CN108933261A - A kind of nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping - Google Patents
A kind of nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping Download PDFInfo
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- CN108933261A CN108933261A CN201810785368.1A CN201810785368A CN108933261A CN 108933261 A CN108933261 A CN 108933261A CN 201810785368 A CN201810785368 A CN 201810785368A CN 108933261 A CN108933261 A CN 108933261A
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Abstract
The invention discloses a kind of nickel cobalt of cerium dopping lithium aluminate/grapheme composite positive electrode material preparation methods, belong to the preparation technical field of lithium ion secondary battery anode material.Technical solution of the present invention main points are as follows: a kind of nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping, synthesis, the synthesis of carbon base body-grapheme material and the nickel cobalt lithium aluminate/grapheme composite positive electrode material synthesis of target product cerium dopping of the nickel cobalt lithium aluminate cathode material including cerium dopping and etc..The present invention effectively inhibits the side reaction between positive electrode and electrolyte by cerium dopping, and then improves the cyclical stability of lithium ion battery；It can be improved the electronic conductivity and ion transmission efficiency of positive electrode by carbon base body-graphene coated, and then improve the high rate performance of lithium ion battery.
Description
Technical field
The invention belongs to the energy and new material technology field, are related to a kind of preparation side of lithium ion secondary battery anode material
A kind of method, and in particular to nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping.
Background technique
Where the energy is the power of human social development, it is tight to realize that the sustainable development of the energy is that the mankind face 21 century
High challenge.Clean reproducible energy is developed in the aggravation of the problems such as with conventional fossil fuel bring greenhouse effects, environmental pollution
It is concerned by people more and more.Therefore, various new energy, such as solar energy, wind energy, underground heat, nuclear energy, biomass energy, sea
Ocean can wait, because being possible to solve shortage of resources and the support and promotion due to problem of environmental pollution by countries in the world.And secondary electricity
Pond is the important devices converted between chemical energy and electric energy, and rationally and effectively utilizes and store the important matchmaker of these new energy
It is situated between.
Mainstream power battery of the lithium battery as future development, many advantages not having with conventional batteries and biggish
Skill upgrading and cost decline space.Due to cost or capacity etc., traditional anode material for lithium-ion batteries (cobalt
It is positive electrode and manganese cathode material) it is difficult to positive electrode as high-power power battery, therefore development cost is low, capacity
High novel anode material is current international development trend, and ternary material nickel cobalt lithium aluminate (NCA) is used as lithium battery anode
One of research hotspot of material has many advantages, such as that capacity is high, thermal stability is good, relative low price and toxicity are lower, but high
Nickel positive electrode Li during the sintering process+With Ni2+It is easy to produce cationic mixing, leading to positive electrode, irreversible capacity increases for the first time
Add and cycle performance fails.In addition the active oxygen anion on nickelic positive electrode surface is easy and the CO in air2And H2O occurs
Reaction generates carbonate, while Li+Surface is moved to from ontology and generates LiOH and Li on the surface of the material2CO3, to positive electrode
Processing performance and high-temperature shelf property produce serious influence.Positive electrode NCA can be with electrolysis in wide voltage range
Strong side reaction occurs for liquid, increases impedance of the battery in charge and discharge process, reduces the chemical property of material.Due to itself
The reason of property, it still has the defect of cyclical stability difference, this largely also limits it and further develops.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple process and the nickel cobalt aluminic acids of low-cost cerium dopping
