ion
Batteries."Journal of The Electrochemical Society 2010.157(7):A899] use sodium carbonate
As precipitant, sulfate prepares spinel-type nickel ion doped as manganese source and nickel source, its 0.2C, first circle under 1C, 5.0C multiplying power
Charge/discharge capacity is respectively 136.7,129.2 and 108.8mAh g-1.
Meanwhile, during the course of the reaction the control of pH is required with higher, sintering process complexity, energy charge is huge.As China
Patent application Patent No. 201210532234.1 discloses the nickel ion doped material that a kind of coprecipitation prepares manganese Concentraton gradient,
Make its manganese high in the concentration of internal layer, play rock-steady structure effect, low in outer layer concentration, reduce the erosion to electrode material for the electrolyte,
But its precursor synthesis step is excessively loaded down with trivial details, and commercial production difficulty is larger.
Therefore, it is necessary to propose a kind of positive electrode material precursor preparation method and sintering method and lithium ion battery.
Content of the invention
The invention mainly solves the technical problem of for the deficiency of existing production technology, proposing a kind of positive electrode forerunner
Preparation and sintering method and lithium ion battery, in the form of sheets, offspring is made up of presoma primary particle lamellar
Spherical so that material has large specific surface area, lift its high rate performance.
The present invention is achieved through the following technical solutions above-mentioned required solve problem：
A kind of positive electrode material precursor preparation method, it comprises the steps：
1a) configure mixed solution A：By Ni：Mn=1:3 configure soluble nickel source compounds and manganese source compound and are mixed
Close solution A；
1b) configure mixed solution B；
1c) mixed solution A and mixed solution B are added dropwise in reaction vessel and are sufficiently stirred for；
1d) well-beaten mixed solution A and mixed solution B are carried out still aging, after carry out filtering and washing；
1e) dry, and finally give positive electrode material precursor.
Further, described step 1b) in mixed solution B be the mixed solution of (NH4) 2C2O4 H2O and deionized water,
It is excessive 0%-20% by measuring than (NH4) 2C2O4 H2O.
Further, step 1c) in, whipping temp is 30 ° -70 °, and during stirring, pH value is controlled in 4-7.
Further, step 1d) in, washing is to be washed using distilled water, and washing times are three times；When being aged simultaneously
Between be 12h.
Further, described drying is dried for being placed in the drying container being made up of vacuum drying oven, drying temperature
For 60 ° -100 °, the time is 12h.
A kind of positive electrode material precursor sintering method, comprises the steps：
2a) high magnification nickel lithium manganate cathode material presoma is mixed with lithium source；
2b) mixed high magnification nickel lithium manganate cathode material presoma and lithium source inserted and be made up of microwave sintering ore deposit
In sintering container：
2c) control sintering container to be warming up to 400 ° -600 ° in 20 ° -50 °/min to be incubated, cool down afterwards；
2d) control sintering container to be warming up to 700 ° -1000 ° in 20 ° -50 °/min and be incubated again, after cool down again；
2e) it is tempered.
Further, described lithium source is made up of Li2CO3, and by metering ratio, lithium source addition is excessive 0%-10%.
Further, step 2e) for Muffle furnace, temperature is 500 ° -700 ° to the middle container that is tempered.
Further, described step 2e) in the temperature time be 12h, step 2c) and step 2d) in, insulation with again
Temperature retention time is 30～120min.
A kind of lithium ion battery, presoma is burnt by positive electrode material precursor by after the preparation of positive electrode material precursor preparation method
Knot method is sintered gained.
Compared with prior art, the positive electrode material precursor preparation method of the present invention and sintering method and lithium-ion electric
The having the beneficial effects that of pond：Using oxalates series precipitant, effectively simplify the building-up process of co-precipitation nickel manganese presoma,
And the technique of material microwave Fast Sintering is so as to manufacturing cycle greatly shortens, obtains the nickel ion doped material of bigger serface, have
The high rate charge-discharge performance that improve electrode material of effect.
