CN103311513B - A kind of high-performance layed solid-solution lithium electricity positive electrode and preparation method thereof - Google Patents
A kind of high-performance layed solid-solution lithium electricity positive electrode and preparation method thereof Download PDFInfo
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- CN103311513B CN103311513B CN201310215926.8A CN201310215926A CN103311513B CN 103311513 B CN103311513 B CN 103311513B CN 201310215926 A CN201310215926 A CN 201310215926A CN 103311513 B CN103311513 B CN 103311513B
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Abstract
The invention discloses a kind of high-performance layed solid-solution lithium electricity positive electrode and preparation method thereof, the material can use Li [Li1/ 3Mn2/3]O2·(1‑x)LiMO2(M=Ni, Co, Mn) is represented, is by lamellar compound Li [Li1/3Mn2/3]O2(i.e. Li2MnO3) and LiMO2Composition.Preparation method is：Manganese, nickel, the sulfate of cobalt, nitrate, acetate etc. are dissolved in into water by a certain percentage first and are configured to mixed-cation solution, with stirring, appropriate precipitant is added in mixed solution with certain speed, synthesize mixed hydroxides or carbonate coprecipitation presoma, dried presoma and lithium salts are pressed into the amount of certain material than wet method mixed at high speed, it is put into the logical oxygen of atmosphere furnace and carries out step sintering and obtain solid-solution material, finally, surface modification is carried out to material.The advantage of the method is：In the solution co-precipitation can make to be fully contacted between metal ion, can substantially reach atom level reaction level so that the pattern of presoma is easily controllable, even particle size distribution, material is carried out surface modification be conducive to improve its chemical property stablize.
Description
Technical field
The present invention relates to a kind of high-performance layed solid-solution lithium electricity positive electrode and preparation method thereof, category new energy materialses neck
Domain.
Background technology
xLi[Li1/3Mn2/3]O2·(1-x)LiMO2(M=Ni, Co, Mn) is by lamellar compound Li [Li1/3Mn2/3]O2(i.e.
Li2MnO3) and LiMO2The solid solution cathode material of composition.Specific discharge capacity in 2.0V-4.8V after optimization can exceed
300mAh/g, energy density reach 900Wh/kg.Consider performance and cost at present, M be Ni-Mn and Ni-Mn-Co more
It is preferable.Recent years, in view of cobalt price is high and environmental pollution, Li-Ni-Mn-O systems are of much attention, have Li [NixLi1/3-2x/ 3Mn2/3-x/3]O2With Li [NixLi1/3-x/3Mn2/3-2x/3]O2Two kinds of structural formulas.
Since the serial composite positive pole is proposed from Thackeray in 2004, which relies on, and thermal stability is good, specific capacity
The excellent chemical properties such as height, charge and discharge voltage width and low cost, eco-friendly comprehensive sexual clorminance receive extensive pass
Note, has been increasingly becoming the focus of domain expert's scholar's research, while the material is also considered as lithium of future generation by numerous experts and scholars
The choosing of the ideal of ion battery positive electrode.
The content of the invention
The purpose of the present invention be just to provide a kind of high-performance layed solid-solution lithium electricity positive electrode with and preparation method thereof.
The purpose of the present invention is realized by following technical proposal：First by manganese, nickel, the sulfate of cobalt, nitrate, acetic acid
Salt etc. is dissolved in water by a certain percentage and is configured to mixed-cation solution.With stirring, added in mixed solution with certain speed
Enter appropriate precipitant, strictly control precipitation temperature, acidity, the condition such as mixing speed make in solution by evenly mixing each
Component is according to target measured than being precipitated out, and synthesizes mixed hydroxides or carbonate coprecipitation presoma.Before dried
Body and lithium salts are driven by the amount of certain material than wet method mixed at high speed, the logical oxygen of atmosphere furnace is put into and is carried out step sintering and obtain solid solution
Body material.Finally, surface modification is carried out to material, the initial capacity for maintaining active material itself higher prevents metal ion from existing
Dissolving in electrolyte, and suppress the generation of side reaction, further improve the performance of the material.Specifically include the following steps：
1）Weigh manganese, nickel, the sulfate of cobalt, nitrate or acetate, deionized water dissolving first according to a certain percentage
It is configured to certain density mixed solution.
2）With stirring, in mixed solution, appropriate precipitant, reaction temperature is added to be set in 35-70 DEG C, pH controls
In 8.5-11, each component in solution by evenly mixing is according to target measured than being precipitated out, synthesize mixing hydroxide
Thing or carbonate coprecipitation presoma.
