CN103311513A - High-performance layered solid-solution lithium-battery positive material and preparation method thereof - Google Patents
High-performance layered solid-solution lithium-battery positive material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-performance layered solid-solution lithium-battery positive material and a preparation method thereof. The substance can be expressed as Li[Li1/3Mn2/3]O2.(1-x)LiMo2 (M=Ni, Co and Mn) and consists of a layered compound Li[Li1/3Mn2/3]O2 (i.e. Li2MnO3) and LiMo2. The preparation method comprises the following steps of: firstly, dissolving sulfate, nitrate and acetate of manganese, nickel and cobalt into water according to a given ratio to prepare a mixed positive ion solution, and adding an appropriate precipitator into the mixed solution at a given speed while the solution is stirred, thus synthesizing a mixed hydroxide or carbonate co-precipitation precursor; mixing the dried precursor with lithium salt according to a given substance volume ratio through a wet method at a high speed, and carrying out step-by-step sintering on the mixture in an atmosphere furnace, into which oxygen is introduced, to obtain a solid-solution material; and finally, decorating the surface of the material. The method has the advantages that by adopting the co-precipitation in the solution, metal ions can adequately contact one another, and an atomic reaction level can be basically reached, so that the shape of the precursor is easy to control, and the granularity is uniform; the surface decoration of the material is favorable for the stability of the electrochemical performance of the material.
Description
Technical field
The present invention relates to a kind of high-performance stratiform solid solution lithium electricity positive electrode and preparation method thereof, belong to the new energy materials field.
Background technology
XLi[Li
1/3Mn
2/3] O
2(1-x) LiMO
2(M=Ni, Co, Mn) is by lamellar compound Li[Li
1/3Mn
2/3] O
2(be Li
2MnO
3) and LiMO
2The solid solution positive electrode of forming.Can surpass 300mAh/g by optimizing the back at the specific discharge capacity of 2.0V-4.8V, energy density reaches 900Wh/kg.Take all factors into consideration performance and cost at present, M is that Ni-Mn and Ni-Mn-Co are comparatively desirable.Recent years, in view of cobalt price height and environmental pollution, Li-Ni-Mn-O system receives more concerns, and Li[Ni is arranged
xLi
1/3-2
x/ 3
Mn
2/3-
x/ 3
] O
2And Li[Ni
xLi
1/3-x/3Mn
2/3-2
x/ 3
] O
2Two kinds of structural formulas.
Since Thackeray in 2004 proposes this series composite positive pole, it relies on that thermal stability is good, specific capacity is high, charge and discharge excellent electrochemical properties such as voltage is wide and low, the eco-friendly comprehensive advantage of cost has been subjected to paying close attention to widely, become the focus of this domain expert's scholar's research gradually, this material also is considered as the choosing of the ideal of lithium ion power battery cathode material of future generation by numerous experts and scholars simultaneously.
Summary of the invention
Purpose of the present invention just providing a kind of high-performance stratiform solid solution lithium electricity positive electrode with and preparation method thereof.
The objective of the invention is to realize by following technical proposal: first sulfate with manganese, nickel, cobalt, nitrate, acetate etc. are the water-soluble mixed-cation solution that is mixed with by a certain percentage.Follow stirring, in mixed solution, add suitable precipitation reagent with certain speed, conditions such as strict control precipitation temperature, acidity, mixing speed are according to target measured than being precipitated out each component that has mixed in the solution, synthesize mixed hydroxides or carbonate coprecipitation presoma.With dried presoma and lithium salts by certain amount of substance than wet method high-speed mixing, put into the logical oxygen of atmosphere furnace and carry out the substep sintering and obtain solid-solution material.At last, material is carried out finishing, keep the higher initial capacity of active material self, stop the dissolving of metal ion in electrolyte, and suppress the generation of side reaction, further improve the performance of this material.Specifically comprise following a few step:
1) takes by weighing sulfate, nitrate or the acetate of manganese, nickel, cobalt at first according to a certain percentage, be mixed with certain density mixed solution with deionized water dissolving.
2) follow stirring, add suitable precipitation reagent in mixed solution, reaction temperature is set in 35-70 ℃, and pH controls at 8.5-11, each component that has mixed in the solution is according to target measured than being precipitated out, synthesize mixed hydroxides or carbonate coprecipitation presoma.
3) presoma after filtration, behind washing and the drying process with lithium salts by certain amount of substance than wet method high-speed mixing.
4) mixture is put into ceramic material pool alms bowl and be built in atmosphere furnace, substep sintering under oxygen atmosphere, after the cooling, the process fragmentation is sieved and is obtained the stratiform solid-solution material.
