CN109065857A - Treatment method for reducing residual alkali on surface of high-nickel material - Google Patents
Treatment method for reducing residual alkali on surface of high-nickel material Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000000463 material Substances 0.000 title claims abstract description 70
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 65
- 239000003513 alkali Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000005253 cladding Methods 0.000 claims description 15
- 238000003672 processing method Methods 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 229910001679 gibbsite Inorganic materials 0.000 claims description 2
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 2
- 229910013100 LiNix Inorganic materials 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 8
- 229910013716 LiNi Inorganic materials 0.000 description 6
- 229910003005 LiNiO2 Inorganic materials 0.000 description 5
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910032387 LiCoO2 Inorganic materials 0.000 description 3
- 229910011328 LiNi0.6Co0.2Mn0.2O2 Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910002993 LiMnO2 Inorganic materials 0.000 description 2
- 229910013421 LiNixCoyMn1-x-yO2 Inorganic materials 0.000 description 2
- 229910013427 LiNixCoyMn1−x−yO2 Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910013292 LiNiO Inorganic materials 0.000 description 1
- 229910013485 LiNixM1-xO2 Inorganic materials 0.000 description 1
- 229910013495 LiNixM1−xO2 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
-
- 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
- H01M4/366—Composites as layered products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a treatment method for reducing residual alkali on the surface of a high nickel material, which comprises the following steps: cleaning: cleaning a high-nickel material by using a supercritical fluid; coating: coating the cleaned high nickel material; and (3) sintering: sintering at 300-800 ℃ in the atmosphere to finally prepare the low-residual-alkali high-nickel material. The supercritical fluid is utilized to clean the high nickel material, so that the drying environment in the preparation process of the high nickel material is ensured while the residual alkali on the surface of the high nickel material is effectively reduced, and the processing performance and the electrochemical performance of the high nickel material are ensured.
Description
Technical field
The invention belongs to field of lithium ion battery anode, and in particular to a kind of place for reducing high-nickel material surface residual alkali
Reason method.
Background technique
Lithium ion battery has as new cleaning fuel in the increasingly prominent contemporary society of environmental problem more and more extensive
Application.With the development of the society, the demand of people's lighter, longer life expectancy lithium ion battery to quality is increasingly urgent.Lithium from
The improvement of sub- battery performance is critical to start with from its electrode material, and positive electrode specific capacity, which has become, promotes lithium ion battery ratio
One of key factor of energy.
In currently used several layered cathode materials, LiCoO2Multiplying power and cycle performance it is excellent, simple production process,
But it is expensive, seriously pollutes environment, and anti-over-charging performance is poor, there are security risks；LiNiO2Capacity it is high, cost
It is low, it is environmental-friendly, but its synthesis condition is harsh, and structural stability is poor, and there are lithium nickel mixing phenomenons to lead to cycle performance in crystal
It is poor；LiMnO2With high capacity, advantages of environment protection, but structural instability is easy to be changed into spinel structure.Have
The ternary system positive electrode LiNi of layer structurexCoyMn1-x-yO2, this positive electrode is by LiCoO2, LiNiO2, LiMnO2Three
The advantages of kind stratified material, is combined together, and the cycle performance that existing high capacity has had again compares LiCoO2It is cheap, performance
Better than each one-component positive electrode, there are apparent trielement synergistic effects.
But ternary system positive electrode LiNixCoyMn1-x-yO2It is higher (x >=0.6) that there is also disadvantage, especially nickel contents
Material in air be easy and CO2And H2O reacts, and generates LiOH and Li on the surface of the material2CO3, referred to as surface is residual
Alkali.The alkali compounds on positive electrode surface is mainly derived from two aspects, and one is in actual production process, because of lithium
Salt has certain volatilization in high-temperature burning process, and when ingredient can improve Li/M ratio (i.e. lithium salts is suitably excessive) slightly to make up
It is lost caused by sintering process, therefore how much can all have a small amount of Li residue (at high temperature with Li2The form presence of O)；Two
It is that temperature is reduced to Li after room temperature2O can adsorb the CO in air2And H2O and form LiOH and Li2CO3Deng.
