CN109273709A - A kind of preparation method of nickel-cobalt-manganese ternary oxide - Google Patents
A kind of preparation method of nickel-cobalt-manganese ternary oxide Download PDFInfo
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- CN109273709A CN109273709A CN201810872486.6A CN201810872486A CN109273709A CN 109273709 A CN109273709 A CN 109273709A CN 201810872486 A CN201810872486 A CN 201810872486A CN 109273709 A CN109273709 A CN 109273709A
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- cobalt
- nickel
- ternary oxide
- manganese ternary
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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
- 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
- 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
Abstract
The invention discloses a kind of preparation methods of nickel-cobalt-manganese ternary oxide, comprising the following steps: is calcined in air or oxygen atmosphere using the co-precipitation hydroxide precursor of nickel cobalt manganese and obtains nickel-cobalt-manganese ternary oxide, the calcination operation carries out in rotary kiln.The calcination temperature is 450~600 DEG C, and the time is 0.5~3.5h.Axially disposed multiple backgauge board groups on the rotary kiln inner wall, each backgauge board group include circumferential equally distributed muti-piece striker plate, and the rotary kiln for being divided into different warm areas by the backgauge board group.Compared with prior art, the present invention program has easy to operate, high-efficient, low power consumption and other advantages.
Description
Technical field
The present invention relates to new energy materials production fields, and in particular to a kind of preparation method of nickel-cobalt-manganese ternary oxide.
Background technique
In today that global pollution is on the rise, developing green clean energy resource is particularly important.Lithium ion battery due to
The advantages that it has high-energy density, height ratio capacity and has extended cycle life, becomes the first choice of current electronic product power source.Nickel
Cobalt-manganese ternary positive electrode is due to having the advantages that height ratio capacity, cheap and preferable environment friendly, it has also become most
One of anode material for lithium ion battery with high power capacity of prospect.Nickel-cobalt-manganternary ternary anode material has price low, while there is height to put
The advantages that electric specific capacity and energy density.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of uniformity of temperature profile, material is heated evenly, sintering time
Controllable and the nickel-cobalt-manganese ternary oxide of high production efficiency preparation method.
In order to solve the above-mentioned technical problem, a kind of the technical solution adopted by the present invention are as follows: system of nickel-cobalt-manganese ternary oxide
Preparation Method, comprising the following steps: calcined in air or oxygen atmosphere using the co-precipitation hydroxide precursor of nickel cobalt manganese
To nickel-cobalt-manganese ternary oxide, the calcination operation carries out in rotary kiln.
Further, the rotary kiln is ceramic liner rotary kiln, it is preferable that the ceramics are multiple based on aluminium oxide
Close the ceramics of formula.
Further, axially disposed multiple backgauge board groups on the rotary kiln inner wall, each backgauge board group include circumferential
Equally distributed muti-piece striker plate, the rotary kiln for being divided into different warm areas by the backgauge board group.
Further, the calcination temperature is 450~600 DEG C, and the time is 0.5~3.5h.
Further, the rotary kiln includes preheating zone, heat tracing zone and cooling zone.
Further, the preheating zone temperature of the rotary kiln is 200~400 DEG C, when heating a length of 0.3~0.5h；Heating
Heat preservation zone temperature is 400~550 DEG C, when heating a length of 0.4~3.0h；The cooling zone temperature is 150~350 DEG C.
The beneficial effects of the present invention are: the present invention program preparation method, it can be achieved that nickel-cobalt-manganese ternary oxide it is uniform
Efficiently preparation, avoid in Material Manufacturing Process cause oxygen demand to increase because moisture is excessively high, the heat proof material in track, SiC
The defects of seriously corroded of heat-generating pipe etc., the present invention has not only saved production, cost of investment, but also product homogeneity is good, avoids
Introducing new impurity.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph under the different multiplying of nickel-cobalt-manganese ternary oxide made from the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph under the different multiplying of nickel-cobalt-manganese ternary oxide made from the embodiment of the present invention 2；
Fig. 3 is the scanning electron microscope (SEM) photograph under the different multiplying of nickel-cobalt-manganese ternary oxide made from the embodiment of the present invention 3.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, below in conjunction with embodiment and cooperate attached
Figure is explained.
A kind of preparation method of nickel-cobalt-manganese ternary oxide, comprising the following steps: utilize the co-precipitation hydroxide of nickel cobalt manganese
Object presoma is calcined in air or oxygen atmosphere and obtains nickel-cobalt-manganese ternary oxide, the calcination operation in rotary kiln into
Row.
As can be seen from the above description, the beneficial effects of the present invention are: the present invention program preparation method is, it can be achieved that nickel cobalt manganese three
The efficient preparation of first oxide, avoid cause oxygen demand to increase because moisture is excessively high, the heat proof material in track, SiC fever
The defects of seriously corroded of pipe etc., the present invention program have not only saved production cost, but also avoid and introduce new impurity.
Further, the rotary kiln is ceramic liner rotary kiln, it is preferable that the ceramics are multiple based on aluminium oxide
Close the ceramics of formula.