5) material is carried out finishing, further improve the performance of this material.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, described nickel salt is Ni(NO
3)
26H
2O, NiSO
46H
2O, Ni(CH
3COO)
24H
2Among the O one or more.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, described manganese salt is Mn(NO
3)
2, MnSO
4H
2O, Mn(CH
3COO)
2H
2Among the O one or more.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, described cobalt salt is Co(NO
3)
26H
2O, CoSO
47H
2O, Co(CH
3COO)
24H
2O etc.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, described precipitation reagent is hydroxide co-precipitation or carbonate coprecipitation, is generally NaOH, NH
4Among OH, KOH, the LiOH one or more.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, in the process of described preparation presoma, the temperature of reaction system is preferably 55 ℃, and the pH value is preferably about 10.0.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, described lithium salts mostly is lithium hydroxide, also can be lithium carbonate or lithium nitrate; Mixing method can the dry blend wet mixing, preferably uses the wet mixing of high-speed mixing comminutor, and the time is preferably 2h.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, described substep sintering, 500 ℃ of insulations of once sintered scheme optimization 4h rises to 750 ℃ of insulation 6h then; Double sintering is preferably 850 ℃ of insulation 12h, and hot stage is logical oxygen all.
In the preparation process of above-mentioned high-performance stratiform solid solution lithium electricity positive electrode, described finishing refers to material is coated, and coating material commonly used is V
2O
5, LiV
3O
8, TiO
2, AlF
3, Al
2O
3, Co
3(PO
4)
2And C coats.
The prepared solid-solution material of the present invention is layer structure, and first charge-discharge specific capacity mean value is respectively 294.5mAh/g, 267.4 mAh/g; Average grain diameter is in 11-15 μ m, tap density〉1.8g/cm3, specific area 0.3-0.6 ㎡/g, pH≤11, Fe content 40-60ppm, Cu content are less than 10ppm, and other impurity are all less than 5ppm.
Description of drawings
Fig. 1 is the SEM figure of prepared solid solution positive electrode.
Fig. 2 is the XRD collection of illustrative plates of prepared solid solution positive electrode.
Embodiment
Take by weighing nickelous sulfate 167.1g at first respectively, manganese sulfate 446.4g, cobaltous sulfate 178.8g; Follow stirring, adding concentration with 200 milliliters/hour flow speed in the mixed solution is that the ammonia spirit of 5mol/L and the sodium hydroxide solution of 1mol/L are made precipitation reagent, reaction temperature is set in 50 ℃, pH control is about 10.5, each component that has mixed in the solution is according to target measured than being precipitated out, synthesize mixed hydroxides co-precipitation presoma.With dried presoma and 207.7g monohydrate lithium hydroxide wet method high-speed mixing 2 hours, the material alms bowl of packing into is put into the logical oxygen of atmosphere furnace and is carried out the substep sintering, once calcine through two sections constant temperature sintering, at first 500 ℃ of constant temperature 4 hours, then 750 ℃ of constant temperature 6 hours, after the cooling, pulverize and carry out double sintering again, program is 900 ℃ of insulations 8 hours.Cooled material crushing and classification processing is obtained solid-solution material.At last, use Al
2O
3Material is carried out the surface coat, keep the higher initial capacity of active material self, stop the dissolving of metal ion in electrolyte, and suppress the generation of side reaction, further improve the performance of this material.After testing, this material tap density is 1.85g/cm3, particle diameter D
50Be 13.26 μ m, specific area 0.45 ㎡/g, the pH value is 10.96, the first charge-discharge specific capacity is respectively 285.4mAh/g, 258.6mAh/g.
Embodiment 2
Take by weighing nickelous sulfate 167.1g at first respectively, manganese sulfate 446.4g, cobaltous sulfate 178.8g; Follow stirring, adding concentration with 150 milliliters/hour flow speed in the mixed solution is that the ammonia spirit of 5mol/L and the sodium hydroxide solution of 1mol/L are made precipitation reagent, reaction temperature is set in 55 ℃, pH control is about 10.0, each component that has mixed in the solution is according to target measured than being precipitated out, synthesize mixed hydroxides co-precipitation presoma.With dried presoma and 207.7g monohydrate lithium hydroxide wet method high-speed mixing 2 hours, the material alms bowl of packing into is put into the logical oxygen of atmosphere furnace and is carried out the substep sintering, once calcine through two sections constant temperature sintering, at first 500 ℃ of constant temperature 4 hours, then 750 ℃ of constant temperature 6 hours, after the cooling, pulverize and carry out double sintering again, program is 850 ℃ of insulations 12 hours.Cooled material crushing and classification processing is obtained solid-solution material.At last, use V
2O
5Material is carried out the surface coat, keep the higher initial capacity of active material self, stop the dissolving of metal ion in electrolyte, and suppress the generation of side reaction, further improve the performance of this material.After testing, this material tap density is 2.00g/cm3, particle diameter D
50Be 12.16 μ m, specific area 0.47 ㎡/g, the pH value is 10.38, the first charge-discharge specific capacity is respectively 296.6mAh/g, 268.3mAh/g.