Brief description
Fig. 1 is the structural representation of embodiment 1；
Specific embodiment
Embodiment 1：
A kind of forerunner's preparation and sintering method a, it comprises the steps：
1) weigh 6.571g NiSO4 and 12.675g MnSO4, be added in 100ml deionized water, be completely dissolved and obtain
Mixed solution A
2) weigh 14.2 (NH4) 2C2O4 H2O to be added in 100ml deionized water, be completely dissolved and obtain mixed solution B；
3) mixed solution A and mixed solution B solution are simultaneously added dropwise in reactor with given pace, and reaction temperature is 50
DEG C, adjusting pH is 6, stirs 2h after being added dropwise to complete；
4) static ageing 12h, rear filtering and washing solution, and dried using the drying container being made up of vacuum drying oven
Dry, drying temperature is 100 °, and the time finally gives oxalate precursor for 12h, and the chemistry of oxalate precursor becomes
Ni0.5Mn1.5(C2O4)2；
5) weigh 2g oxalate precursor, the lithium source being made up of Li2CO3 with 0.21g is sufficiently mixed, be placed in being burnt by microwave
In the sintering container that knot ore deposit is constituted, control sintering container to be warming up to 500 DEG C in 20 DEG C/min and carry out being incubated 30min, cool down afterwards；
6) control sintering container in 20 DEG C/min be warming up to again 900 DEG C carry out be incubated 30min, after cool down again；
7) step 6 will be carried out) after oxalate precursor be placed in the tempering container being made up of Muffle furnace with lithium source mixture
In, control tempering vessel temp in 700 DEG C and to be incubated 12h, before preparing the nickel ion doped being made up of LiNi0.5Mn1.5O4
Drive body.
Step 7) the nickel ion doped presoma of preparing gained is applied to lithium ion battery.
Refer to Fig. 1, it is that oxalate precursor manufactured in the present embodiment (shows as figure a) and microwave sintering for accompanying drawing 1
Nickel ion doped presoma afterwards (shows as figure b) scanning electron microscopy.It can be seen that oxalate precursor has lamellar
Primary particle composition globoid, particle size be about 20 μm.Nickel ion doped presoma after microwave sintering, particle size is about
For 15 μm about, it is made up of a large amount of 1～2 μm about of primary particle, porosity is larger, such structure is conducive to and electrolyte
It is fully contacted, improve the high rate performance of electrode material.
Embodiment 2：
A kind of forerunner's preparation and sintering method b, it comprises the steps：
1) weigh 6.571g NiSO4 and 12.675g MnSO4, be added in 100ml deionized water, be completely dissolved and obtain
Mixed solution A
2) weigh 17.04g (NH4) 2C2O4 H2O to be added in 100ml deionized water, be completely dissolved and obtain mixed solution
B；
3) mixed solution A and mixed solution B solution are simultaneously added dropwise in reactor with given pace, and reaction temperature is 30
DEG C, adjusting pH is 4, stirs 3h after being added dropwise to complete；
4) static ageing 18h, rear filtering and washing solution, and dried using the drying container being made up of vacuum drying oven
Dry, drying temperature is 60 °, and the time finally gives oxalate precursor for 12h, and the chemistry of oxalate precursor becomes
Ni0.5Mn1.5(C2O4)2；
5) weigh 2g oxalate precursor, the lithium source being made up of Li2CO3 with 0.225g is sufficiently mixed, and is placed in by microwave
In the sintering container that sintering deposit is constituted, control sintering container to be warming up to 400 DEG C in 50 DEG C/min and carry out being incubated 120min, cold afterwards
But；
6) control sintering container in 50 DEG C/min be warming up to again 700 DEG C carry out be incubated 120min, after cool down again；
7) step 6 will be carried out) after oxalate precursor be placed in the tempering container being made up of Muffle furnace with lithium source mixture
In, control tempering vessel temp in 600 DEG C and to be incubated 18h, before preparing the nickel ion doped being made up of LiNi0.5Mn1.5O4
Drive body.
Step 7) the nickel ion doped presoma of preparing gained is applied to lithium ion battery.
Embodiment 3
A kind of forerunner's preparation and sintering method c, it comprises the steps：
1) weigh 6.571g NiSO4 and 12.675g MnSO4, be added in 100ml deionized water, be completely dissolved and obtain
Mixed solution A
2) weigh 15.62g (NH4) 2C2O4 H2O to be added in 100ml deionized water, be completely dissolved and obtain mixed solution
B；
3) mixed solution A and mixed solution B solution are simultaneously added dropwise in reactor with given pace, and reaction temperature is 70
DEG C, adjusting pH is 5, stirs 5h after being added dropwise to complete；
4) static ageing 24h, rear filtering and washing solution, and dried using the drying container being made up of vacuum drying oven
Dry, drying temperature is 80 °, and the time finally gives oxalate precursor for 12h, and the chemistry of oxalate precursor becomes
Ni0.5Mn1.5(C2O4)2；
5) weigh 2g oxalate precursor, the lithium source being made up of Li2CO3 with 0.232g is sufficiently mixed, and is placed in by microwave
In the sintering container that sintering deposit is constituted, control sintering container to be warming up to 400 DEG C in 50 DEG C/min and carry out being incubated 120min, cold afterwards
But；
6) control sintering container in 50 DEG C/min be warming up to again 700 DEG C carry out be incubated 120min, after cool down again；
7) step 6 will be carried out) after oxalate precursor be placed in the tempering container being made up of Muffle furnace with lithium source mixture
In, control tempering vessel temp in 600 DEG C and to be incubated 18h, before preparing the nickel ion doped being made up of LiNi0.5Mn1.5O4
Drive body.
