CN109671924A - A kind of preparation method of nickel-cobalt-manganternary ternary anode material - Google Patents
A kind of preparation method of nickel-cobalt-manganternary ternary anode material Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H—ELECTRICITY
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- 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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- 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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Abstract
A kind of preparation method of nickel-cobalt-manganternary ternary anode material, it is characterised in that: be passed through carbon dioxide and oxygen mixture into reaction unit, nickel cobalt manganese mixed solution is added, control reaction solution pH is 9.5 ~ 10.5, and the core of nickel-cobalt-manganese ternary presoma is prepared at 75 ~ 95 DEG C；Reaction temperature is adjusted to 45 ~ 65 DEG C, reaction solution pH to 11.5 ~ 12.5 is adjusted after crystallization；Nickel cobalt manganese mixed solution and enveloping agent solution are added, control reaction solution pH is 11.5 ~ 12.5, and reaction temperature is 45 ~ 65 DEG C, prepares the shell of nickel-cobalt-manganese ternary presoma；By the aged equal post-processing of product, the nickel-cobalt-manganese ternary presoma of compound α Yu β type core-shell structure are obtained；Again with lithium hydroxide ball milling mixing, high temperature sintering obtains pre-burning tertiary cathode material；High temperature sintering obtains nickel-cobalt-manganternary ternary anode material again.The capacity of positive electrode prepared by the present invention is good, and repeatedly capacity retention ratio is higher after circulation, and chemical property is prominent.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of preparation side of nickel-cobalt-manganternary ternary anode material
Method.
Background technique
General tertiary cathode material is secondary spherical particle and hydrogen made of being reunited as nickel cobalt manganese hydroxide small grains
It is calcined after lithia mixing.However, being had the following problems for nickelic tertiary cathode material especially secondary spherical particle:
1, in nickelic tertiary cathode material sintering process, sintering temperature is lower, causes Li ion insertion speed slower, slightly for granularity
Big secondary ball particle, since primary particle accumulates densification, lithium is difficult to burn into inside particle, and particle inside and outside is caused to melt lithium not
, cause positive electrode remnants lithium higher, capacity is relatively low, i.e. the processing performance of ternary precursor is bad；2, ternary is generally used
After multiple charge and discharge cycles, the capacity of battery, cycle performance, security performance reduce the battery of positive electrode.Mainly due to
Following reason: the charge and discharge process of battery is really the insertion abjection due to Li ion in positive electrode, is from microcosmic angle
Positive electrode is deviate from continuous insertion of the Li ion in positive electrode, and positive electrode lattice dilation therewith, volume is not
Disconnected variation, constantly changes being macroscopically embodied in the primary particle volume for forming secondary ball particle, since anisotropy is led
It causes stress between primary particle constantly to increase, small crack is gradually formed between primary particle, small crack is gradually increased, and is eventually led to secondary
The rupture of ball particle.Positive electrode and electrolyte contacts area increase after secondary ball breakage of particles, between positive electrode and electrolyte
SEI film is formed again, and positive electrode increases with electrolyte side reaction.Causing battery capacity reduces, and cycle performance is deteriorated, safety
The series of problems such as energy reduction.