Ternary system positive electrode LiNixCoyMn1-x-yO2Surface residual alkali too high levels can be brought to chemical property it is all
More negative effects.It is that it will affect coating first, NCA and rich nickel ternary material are readily formed g., jelly-like in homogenization process,
It is mainly exactly because caused by the basic anhydride content too high water absorption on their surfaces；Next, which is embodied in, increases the irreversible of battery
Capacitance loss, while deteriorating cycle performance.
What domestic manufacturer generallyd use at present is washed to high-nickel material, then in lower temperature double sintering
Technique reduces the surface residual alkali content of high-nickel material, this method surface residual alkali can be cleaned ratio more thoroughly, but its disadvantage
Hold also clearly: high-nickel material multiplying power and cycle performance after such as handling are decreased obviously, and seriously constrain high-nickel material
Large-scale application.
Summary of the invention
Aiming at the shortcomings in the prior art, the present invention provides it is a kind of reduce high-nickel material surface residual alkali processing method,
High-nickel material is cleaned using supercritical fluid, cladding processing is carried out to the high-nickel material after cleaning, what is be finally sintered is low
The high-nickel material of surface residual alkali guarantees in high-nickel material preparation process while high-nickel material surface residual alkali is effectively reduced
Dry environment ensure that the processing performance and chemical property of high-nickel material.
The present invention to achieve the goals above, using following technical scheme:
A kind of processing method reducing high-nickel material surface residual alkali, comprising the following steps:
(1) it cleans: high-nickel material being cleaned using supercritical fluid；
(2) it coats: the high-nickel material after cleaning is coated；
(3) be sintered: in atmosphere, 300 ~ 800 DEG C are sintered the high-nickel material that low residual alkali is finally made.
Further scheme, the chemical molecular formula of the high-nickel material are as follows: LiNixM1-xO2, wherein 0.6≤x≤1.0, M choosing
It is one or more of from Co, Mn, Al, Mg.
Further scheme, the supercritical fluid are carbon dioxide, methanol, water or chlorofluorocarbons.
Preferably, the supercritical fluid is carbon dioxide.
Further scheme, the cleaning process is that high-nickel material is placed in the extraction kettle equipped with supercritical fluid, in room
Under conditions of temperature, 8 ~ 35MPa, clean 0.1 ~ 0.5 hour, at least cleaning is primary.
Further scheme, the cladding process are after the completion of high-nickel material cleans, to squeeze into packet in extraction kettle partial volume auxiliary pump
Object processing agent solution is covered, carries out cladding processing with supercritical fluid, under conditions of room temperature, 8 ~ 35MPa, processing 0.1 ~ 0.5 is small
When, at least cladding processing is primary.
Further scheme, the coating processing agent solution are the solution or suspension of nanometer coating.
Preferably, the nanometer coating is Al2O3、ZrO2、CeO2、TiO2、MgO、B2O3、ZnO、LiF、AlF3、Li3PO4、
Al(OH)3One or more of, the mass percent that dosage accounts for the high-nickel material is 0.01% ~ 0.4%.
Preferably, the solvent of the coating processing agent solution is one or more of ethyl alcohol, water, methanol.
Further scheme, the atmosphere are compression drying air or oxygen.
Compared with prior art, the invention has the following advantages: the method that the present invention uses can reduce rapidly it is nickelic
Material surface residual alkali does not use traditional washing conditions to material comprising cladding treatment process using supercritical fluid extraction technique
Expect just washing process, it is ensured that the dry environment in high-nickel material preparation process can effectively improve the processing of high-nickel material
Performance and chemical property.
Detailed description of the invention
Fig. 1 is the SEM pattern comparison diagram of 1 surface residual alkali of embodiment high-nickel material before and after the processing.
Fig. 2 is under the residual alkali button cell 1C multiplying power that high-nickel material is assembled into respectively before and after the processing in surface in embodiment 1
Cycle performance comparison diagram.
Specific embodiment
Further clear and complete explanation is done to technical solution of the present invention with specific embodiment with reference to the accompanying drawing.