As can be seen from the above description, the beneficial effects of the present invention are: ceramic liner rotary kiln is used, so that the nickel cobalt of production
Manganese ternary oxidation magnetic foreign body content it is lower, used in routine techniques high-temperature steel liner rotary kiln common metal foreign matter for
1100-1500ppb, and the present invention program can be down to 10ppb using ceramic liner rotary kiln magnetic foreign body, while ceramics is wear-resisting
6 times higher than steel of degree or more.The anticorrosive high temperature resistant refractory material such as mullite, zirconium oxide and three oxygen can be added in the ceramics
Change two aluminium compounding.
Further, axially disposed multiple backgauge board groups on the rotary kiln inner wall, each backgauge board group include circumferential
Equally distributed muti-piece striker plate, the rotary kiln for being divided into different warm areas by the backgauge board group.
Further, the calcination temperature is 450~600 DEG C, and the time is 0.5~3.5h.
Further, the rotary kiln includes preheating zone, heat tracing zone and cooling zone.
Further, the preheating zone temperature of the rotary kiln is 200~500 DEG C, when heating a length of 0.3~0.5h；Heating
Heat preservation zone temperature is 450~550 DEG C, when heating a length of 0.4~3.0h；The cooling zone temperature is 250~350 DEG C.
As can be seen from the above description, the beneficial effects of the present invention are: the heat tracing zone temperature section control of rotary kiln, hydrogen
The decomposition reaction of oxide is more complete, and oxidation is uniform, while more energy saving.
The embodiment of the present invention one are as follows: a kind of preparation method of nickel-cobalt-manganese ternary oxide, specifically includes the following steps: sharp
With the co-precipitation hydroxide precursor (molar ratio of nickel cobalt manganese is 5:2:3) of nickel cobalt manganese, calcining obtains nickel cobalt manganese three in air
First oxide, the calcination operation carry out in rotary kiln.The rotary kiln be aluminum oxide based on compound prescription pottery
Porcelain liner rotary kiln.
The rotary kiln includes preheating zone, heat tracing zone and cooling zone.For being returned to presoma thermal dehydration processing
The preheating zone temperature of rotary kiln is 200 DEG C, when heating a length of 0.3h；Heat tracing zone temperature is 550 DEG C, when heating a length of 0.4h；
The cooling zone temperature is 250 DEG C.
The embodiment of the present invention two are as follows: a kind of preparation method of nickel-cobalt-manganese ternary oxide, the difference with embodiment one is only
Be: the heating temperature of rotary kiln is different, specifically: the preheating zone temperature of the rotary kiln for handling oxidation of precursor is
300 DEG C, when heating a length of 0.5h；Heat tracing zone temperature is 400 DEG C, when heating a length of 2.5h；The cooling zone temperature is 300
℃。
The embodiment of the present invention three are as follows: a kind of preparation method of nickel-cobalt-manganese ternary oxide, the difference with embodiment one is only
Be: the heating temperature of rotary kiln is different, specifically: the preheating zone temperature of the rotary kiln for handling oxidation of precursor is
400 DEG C, when heating a length of 0.3h；Heat tracing zone temperature is 500 DEG C, when heating a length of 2h；The cooling zone temperature is 150
℃。
Electron microscope characterization is scanned to nickel-cobalt-manganese ternary oxide made from Examples 1 to 3, as a result successively such as Fig. 1~3
It is shown, it can be seen from the figure that nickel-cobalt-manganese ternary oxide shape made from the present invention program is regular, it is substantially in ball-type, size
Distribution is more concentrated.
Laser particle analyzer, tap density meter, specific surface instrument are passed through to nickel-cobalt-manganese ternary oxide made from Examples 1 to 3
(Brunauer Emmett Teller) and inductive coupling plasma spectrometer (ICP) carry out partial size, tap density (Tap
Density, TD), the content of specific surface area and nickel cobalt manganese carry out characterization measurement, as a result as shown in table 1 below:
1 partial size of table, tap density, and nickel cobalt manganese content test result table more long-pending than table table
Impurity content in nickel-cobalt-manganese ternary oxide made from Examples 1 to 3 is measured by ICP, as a result such as
Shown in the following table 2:
2 impurity content measurement result table of table
From table 2 it can be seen that impurity content is extremely low in nickel-cobalt-manganese ternary oxide made from the method for the present invention, and magnetic different
Object content is only 9ppb.
The embodiment of the present invention four are as follows: a kind of preparation method of nickel-cobalt-manganese ternary oxide, the difference with embodiment one is only
Be: in the co-precipitation hydroxide precursor of cobalt manganese, the molar ratio of nickel cobalt manganese is 6:2:2, using made from the method for the present invention
Magnetic foreign body content is only 8ppb in nickel-cobalt-manganese ternary oxide.
The embodiment of the present invention five are as follows: a kind of preparation method of nickel-cobalt-manganese ternary oxide, the difference with embodiment one is only
Be: in the co-precipitation hydroxide precursor of cobalt manganese, the molar ratio of nickel cobalt manganese is 8:1:1, using made from the method for the present invention
Magnetic foreign body content is only 8ppb in nickel-cobalt-manganese ternary oxide.