3）Presoma presses the amount of certain material than wet method mixed at high speed with lithium salts Jing after filtration, washing and drying process.
4）Mixture is put into into ceramic material pool alms bowl and is built in atmosphere furnace, the step sintering under oxygen atmosphere, after cooling, is passed through
Broken sieving obtains layed solid-solution material.
5）Surface modification is carried out to material, the performance of the material is further improved.
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, the nickel salt is Ni（NO3）2·6H2O、
NiSO4·6H2O、Ni（CH3COO）2·4H2One or more in O.
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, described manganese salt is Mn（NO3）2、
MnSO4·H2O、Mn（CH3COO）2·H2One or more in O.
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, described cobalt salt is Co（NO3）2·
6H2O、CoSO4·7H2O、Co（CH3COO）2·4H2O etc..
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, described precipitant is that hydroxide is common
Precipitate or carbonate coprecipitation, usually NaOH, NH4One or more in OH, KOH, LiOH.
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, it is described prepare presoma during,
The temperature of reaction system is preferably 55 DEG C, and pH value is preferably 10.0 or so.
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, described lithium salts mostly is Lithium hydrate,
Can also be lithium carbonate or lithium nitrate；Mixing method can be with dry blend wet mixing, and preferably with mixed at high speed comminutor wet mixing, the time is excellent
Elect 2h as.
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, the step sintering, once sintered side
Then preferably 500 DEG C insulation 4h of case rise to 750 DEG C of insulation 6h；Double sintering is preferably 850 DEG C of insulation 12h, and hot stage leads to
Oxygen.
In the preparation process of above-mentioned high-performance layed solid-solution lithium electricity positive electrode, the surface modification is referred to be entered to material
Row cladding, conventional cladding material is V2O5、LiV3O8、TiO2、AlF3、Al2O3、Co3(PO4)2And C claddings.
Solid-solution material prepared by the present invention is layer structure, and first charge-discharge specific capacity meansigma methodss are respectively
294.5mAh/g, 267.4 mAh/g；Mean diameter at 11-15 μm, tap density>1.8g/cm, specific surface area 0.3-0.6 ㎡/
G, pH≤11, Fe contents 40-60ppm, Cu contents are less than 10ppm, and other impurities are respectively less than 5ppm.
Description of the drawings
Fig. 1 is the SEM figures of prepared solid solution cathode material.
Fig. 2 is the XRD spectrum of prepared solid solution cathode material.
Specific embodiment
Embodiment 1
Weigh nickel sulfate 167.1g, manganese sulfate 446.4g, cobaltous sulfate 178.8g first respectively；With stirring, with 200 millis
L/h flow speed add in mixed solution concentration be 5mol/L ammonia spirit and 1mol/L sodium hydroxide solution
Make precipitant, reaction temperature is set in 50 DEG C, pH controls 10.5 or so, make each component in solution by evenly mixing by
Target metering ratio is precipitated out, and synthesizes mixed hydroxides co-precipitation presoma.Will be dried presoma mono- with 207.7g
Water lithium hydroxide wet method mixed at high speed 2 hours, loads and expects that alms bowl is put into the logical oxygen of atmosphere furnace and carries out step sintering, once calcine Jing two
Section Isothermal sinter, first in 500 DEG C of constant temperature 4 hours, then in 750 DEG C of constant temperature 6 hours, after cooling, crushing carries out secondary burning again
Knot, program are 900 DEG C and are incubated 8 hours.Solid-solution material is obtained to the crushing material staged care after cooling.Finally, use Al2O3
Carry out Surface coating to material, the initial capacity for maintaining active material itself higher prevents metal ion in the electrolytic solution molten
Solution, and suppress the generation of side reaction, further improve the performance of the material.After testing, the material tap density is 1.85g/
Cm, particle diameter D50For 13.26 μm, 0.45 ㎡ of specific surface area/g, pH value are 10.96, and first charge-discharge specific capacity is respectively
285.4mAh/g、258.6mAh/g。
Embodiment 2
Weigh nickel sulfate 167.1g, manganese sulfate 446.4g, cobaltous sulfate 178.8g first respectively；With stirring, with 150 millis
L/h flow speed add in mixed solution concentration be 5mol/L ammonia spirit and 1mol/L sodium hydroxide solution
Make precipitant, reaction temperature is set in 55 DEG C, pH controls 10.0 or so, make each component in solution by evenly mixing by
Target metering ratio is precipitated out, and synthesizes mixed hydroxides co-precipitation presoma.Will be dried presoma mono- with 207.7g
Water lithium hydroxide wet method mixed at high speed 2 hours, loads and expects that alms bowl is put into the logical oxygen of atmosphere furnace and carries out step sintering, once calcine Jing two
Section Isothermal sinter, first in 500 DEG C of constant temperature 4 hours, then in 750 DEG C of constant temperature 6 hours, after cooling, crushing carries out secondary burning again