Summary of the invention
In view of the above technical deficiency, it is an object of that present invention to provide a kind of preparation sides of nickel-cobalt-manganternary ternary anode material
Method.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of preparation side of nickel-cobalt-manganternary ternary anode material
Method successively includes the following steps:
Step (1), the gaseous mixture of carbon dioxide and oxygen is passed through into reaction unit, nickel cobalt manganese is at the uniform velocity added into reaction unit
Mixed solution, while it is 9.5 ~ 10.5 that aqueous slkali, which is added, to control the pH value of the reaction solution in the reaction unit, the process that feeds intake is strong
Strong stirring, and the core of the nickel-cobalt-manganese ternary presoma of core-shell structure is prepared under 75 ~ 95 DEG C of reaction temperatures, which is α type structure
Nickel-cobalt-manganese ternary presoma；
Step (2) suspends liquid feeding, the gaseous mixture is switched to nitrogen, adjusts temperature in the reaction unit to 45 ~ 65
DEG C, after crystallization 1 ~ 2 hour, the pH value of aqueous slkali adjustment reaction solution is added to 11.5-12.5；
Step (3), then the reaction is added in the nickel cobalt manganese mixed solution and enveloping agent solution in a manner of at the uniform velocity cocurrent respectively
In device, while it is 11.5 ~ 12.5 that aqueous slkali, which is added, to control the pH value of the reaction solution in the reaction unit, and the process that feeds intake is strong
Stirring, control reaction temperature are 45 ~ 65 DEG C, and reaction prepares the nickel-cobalt-manganese ternary forerunner of core-shell structure under nitrogen atmosphere protection
The shell of body, the shell are the nickel-cobalt-manganese ternary presoma of β type structure；
Step (4), the product that the step (3) is obtained is aged, solid-liquor separation, washing and drying process, obtain compound α with
The nickel-cobalt-manganese ternary presoma of β type core-shell structure；
Step (5), the nickel-cobalt-manganese ternary presoma and lithium hydroxide ball milling mixing of the core-shell structure that the step (4) is obtained,
Wherein nickel cobalt manganese three summation and the molar ratio of lithium hydroxide are 1:1.05 in the nickel-cobalt-manganese ternary presoma of the core-shell structure,
It is sintered 6 ~ 10 hours for 400 ~ 600 DEG C in air atmosphere, obtains pre-burning tertiary cathode material；
Step (6), the pre-burning tertiary cathode material that the step (5) is obtained 700 ~ 900 DEG C of high temperature sinterings under oxygen atmosphere
20 ~ 30 hours, obtain nickel-cobalt-manganternary ternary anode material.
Preferably, in the step (1) and step (3), the nickel salt in the nickel cobalt manganese mixed solution be sulfate,
At least one of nitrate and chloride, cobalt salt are at least one of sulfate, nitrate and chloride, and manganese salt is
At least one of sulfate, nitrate and chloride, Ni in nickel cobalt manganese mixed solution2+:(Co2++Mn2+) molar ratio be
2.33~7.33:1。
Preferably, the volumetric concentration of carbon dioxide is 10 ~ 20% in the gaseous mixture, dioxy in the step (1)
The molar ratio for changing carbon and cobalt ions and manganese ion sum of the two is 0.5 ~ 1:1.
Preferably, in the step (1), nickel ion is divalent in the core, and the valence state of cobalt ions and manganese ion is equal
For trivalent, general formula is [Ni2+ 1−x-yCo3+ x Mn3+ y(OH)2]CO3 2- (x+y)/2, wherein 0.17≤(x+y)≤0.33.
Preferably, the valence state of nickel ion, cobalt ions and manganese ion is divalent in the shell in the step (3),
Its general formula is Ni2+ 1-x-yCo2+ xMn2+ y(OH)2, wherein 0.17≤(x+y)≤0.33.
Preferably, the complexing agent is in ammonium hydroxide, ammonium sulfate, ammonium nitrate and ammonium chloride in the step (3)
At least one, it is 1-2mol/L that complexing agent controls ammonia content in reaction solution.
Preferably, the speed of stirring is 100 ~ 300rpm in the step (1).
Preferably, the speed of stirring is 300 ~ 600rpm in the step (3).
Preferably, the aqueous slkali is sodium hydroxide solution in the step (1), step (2) and step (3)
Or potassium hydroxide solution.
Design feature and beneficial effect of the invention is: the compound α and β type nickel cobalt manganese of elder generation's synthesis core shell structure of the present invention
Ternary precursor, then by the compound α and the sintering of β type nickel-cobalt-manganese ternary presoma in tertiary cathode material.This kind of compound α and β type
The nickel-cobalt-manganese ternary presoma of core-shell structure due to being loose α type hydroxide particles inside its particle, outside for accumulation compared with
Fine and close β type hydroxide is obtained after sintering with the nickel-cobalt-manganternary ternary anode material after bearing structure.The presoma sintering
Processing performance is more preferable, and remaining lithium is lower after being embodied in sintering.The more general positive electrode performance of positive electrode is more excellent, tool
Body surface is now since secondary ball particle internal voids are more, and lithium ion transition is more unobstructed, crystal is ruptured as caused by anisotropy
It reduces, therefore the capacity of the positive electrode is good, repeatedly capacity retention ratio is higher after circulation, and chemical property is prominent.
Detailed description of the invention
Fig. 1 is the XRD diagram of embodiment and comparative example ternary precursor；
Fig. 2 is that embodiment and comparative example presoma section SEM scheme；
Fig. 3 is embodiment and 100 weeks circulation volume tendency charts of comparative example.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and embodiments.