In conclusion a kind of preparation method of nickel-cobalt-manganese ternary oxide provided by the invention, has easy to operate, efficiency
High, low power consumption and other advantages.
Calcination temperature alleged by the present invention is 450~600 DEG C, and the time is that 0.5~3.5h refers in the calcination of not partition heating
Time and temperature.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright specification and accompanying drawing content are applied directly or indirectly in relevant technical field, similarly include
In scope of patent protection of the invention.
Claims (7)
1. a kind of preparation method of nickel-cobalt-manganese ternary oxide, it is characterised in that: the following steps are included: utilizing the coprecipitated of nickel cobalt manganese
Shallow lake hydroxide precursor calcines in air or oxygen atmosphere and obtains nickel-cobalt-manganese ternary oxide, and the calcination operation is turning round
It is carried out in kiln.
2. the preparation method of nickel-cobalt-manganese ternary oxide according to claim 1, it is characterised in that: the rotary kiln is pottery
Porcelain liner rotary kiln.
3. the preparation method of nickel-cobalt-manganese ternary oxide according to claim 2, it is characterised in that: the ceramics are with oxygen
The ceramics of compound prescription based on change aluminium.
4. the preparation method of nickel-cobalt-manganese ternary oxide according to claim 1, it is characterised in that: the rotary kiln inner wall
Upper axially disposed multiple backgauge board groups, each backgauge board group include circumferential equally distributed muti-piece striker plate.
5. the preparation method of nickel-cobalt-manganese ternary oxide according to claim 1, it is characterised in that: the calcination temperature is
450~600 DEG C, the time is 0.5~3.5h.
6. the preparation method of nickel-cobalt-manganese ternary oxide according to claim 1, it is characterised in that: the rotary kiln includes
Preheating zone, heat tracing zone and cooling zone.
7. the preparation method of nickel-cobalt-manganese ternary oxide according to claim 6, it is characterised in that: preheating zone temperature is
200~400 DEG C, when heating a length of 0.3~0.5h；Heat tracing zone temperature is 400~550 DEG C, when heating a length of 0.4~
3.0h；The cooling zone temperature is 150~350 DEG C.
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| CN201810872486.6A CN109273709A (en) | 2018-08-02 | 2018-08-02 | A kind of preparation method of nickel-cobalt-manganese ternary oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110444756A (en) * | 2019-08-19 | 2019-11-12 | 湖南金富力新能源股份有限公司 | The anode material for lithium-ion batteries and preparation method that are prepared with pyroreaction device and application |
| CN110534737A (en) * | 2019-09-16 | 2019-12-03 | 江西省科学院应用化学研究所 | A kind of high magnification doping type nickel-cobalt-manganese ternary material and preparation method thereof |
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| CN105680038A (en) * | 2016-04-22 | 2016-06-15 | 柳州凯通新材料科技有限公司 | Method for synthesizing LiNixCoyMn1-x-yO2 anode material with sol-gel process |
| CN105870414A (en) * | 2016-04-22 | 2016-08-17 | 柳州凯通新材料科技有限公司 | Process for synthesizing lithium nickel manganese cobalt positive electrode material by co-precipitation method |
| CN106091677A (en) * | 2016-02-01 | 2016-11-09 | 长兴鼎力窑炉设备厂 | Heating ceramic inner bag rotary furnace in a kind of |
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Patent Citations (4)
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| CN102709541A (en) * | 2012-04-06 | 2012-10-03 | 杭州金马能源科技有限公司 | Method for preparing high-density lithium ion battery anode material-lithium nickel manganese cobalt and special calcinator |
| CN106091677A (en) * | 2016-02-01 | 2016-11-09 | 长兴鼎力窑炉设备厂 | Heating ceramic inner bag rotary furnace in a kind of |
| CN105680038A (en) * | 2016-04-22 | 2016-06-15 | 柳州凯通新材料科技有限公司 | Method for synthesizing LiNixCoyMn1-x-yO2 anode material with sol-gel process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110444756A (en) * | 2019-08-19 | 2019-11-12 | 湖南金富力新能源股份有限公司 | The anode material for lithium-ion batteries and preparation method that are prepared with pyroreaction device and application |
| CN110444756B (en) * | 2019-08-19 | 2020-12-01 | 湖南金富力新能源股份有限公司 | Lithium ion battery anode material prepared by high-temperature reaction device, preparation method and application |
| CN110534737A (en) * | 2019-09-16 | 2019-12-03 | 江西省科学院应用化学研究所 | A kind of high magnification doping type nickel-cobalt-manganese ternary material and preparation method thereof |
| CN110534737B (en) * | 2019-09-16 | 2021-04-13 | 江西省科学院应用化学研究所 | High-rate doped nickel-cobalt-manganese ternary material and preparation method thereof |
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| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Li Junxiu Inventor after: Huang Bing Inventor after: Li Ke Inventor before: Li Junxiu Inventor before: Huang Bing Inventor before: Li Ke Inventor before: Wang Hangbao |
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Application publication date: 20190125 |