Knot, program are 850 DEG C and are incubated 12 hours.Solid-solution material is obtained to the crushing material staged care after cooling.Finally, use V2O5
Carry out Surface coating to material, the initial capacity for maintaining active material itself higher prevents metal ion in the electrolytic solution molten
Solution, and suppress the generation of side reaction, further improve the performance of the material.After testing, the material tap density is 2.00g/
Cm, particle diameter D50For 12.16 μm, 0.47 ㎡ of specific surface area/g, pH value are 10.38, and first charge-discharge specific capacity is respectively
296.6mAh/g、268.3mAh/g。
Embodiment 3
Weigh nickel sulfate 167.1g, manganese sulfate 446.4g, cobaltous sulfate 178.8g first respectively；With stirring, with 120 millis
L/h flow speed add in mixed solution concentration be 5mol/L ammonia spirit and 1mol/L sodium hydroxide solution
Make precipitant, reaction temperature is set in 60 DEG C, pH controls 11.0 or so, make each component in solution by evenly mixing by
Target metering ratio is precipitated out, and synthesizes mixed hydroxides co-precipitation presoma.Will be dried presoma mono- with 207.7g
Water lithium hydroxide wet method mixed at high speed 2 hours, loads and expects that alms bowl is put into the logical oxygen of atmosphere furnace and carries out step sintering, once calcine Jing two
Section Isothermal sinter, first in 500 DEG C of constant temperature 4 hours, then in 750 DEG C of constant temperature 6 hours, after cooling, crushing carries out secondary burning again
Knot, program are 850 DEG C and are incubated 8 hours.Solid-solution material is obtained to the crushing material staged care after cooling.Finally, use V2O5It is right
Material carries out Surface coating, the initial capacity for maintaining active material itself higher, prevents metal ion dissolving in the electrolytic solution,
And suppress the generation of side reaction, further improve the performance of the material.After testing, the material tap density is 1.90g/cm,
Particle diameter D50For 12.36 μm, 0.46 ㎡ of specific surface area/g, pH value are 11.16, and first charge-discharge specific capacity is respectively 292.4mAh/
g、267.6mAh/g。
Claims (9)
1. a kind of high-performance layed solid-solution lithium electricity positive electrode, it is characterised in that the material is layer structure, first charge-discharge
Specific capacity meansigma methodss are respectively 294.5mAh/g, 267.4mAh/g；Mean diameter at 11-15 μm, tap density>1.8g/cm3,
Specific surface area 0.3-0.6m2/ g, pH≤11, Fe contents 40-60ppm, Cu contents are less than 10ppm, and other impurities are respectively less than 5ppm；
The lithium electricity positive electrode is prepared according to the following steps：
1) manganese, nickel, the sulfate of cobalt these three metals, nitrate or acetate are weighed first according to a certain percentage, deionization is used
Water dissolution is configured to certain density mixed solution；
2) with stirring, in mixed solution, appropriate precipitant, reaction temperature is added to be set in 35-70 DEG C, pH controls exist
8.5-11, makes each component in solution by evenly mixing according to target measure than being precipitated out, synthesizes mixed hydroxides
Or carbonate coprecipitation presoma；
3) presoma compares mixed at high speed by the amount of certain material with lithium salts Jing after filtration, washing and drying process；
4) mixture is put into into ceramic material alms bowl and is built in atmosphere furnace, the step sintering under oxygen atmosphere：Once sintered scheme is 500
DEG C insulation 4h then rise to 750 DEG C insulation 6h, double sintering be 850 DEG C insulation 12h, hot stage lead to oxygen；After cooling, Jing
Cross broken sieving and obtain a layer solid-solution material；
5) surface modification is carried out to material, further improves the performance of the material.
2. the preparation method of a kind of high-performance layed solid-solution lithium electricity positive electrode, it is characterised in that carry out in the steps below：
1) manganese, nickel, the sulfate of cobalt these three metals, nitrate or acetate are weighed first according to a certain percentage, deionization is used
Water dissolution is configured to certain density mixed solution；
2) with stirring, in mixed solution, appropriate precipitant, reaction temperature is added to be set in 35-70 DEG C, pH controls exist
8.5-11, makes each component in solution by evenly mixing according to target measure than being precipitated out, synthesizes mixed hydroxides
Or carbonate coprecipitation presoma；The mol ratio of Mn in the presoma, Ni, Co arbitrarily can be adjusted；
3) presoma compares mixed at high speed by the amount of certain material with lithium salts Jing after filtration, washing and drying process；
4) mixture is put into into ceramic material alms bowl and is built in atmosphere furnace, the step sintering under oxygen atmosphere：Once sintered scheme is 500
DEG C insulation 4h then rise to 750 DEG C insulation 6h, double sintering be 850 DEG C insulation 12h, hot stage lead to oxygen；After cooling, Jing
Cross broken sieving and obtain a layer solid-solution material；
5) surface modification is carried out to material, further improves the performance of the material.