Step 7) the nickel ion doped presoma of preparing gained is applied to lithium ion battery.
Compared with prior art, forerunner's preparation that embodiment 1-3 is shown and the beneficial effect of sintering method exist
In：Using oxalates series precipitant, effectively simplify the building-up process of co-precipitation nickel manganese presoma, and material microwave is quick
The technique of sintering, so as to manufacturing cycle greatly shortens, obtains the nickel ion doped material of bigger serface, effectively raises electrode
The high rate charge-discharge performance of material.
Above-described is only some embodiments of the present invention.For the person of ordinary skill of the art, not
On the premise of departing from the invention design, some deformation can also be made and improve, these broadly fall into the protection model of the present invention
Enclose.
Claims (10)
1. a kind of positive electrode material precursor preparation method it is characterised in that：Comprise the steps：
1a) configure mixed solution A：By Ni：Mn=1:3 configuration soluble nickel source compounds and manganese source compound obtaining mix molten
Liquid A；
1b) configure mixed solution B；
1c) mixed solution A and mixed solution B are added dropwise in reaction vessel and are sufficiently stirred for；
1d) well-beaten mixed solution A and mixed solution B are carried out still aging, after carry out filtering and washing；
1e) dry, and finally give positive electrode material precursor.
2. positive electrode material precursor preparation method according to claim 1 it is characterised in that：Described step 1b) middle mixing
Solution B is (NH4)2C2O4·H2O and the mixed solution of deionized water, by metering than (NH4)2C2O4·H2O is excessive 0%-
20%.
3. positive electrode material precursor preparation method according to claim 1 it is characterised in that：Step 1c) in, whipping temp
For 30 ° -70 °, during stirring, pH value is controlled in 4-7.
4. positive electrode material precursor preparation method according to claim 1 it is characterised in that：Step 1d) in, wash as profit
Washed with distilled water, washing times are three times；Digestion time is 12h simultaneously.
5. the positive electrode material precursor preparation method according to claim 1-4 any one it is characterised in that：Described drying
Dried for being placed in the drying container being made up of vacuum drying oven, drying temperature is 60 ° -100 °, the time is 12h.
6. a kind of positive electrode material precursor sintering method it is characterised in that：Comprise the steps：
2a) high magnification nickel lithium manganate cathode material presoma is mixed with lithium source；
2b) mixed high magnification nickel lithium manganate cathode material presoma and lithium source are inserted the sintering being made up of microwave sintering ore deposit
In container：
2c) control sintering container to be warming up to 400 ° -600 ° in 20 ° -50 °/min to be incubated, cool down afterwards；
2d) control sintering container to be warming up to 700 ° -1000 ° in 20 ° -50 °/min and be incubated again, after cool down again；
2e) it is tempered.
7. positive electrode material precursor sintering method according to claim 6 it is characterised in that：Described lithium source is by Li2CO3Structure
Become, by metering ratio, lithium source addition is excessive 0%-10%.
8. positive electrode material precursor sintering method according to claim 6 it is characterised in that：Step 2e) middle tempering container
For Muffle furnace, temperature is 500 ° -700 °.
9. the positive electrode material precursor sintering method according to claim 6-8 any one it is characterised in that：Described step
In 2e), the temperature time is 12h, step 2c) and step 2d) in, insulation and again temperature retention time are 30～120min.
10. a kind of comprise by described in claim 1 positive electrode material precursor preparation method preparation after through described in claim 6
The lithium ion battery of the high magnification nickel lithium manganate cathode material presoma of positive electrode material precursor sintering method sintering.
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| CN108288711A (en) * | 2018-02-12 | 2018-07-17 | 成都理工大学 | A kind of quaternary lithium-ion battery positive electrode material and preparation method |
| CN109713277A (en) * | 2018-12-29 | 2019-05-03 | 蜂巢能源科技有限公司 | Anode material for lithium-ion batteries and preparation method, lithium ion battery |
| CN111048739A (en) * | 2019-12-25 | 2020-04-21 | 中国科学院过程工程研究所 | Ternary positive electrode slurry, preparation method thereof and lithium battery |
| CN114408987A (en) * | 2022-03-30 | 2022-04-29 | 宜宾锂宝新材料有限公司 | Nickel-cobalt-manganese precursor, ternary cathode material and preparation method thereof |
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Application publication date: 20170308 |