Embodiment 1
High-nickel material used in the present embodiment is LiNi0.85Co0.1Mn0.05O2, surface residual alkali processing step is as follows:
(1) it cleans: by high-nickel material LiNi0.85Co0.1Mn0.05O2It is placed in equipped with supercritical CO2Extraction kettle in, room temperature,
It under conditions of 10MPa, cleans 0.2 hour, repeats above-mentioned cleaning process 3 times；
(2) it coats: squeezing into Al in extraction kettle partial volume auxiliary pump2O3Aqueous solution, use supercritical CO2Cladding processing is carried out, in room
Temperature under conditions of 10MPa, handles 0.2 hour, wherein Al2O3Dosage account for high-nickel material LiNi0.85Co0.1Mn0.05O2Quality hundred
Divide the 0.2% of ratio, repeat above-mentioned cladding process 2 times,；
(3) be sintered: by treated, powder is heated to 600 DEG C in oxygen atmosphere, keeps the temperature 5 hours, then natural cooling, final
To the high-nickel material LiNi of low residual alkali0.85Co0.1Mn0.05O2。
Embodiment 2
High-nickel material used in the present embodiment is LiNi0.6Co0.2Mn0.2O2, surface residual alkali processing step is as follows:
(1) it cleans: by high-nickel material LiNi0.6Co0.2Mn0.2O2Be placed in the extraction kettle equipped with supercritical methanol, room temperature,
It under conditions of 20MPa, cleans 0.1 hour, repeats above-mentioned cleaning process 2 times；
(2) it coats: squeezing into extraction kettle partial volume auxiliary pump containing Al2O3、ZrO2And TiO2Ethanol solution, use supercritical CO2Into
The processing of row cladding is handled 0.1 hour, wherein Al under conditions of room temperature, 20MPa2O3、ZrO2And TiO2Dosage account for nickelic material
Expect LiNi0.6Co0.2Mn0.2O2The 0.4% of mass percent, cladding processing 1 time；
(3) be sintered: by treated, powder is heated to 300 DEG C in oxygen atmosphere, keeps the temperature 5 hours, then natural cooling, final
To the high-nickel material LiNi of low residual alkali0.6Co0.2Mn0.2O2。
Embodiment 3
High-nickel material used in the present embodiment is LiNiO2, surface residual alkali processing step is as follows:
(1) it cleans: by high-nickel material LiNiO2It is placed in equipped with supercritical CO2Extraction kettle in, under conditions of room temperature, 35MPa,
Cleaning 0.5 hour, cleaning are primary；
(2) it coats: squeezing into Al (OH) in extraction kettle partial volume auxiliary pump3Aqueous solution, use supercritical CO2Cladding processing is carried out,
Under conditions of room temperature, 35MPa, handle 0.5 hour, wherein Al (OH)3Dosage account for high-nickel material LiNiO2Mass percent
0.3%, cladding processing is primary；
(3) be sintered: by treated, powder is heated to 800 DEG C in compression drying air, keeps the temperature 5 hours, then natural cooling,
Finally obtain the high-nickel material LiNiO of low residual alkali2。
Embodiment 4
High-nickel material used in the present embodiment is LiNi0.65Co0.15Mg0.2O2, surface residual alkali processing step is as follows:
(1) it cleans: by high-nickel material LiNi0.65Co0.15Mg0.2O2It is placed in equipped with overcritical H2In the extraction kettle of O, room temperature,
Under conditions of 8MPa, clean 0.3 hour, repeated washing 4 times；
(2) it coats: squeezing into extraction kettle partial volume auxiliary pump containing Al2O3、B2O3Ethanol solution, with overcritical H2O is coated
Processing is handled 0.3 hour, wherein Al under conditions of room temperature, 8MPa2O3And B2O3Dosage account for high-nickel material
LiNi0.65Co0.15Mn0.2O2The 0.01% of mass percent, repeats cladding 3 times；
(3) be sintered: by treated, powder is heated to 750 DEG C in oxygen atmosphere, keeps the temperature 5 hours, then natural cooling, final
To the high-nickel material LiNi of low residual alkali0.65Co0.15Mn0.2O2。
By the high-nickel material LiNi before being handled in embodiment 10.85Co0.1Mn0.05O2With treated high-nickel material
LiNi0.85Co0.1Mn0.05O2Its surface topography, the result is shown in Figure 1 are observed with scanning electron microscope respectively.