Embodiment
(1) carbon dioxide and oxygen mixture are passed through in reaction unit, wherein the volumetric concentration of carbon dioxide is 15%, two
The molar ratio of carbonoxide and cobalt manganese is 0.6:1；The nickel cobalt manganese mixed solution of 2mol/L is at the uniform velocity opened into feed liquor, wherein nickel cobalt manganese
The mole coefficient ratio of three is 78:11:11；It is 10 ± 0.1 that sodium hydroxide solution control reacting liquid pH value is added simultaneously, is fed intake
Cheng Qianglie stirring, mixing speed 200rpm, and α type nickel-cobalt-manganese ternary presoma is prepared under 80 DEG C of reaction temperatures, chemistry
Formula is [Ni2+ 0.78Co3+ 0.11 Mn3+ 0.11(OH)2]CO3 2- 0.11, the nickel cobalt of the α type nickel-cobalt-manganese ternary presoma as core-shell structure
The core of manganese ternary precursor.
(2) suspend liquid feeding, above-mentioned gaseous mixture is switched into nitrogen, adjusts the reaction unit temperature to 50 DEG C, crystallization 2 is small
Shi Hou is added sodium hydroxide solution and adjusts reacting liquid pH value to 12.
(3) by the step (1) nickel cobalt manganese mixed solution and 4mol/L ammonium nitrate solution enveloping agent solution respectively with
At the uniform velocity the reaction unit is added in cocurrent mode, and it is 1.5mol/L that wherein complexing agent controls ammonia content in reaction solution, adds simultaneously
Entering sodium hydroxide solution to control the pH value of the reaction solution in the reaction unit is 12 ± 0.1, and the process that feeds intake stirs strongly, stirring
Speed is 400rpm, and control reaction temperature is 50 DEG C, and the reaction preparation β type nickel-cobalt-manganese ternary forerunner under nitrogen atmosphere protection
Body, chemical formula Ni2+ 0.78Co2+ 0.11Mn2+ 0.11(OH)2, the nickel cobalt of the β type nickel-cobalt-manganese ternary presoma as core-shell structure
The shell of manganese ternary precursor.
(4) product obtained the step (3) is aged, solid-liquor separation, washing and drying process, obtains compound α and β
The nickel-cobalt-manganese ternary presoma of type core-shell structure.
(5) the nickel-cobalt-manganese ternary presoma for obtaining the step (4) and lithium hydroxide ball milling mixing, wherein the forerunner
Nickel cobalt manganese three summation and the molar ratio of lithium hydroxide are 1:1.05 in body, are sintered 6 hours for 500 DEG C, obtain in air atmosphere
Pre-burning tertiary cathode material.
(6) the pre-burning tertiary cathode material for obtaining the step (5) 800 DEG C of high temperature sinterings 18 under oxygen atmosphere are small
When, obtain final nickel-cobalt-manganternary ternary anode material.
It can be seen that the spy that the precursor samples that embodiment is prepared have α type and β type hydroxide in conjunction with Fig. 1 and Fig. 2
Diffraction maximum is levied, after presoma is mixed lithium roasting, gained nickel-cobalt-manganternary ternary anode material surface compact, internal defect are shown good
Good core-shell structure inheritance.
Comparative example
(1) the nickel cobalt manganese mixed nitrate solution of 2mol/L is added in a manner of at the uniform velocity cocurrent respectively with 4mol/L ammonium nitrate solution
The reaction unit, wherein the mole coefficient ratio of nickel cobalt manganese three is 78:11:11, and complexing agent controls ammonia content in reaction solution
For 1.5mol/L；It is 12 ± 0.1 that sodium hydroxide solution is added simultaneously and controls the pH value of the reaction solution in the reaction unit, is fed intake
Process stirs strongly, mixing speed 400rpm, and control reaction temperature is 50 DEG C, and the reaction preparation β under nitrogen atmosphere protection
Type nickel-cobalt-manganese ternary presoma.
(2) product obtained the step (1) is aged, solid-liquor separation, washing and drying process, obtains compound β type
The nickel-cobalt-manganese ternary presoma of core-shell structure, chemical formula Ni2+ 0.78Co2+ 0.11Mn2+ 0.11(OH)2。
(3) the nickel-cobalt-manganese ternary presoma for obtaining the step (2) and lithium hydroxide ball milling mixing, wherein the forerunner
Nickel cobalt manganese three summation and the molar ratio of lithium hydroxide are 1:1.05 in body, are sintered 6 hours for 500 DEG C, obtain in air atmosphere
Pre-burning tertiary cathode material.