Embodiment 3
Take by weighing nickelous sulfate 167.1g at first respectively, manganese sulfate 446.4g, cobaltous sulfate 178.8g; Follow stirring, adding concentration with 120 milliliters/hour flow speed in the mixed solution is that the ammonia spirit of 5mol/L and the sodium hydroxide solution of 1mol/L are made precipitation reagent, reaction temperature is set in 60 ℃, pH control is about 11.0, each component that has mixed in the solution is according to target measured than being precipitated out, synthesize mixed hydroxides co-precipitation presoma.With dried presoma and 207.7g monohydrate lithium hydroxide wet method high-speed mixing 2 hours, the material alms bowl of packing into is put into the logical oxygen of atmosphere furnace and is carried out the substep sintering, once calcine through two sections constant temperature sintering, at first 500 ℃ of constant temperature 4 hours, then 750 ℃ of constant temperature 6 hours, after the cooling, pulverize and carry out double sintering again, program is 850 ℃ of insulations 8 hours.Cooled material crushing and classification processing is obtained solid-solution material.At last, use V
2O
5Material is carried out the surface coat, keep the higher initial capacity of active material self, stop the dissolving of metal ion in electrolyte, and suppress the generation of side reaction, further improve the performance of this material.After testing, this material tap density is 1.90g/cm3, particle diameter D
50Be 12.36 μ m, specific area 0.46 ㎡/g, the pH value is 11.16, the first charge-discharge specific capacity is respectively 292.4mAh/g, 267.6mAh/g.
Claims (10)
1. a high-performance stratiform solid solution lithium electricity positive electrode is characterized in that this material is layer structure, and first charge-discharge specific capacity mean value is respectively 294.5mAh/g, 267.4 mAh/g; Average grain diameter is in 11-15 μ m, tap density〉1.8g/cm3, specific area 0.3-0.6 ㎡/g, pH≤11, Fe content 40-60ppm, Cu content are less than 10ppm, and other impurity are all less than 5ppm.
2. the preparation method of high-performance stratiform solid solution lithium electricity positive electrode is characterized in that being undertaken by following step:
1) takes by weighing sulfate, nitrate or the acetate of manganese, nickel, these three kinds of metals of cobalt at first according to a certain percentage, be mixed with certain density mixed solution with deionized water dissolving;
2) follow stirring, add suitable precipitation reagent in mixed solution, reaction temperature is set in 35-70 ℃, and pH controls at 8.5-11, each component that has mixed in the solution is according to target measured than being precipitated out, synthesize mixed hydroxides or carbonate coprecipitation presoma; Mn in the described presoma, Ni, the mol ratio of Co can arbitrarily be adjusted;
3) presoma after filtration, compare high-speed mixing with lithium salts by certain amount of substance behind washing and the drying process;
4) mixture is put into the ceramic material alms bowl and be built in atmosphere furnace, substep sintering under oxygen atmosphere, after the cooling, the process fragmentation is sieved and is obtained the stratiform solid-solution material;
5) material is carried out finishing, further improve the performance of this material.
3. according to the preparation method of the described high-performance stratiform of claim 2 solid solution lithium electricity positive electrode, it is characterized in that: Mn in the presoma, Ni, the mol ratio of Co is 52-54:13:13.
4. according to the preparation method of the described high-performance stratiform of claim 2 solid solution lithium electricity positive electrode, it is characterized in that: described nickel salt is Ni(NO
3)
26H
2O, NiSO
46H
2O, Ni(CH
3COO)
24H
2Among the O one or more; Described manganese salt is Mn(NO
3)
2, MnSO
4H
2O, Mn(CH
3COO)
2H
2Among the O one or more; Described cobalt salt is Co(NO
3)
26H
2O, CoSO
47H
2O, Co(CH
3COO)
24H
2O etc.
5. according to the preparation method of the described high-performance stratiform of claim 2 solid solution lithium electricity positive electrode, it is characterized in that: described precipitation reagent is hydroxide or carbonate.
6. according to the preparation method of the described high-performance stratiform of claim 5 solid solution lithium electricity positive electrode, it is characterized in that: described precipitation reagent is NaOH, NH
4Among OH, KOH, the LiOH one or more.
7. according to the preparation method of the described high-performance stratiform of claim 2 solid solution lithium electricity positive electrode, it is characterized in that: described step 2) in the process of preparation presoma, the temperature of reaction system is 55 ℃, and the pH value is 10.0.
8. according to the preparation method of the described high-performance stratiform of claim 2 solid solution lithium electricity positive electrode, it is characterized in that: described lithium salts is a kind of in lithium hydroxide, lithium carbonate or the lithium nitrate; Hybrid mode is a kind of of dry blend wet mixing.
9. according to the preparation method of the described high-performance stratiform of claim 2 solid solution lithium electricity positive electrode, it is characterized in that: described step) substep sintering in 4, once sintered scheme is that 500 ℃ of insulation 4h rise to 750 ℃ of insulation 6h then; Double sintering is 850 ℃ of insulation 12h, and hot stage is logical oxygen all.
10. according to the preparation method of the described high-performance stratiform of claim 2 solid solution lithium electricity positive electrode, it is characterized in that: described finishing refers to material is coated, and coating material is V
2O
5, LiV
3O
8, TiO
2, AlF
3, Al
2O
3, Co
3(PO
4)
2And C coats.
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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 |
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