Again by the high-nickel material LiNi before processing0.85Co0.1Mn0.05O2With treated high-nickel material
LiNi0.85Co0.1Mn0.05O2It is assembled into button cell respectively, charge and discharge are carried out within the scope of 3.0V ~ 4.3V, observe its 1C multiplying power
The cycle performance of lower battery, is as a result shown in Fig. 2.
According to the scanning electron microscope comparison diagram of surface residual alkali before and after the processing (referring to Fig. 1), it can be seen that pass through this hair
After bright method processing, the surface residual alkali of high-nickel material is significantly reduced.
According to fig. 2, it can be seen that using technical solution of the present invention treated button cell that high-nickel material is assembled into,
Its cycle performance of battery is improved significantly.
This hair can be understood and applied the above description of the embodiments is intended to facilitate those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to implementations here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (10)
1. a kind of processing method for reducing high-nickel material surface residual alkali, it is characterised in that: the following steps are included:
(1) it cleans: high-nickel material being cleaned using supercritical fluid；
(2) it coats: the high-nickel material after cleaning is coated；
(3) be sintered: in atmosphere, 300 ~ 800 DEG C are sintered the high-nickel material that low residual alkali is finally made.
2. processing method as described in claim 1, it is characterised in that: the chemical molecular formula of the high-nickel material are as follows: LiNixM1- xO2, wherein 0.6≤x≤1.0, M are one or more of in Co, Mn, Al, Mg.
3. processing method as described in claim 1, it is characterised in that: the supercritical fluid is carbon dioxide, methanol, water
Or chlorofluorocarbons.
4. processing method as claimed in claim 3, it is characterised in that: the supercritical fluid is carbon dioxide.
5. processing method as described in claim 1, it is characterised in that: the cleaning process is to be placed in high-nickel material equipped with super
In the extraction kettle of critical fluids, under conditions of room temperature, 8 ~ 35MPa, clean 0.1 ~ 0.5 hour, at least cleaning is primary.
6. processing method as described in claim 1, it is characterised in that: after the completion of the cladding process is high-nickel material cleaning,
Squeezed into extraction kettle partial volume auxiliary pump coating processing agent solution, carry out cladding processing with supercritical fluid, room temperature, 8 ~
Under conditions of 35MPa, handle 0.1 ~ 0.5 hour, at least cladding processing is primary.
7. processing method as claimed in claim 6, it is characterised in that: the coating processing agent solution is nanometer coating
Solution or suspension.
8. processing method as claimed in claim 7, it is characterised in that: the nanometer coating is Al2O3、ZrO2、CeO2、
TiO2、MgO、B2O3、ZnO、LiF、AlF3、Li3PO4、Al(OH)3One or more of, dosage accounts for the matter of the high-nickel material
Measuring percentage is 0.01% ~ 0.4%.
9. such as the described in any item processing methods of claim 6 ~ 8, it is characterised in that: the solvent of the coating processing agent solution
For one or more of ethyl alcohol, water, methanol.
10. processing method as described in claim 1, it is characterised in that: the atmosphere is compression drying air or oxygen.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110040791A (en) * | 2019-04-30 | 2019-07-23 | 合肥国轩高科动力能源有限公司 | Ternary cathode material and preparation method thereof |
| CN111916725A (en) * | 2019-05-08 | 2020-11-10 | 中国石油化工股份有限公司 | Phosphorus-doped lithium battery high-nickel positive electrode material and preparation process thereof |
| CN112072083A (en) * | 2020-07-28 | 2020-12-11 | 昆明理工大学 | Modified high-nickel material and preparation method thereof |
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Application publication date: 20181221 |