3. according to claim 2 high-performance layed solid-solution lithium electricity positive electrode preparation method, it is characterised in that：Forerunner
The mol ratio of Mn in body, Ni, Co is 52-54：13：13.
4. according to claim 2 high-performance layed solid-solution lithium electricity positive electrode preparation method, it is characterised in that：It is described
Nickel salt is Ni (NO3)2·6H2O, NiSO4·6H2O, Ni (CH3COO)2·4H2One or more in O；Described manganese salt is Mn
(NO3)2, MnSO4·H2O, Mn (CH3COO)2·H2One or more in O；Described cobalt salt is Co (NO3)2·6H2O、
CoSO4·7H2O、Co(CH3COO)2·4H2O。
5. according to claim 2 high-performance layed solid-solution lithium electricity positive electrode preparation method, it is characterised in that：It is described
Precipitant be hydroxide or carbonate.
6. according to claim 5 high-performance stratiform with solution lithium electricity positive electrode preparation method, it is characterised in that：It is described
Precipitant be NaOH, NH4One or more in OH, KOH, LiOH.
7. according to claim 2 high-performance stratiform with solution lithium electricity positive electrode preparation method, it is characterised in that：It is described
Step 2) prepare presoma during, the temperature of reaction system is 55 DEG C, and pH value is 10.0.
8. according to claim 2 high-performance stratiform with solution lithium electricity positive electrode preparation method, it is characterised in that：It is described
Lithium salts be Lithium hydrate, lithium carbonate or lithium nitrate in one kind；Hybrid mode is one kind of dry blend wet mixing.
9. according to claim 2 high-performance layed solid-solution lithium electricity positive electrode preparation method, it is characterised in that：It is described
Surface modification refers to and material is coated that cladding material is V2O5, LiV3O8, TiO2, AlF3, A12O3, Co3(PO4)2And C bags
Cover.
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| CN104716315A (en) * | 2013-12-16 | 2015-06-17 | 青岛乾运高科新材料股份有限公司 | Preparation method of lithium ion batteries cathode material solid solution with core-shell structure |
| CN103811745B (en) * | 2014-02-18 | 2017-05-17 | 苏州路特新能源科技有限公司 | Method for preparing high-specific-capacity lithium-enriched lithium battery material |
| CN103794782B (en) * | 2014-02-27 | 2016-08-31 | 北京国能电池科技有限公司 | A kind of lithium-rich manganese base material, its preparation method and lithium ion battery |
| CN104051724A (en) * | 2014-06-06 | 2014-09-17 | 奇瑞汽车股份有限公司 | Carbon-coated nickel-cobalt lithium manganate positive electrode material and preparation method thereof |
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| GB2566473B (en) | 2017-09-14 | 2020-03-04 | Dyson Technology Ltd | Magnesium salts |
| CA3083136C (en) * | 2017-11-22 | 2022-04-12 | Nemaska Lithium Inc. | Processes for preparing hydroxides and oxides of various metals and derivatives thereof |
| GB2569392B (en) | 2017-12-18 | 2022-01-26 | Dyson Technology Ltd | Use of aluminium in a cathode material |
| GB2569387B (en) | 2017-12-18 | 2022-02-02 | Dyson Technology Ltd | Electrode |
| GB2569390A (en) * | 2017-12-18 | 2019-06-19 | Dyson Technology Ltd | Compound |
| GB2569388B (en) | 2017-12-18 | 2022-02-02 | Dyson Technology Ltd | Compound |
| CN114864886B (en) * | 2022-04-02 | 2024-02-27 | 万华化学集团股份有限公司 | Positive electrode material and preparation method thereof |
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Denomination of invention: High-performance layered solid-solution lithium-battery positive material and preparation method thereof Effective date of registration: 20200629 Granted publication date: 20170405 Pledgee: China Construction Bank Corporation Qingdao Zhongshan Road sub branch Pledgor: QINGDAO QIANYUN HIGH-TECH NEW MATERIAL Co.,Ltd. Registration number: Y2020370010025 |