(4) the pre-burning tertiary cathode material for obtaining the step (3) 800 DEG C of high temperature sinterings 18 under oxygen atmosphere are small
When, obtain final nickel-cobalt-manganternary ternary anode material.
Can be seen that the precursor samples that comparative example is prepared in conjunction with Fig. 1 and Fig. 2, there is the feature of β type hydroxide to spread out
Peak is penetrated, after presoma is mixed lithium roasting, gained nickel-cobalt-manganternary ternary anode material surface and inside solid.
Nickelic tertiary cathode material obtained in embodiment and comparative example is assembled into button cell, specific steps are as follows: will
Positive electrode, acetylene black are uniformly mixed with Kynoar (PVDF) by 94: 3: 3 mass ratioes, are stirred 2h, are uniformly coated on aluminium foil
On, rear 80 DEG C of vacuum bakeouts, tabletting cuts the positive plate that diameter is 14mm.Using the pour lithium slice of diameter 16mm as negative electrode tab, with
1mol/L LiPF6+DEC/EC (volume ratio 1: 1) mixed solution is electrolyte, using microporous polypropylene membrane as diaphragm, full of guarantor
It protects in the glove box of gas and carries out being assembled into button cell.Using LAND battery test system, in the voltage model of 2.8~4.35V
In enclosing, 25 DEG C, under the conditions of 0.2C charge and discharge, test above-mentioned button cell first discharge specific capacity and circulation volume holding in 100 weeks
Rate, test data see the table below.And it is lower in conjunction with Fig. 3 to can be seen that sample remnants lithium content in embodiment, holds after 100 circulations
It is higher to measure conservation rate, shows higher chemical property.
Table 1: embodiment and comparative example chemical property contrast table
| Sample number into spectrum | 0.2C discharges (mAh/g) for the first time | Recycle 100 capacity retention ratios (%) | Remaining lithium content (ppm) |
| Embodiment | 224 | 95.99 | 774 |
| Comparative example | 198 | 90.10 | 2268 |
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art's energy
The solution contents of the present invention much of that are simultaneously implemented accordingly, and it is not intended to limit the scope of the present invention.It is all spiritual according to the present invention
Equivalent change or modification made by essence, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of nickel-cobalt-manganternary ternary anode material, it is characterised in that: successively include the following steps:
Step (1), the gaseous mixture of carbon dioxide and oxygen is passed through into reaction unit, nickel cobalt manganese is at the uniform velocity added into reaction unit
Mixed solution, while it is 9.5 ~ 10.5 that aqueous slkali, which is added, to control the pH value of the reaction solution in the reaction unit, the process that feeds intake is strong
Strong stirring, and the core of the nickel-cobalt-manganese ternary presoma of core-shell structure is prepared under 75 ~ 95 DEG C of reaction temperatures, which is α type structure
Nickel-cobalt-manganese ternary presoma；
Step (2) suspends liquid feeding, the gaseous mixture is switched to nitrogen, adjusts temperature in the reaction unit to 45 ~ 65
DEG C, after crystallization 1 ~ 2 hour, the pH value of aqueous slkali adjustment reaction solution is added to 11.5-12.5；
Step (3), then the reaction is added in the nickel cobalt manganese mixed solution and enveloping agent solution in a manner of at the uniform velocity cocurrent respectively
In device, while it is 11.5 ~ 12.5 that aqueous slkali, which is added, to control the pH value of the reaction solution in the reaction unit, and the process that feeds intake is strong
Stirring, control reaction temperature are 45 ~ 65 DEG C, and reaction prepares the nickel-cobalt-manganese ternary forerunner of core-shell structure under nitrogen atmosphere protection
The shell of body, the shell are the nickel-cobalt-manganese ternary presoma of β type structure；
Step (4), the product that the step (3) is obtained is aged, solid-liquor separation, washing and drying process, obtain compound α with
The nickel-cobalt-manganese ternary presoma of β type core-shell structure；
Step (5), the nickel-cobalt-manganese ternary presoma and lithium hydroxide ball milling mixing of the core-shell structure that the step (4) is obtained,
Wherein nickel cobalt manganese three summation and the molar ratio of lithium hydroxide are 1:1.05 in the nickel-cobalt-manganese ternary presoma of the core-shell structure,
It is sintered 6 ~ 10 hours for 400 ~ 600 DEG C in air atmosphere, obtains pre-burning tertiary cathode material；
Step (6), the pre-burning tertiary cathode material that the step (5) is obtained 700 ~ 900 DEG C of high temperature sinterings under oxygen atmosphere
20 ~ 30 hours, obtain nickel-cobalt-manganternary ternary anode material.
2. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: in the step
(1) and in step (3), the nickel salt in the nickel cobalt manganese mixed solution is at least one in sulfate, nitrate and chloride
Kind, cobalt salt is at least one of sulfate, nitrate and chloride, and manganese salt is in sulfate, nitrate and chloride
At least one, Ni in nickel cobalt manganese mixed solution2+:(Co2++Mn2+) molar ratio be 2.33 ~ 7.33:1.
3. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: in the step
(1) in, the volumetric concentration of carbon dioxide is 10 ~ 20% in the gaseous mixture, carbon dioxide and cobalt ions and manganese ion sum of the two
Molar ratio be 0.5 ~ 1:1.
4. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: in the step
(1) in, nickel ion is divalent in the core, and the valence state of cobalt ions and manganese ion is trivalent, and general formula is [Ni2+ 1−x-yCo3+ x
Mn3+ y(OH)2]CO3 2- (x+y)/2, wherein 0.17≤(x+y)≤0.33.
5. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: in the step
(3) in, the valence state of nickel ion, cobalt ions and manganese ion is divalent, general formula Ni in the shell2+ 1-x-yCo2+ xMn2+ y
(OH)2, wherein 0.17≤(x+y)≤0.33.
6. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: in the step
(3) in, the complexing agent is at least one of ammonium hydroxide, ammonium sulfate, ammonium nitrate and ammonium chloride, and complexing agent is controlled in reaction solution
Ammonia content processed is 1-2mol/L.
7. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: in the step
(1) in, the speed of stirring is 100 ~ 300rpm.
8. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: the step (3)
In, the speed of stirring is 300 ~ 600rpm.
9. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that: in the step
(1), in step (2) and step (3), the aqueous slkali is sodium hydroxide solution or potassium hydroxide solution.
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| CN112531155A (en) * | 2019-09-17 | 2021-03-19 | 湖南杉杉新能源有限公司 | Preparation method of positive electrode material precursor and preparation method of positive electrode material |
| CN112531155B (en) * | 2019-09-17 | 2022-05-31 | 巴斯夫杉杉电池材料(宁乡)有限公司 | Preparation method of positive electrode material precursor and preparation method of positive electrode material |
| CN111003734A (en) * | 2019-12-25 | 2020-04-14 | 南通金通储能动力新材料有限公司 | Method for recycling ternary precursor waste |
| CN111422926A (en) * | 2020-04-10 | 2020-07-17 | 浙江帕瓦新能源股份有限公司 | Core-shell structure Al/L a co-doped high-nickel ternary precursor, preparation method thereof and anode material |
| CN111422926B (en) * | 2020-04-10 | 2021-06-29 | 浙江帕瓦新能源股份有限公司 | Core-shell structure Al/La co-doped high-nickel ternary precursor and preparation method thereof, and anode material |
| CN111732132A (en) * | 2020-07-06 | 2020-10-02 | 金驰能源材料有限公司 | Nickel-cobalt-manganese core-shell structure precursor, preparation method thereof and positive electrode material |
| CN112047399A (en) * | 2020-09-07 | 2020-12-08 | 厦门厦钨新能源材料股份有限公司 | Precursor with reticular structure, composite oxide powder, preparation method and application thereof |
| CN112142123B (en) * | 2020-09-18 | 2022-05-20 | 厦门厦钨新能源材料股份有限公司 | Nickel-cobalt-manganese precursor with net structure, nickel-cobalt-manganese composite oxide powder, and preparation method and application thereof |
| CN112142125A (en) * | 2020-09-29 | 2020-12-29 | 山东精工电子科技有限公司 | Method for preparing high-nickel ternary cathode material by secondary growth method |
| CN113036098A (en) * | 2021-02-09 | 2021-06-25 | 横店集团东磁股份有限公司 | Preparation method and application of composite high-nickel ternary blended ferrophosphorus positive electrode material |
| WO2022188181A1 (en) * | 2021-03-12 | 2022-09-15 | 宁德新能源科技有限公司 | Positive electrode material, electrochemical apparatus comprising same, and electronic device |
| CN113603154A (en) * | 2021-07-30 | 2021-11-05 | 广东佳纳能源科技有限公司 | High-voltage nickel-cobalt-manganese ternary precursor and preparation method thereof |
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