Lithium/grapheme composite positive electrode material preparation method, double modification lithium ion battery composite cathode materials made from this method have
Higher high rate performance and cyclical stability.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of nickel cobalt lithium aluminate/graphite of cerium dopping
The preparation method of alkene composite positive pole, it is characterised in that specific steps are as follows:
Step S1: by the nickel cobalt hydroxide precursor Ni of 2~3 parts by weight0.84Co0.16(OH)2, 0.5~2 parts by weight
LiOH·H2O, the Al of 0.03~0.04 parts by weight2O3With the Ce (NO of 0.1~0.4 parts by weight3)3·6H21~3h of O ball milling is obtained
Homogeneous mixture of material, then mixed material is transferred in tube furnace, with the heating rate liter of 1~2 DEG C/min under oxygen atmosphere
Temperature is to 500~600 DEG C of 3~5h of pretreatment, then is warming up to 700~800 DEG C of 6~8h of sintering and is obtaining the nickel cobalt lithium aluminate of cerium dopping just
Pole material；
Step S2: by the natural graphite of 5~7 parts by weight, the K of 4~6 parts by weight2S2O5With the P of 4~6 parts by weight2O5It is added
To dense H2SO4In and be uniformly mixed, then be placed in 80 DEG C of oil bath stir 4~6h after be scattered in deionized water obtain it is dilute
Release sample, dilute sample filtering and washing to neutrality and being stored at room temperature then obtained into pre-oxidation raw material, will pre-oxidation raw material at 0 DEG C
Dense H is added under condition of ice bath2SO4And be uniformly mixed, the potassium permanganate of 25~30 parts by weight is added under stirring conditions,
Deionized water dilution is added after 30~40 DEG C of 1~3h of stirring, diluted sample is add to deionized water and is being stirred
Under conditions of sequentially add hydrogen peroxide, concentrated hydrochloric acid and deionized water, staticly settle layering after continuing 0.5~1h of stirring, pour out
Clear liquid dialyses to neutrality to sample and obtains carbon base body-grapheme material in 40~50 DEG C of vacuum drying；
Step S3: it disperses the nickel cobalt lithium aluminate cathode material of the obtained cerium dopping of the step S1 of 0.5~2 parts by weight in
In ionized water and ultrasonic mixing uniformly obtains mixed liquor A, carbon base body-graphite that the step S2 of 0.05~0.2 parts by weight is obtained
Alkene material is scattered in deionized water and ultrasonic mixing uniformly obtains mixed liquid B, mixed liquor A and mixed liquid B is mixed, ball is added
Ball milling in ink tank, then the good mixture of ball milling is taken out to and is added the pH to 9~11 that ammonium hydroxide adjusts mixed system, it is subsequently placed in poly-
In 140~160 DEG C of 4~6h of hydro-thermal reaction in tetrafluoroethene reaction kettle, it is cooled to room temperature, filtration washing is dried to obtain after taking-up
Nickel cobalt lithium aluminate/grapheme composite positive electrode material of cerium dopping.
Further preferably, O in the entire calcination process of step S12Intake be 60mL/min.
Further preferably, the detailed process of step S1 are as follows: by 2.2023g nickel cobalt hydroxide precursor Ni0.84Co0.16
(OH)2、1.054g LiOH·H2O、0.0382g Al2O3With 0.2182g Ce (NO3)3·6H2O ball milling 2h is uniformly mixed
Material, then mixed material is transferred in tube furnace, 550 DEG C are warming up under oxygen atmosphere with the heating rate of 1.67 DEG C/min
4h is pre-processed, then is warming up to 750 DEG C of sintering 7h and obtains the nickel cobalt lithium aluminate cathode material of cerium dopping.
Further preferably, the detailed process of step S2 are as follows: by 6g natural graphite, 5g K2S2O5With 5g P2O5It is added to 24mL
Dense H2SO4In and be uniformly mixed, then be placed in 80 DEG C of oil bath stir 5h after be scattered in 700mL deionized water obtain it is dilute
Release sample, then by dilute sample filtering and washing to neutrality and be stored at room temperature 35h obtain pre-oxidation raw material, will pre-oxidation raw material exist
The dense H of 240mL is added under 0 DEG C of condition of ice bath2SO4And be uniformly mixed, 27.5g potassium permanganate is added under stirring conditions, then
The dilution of 500mL deionized water is added after 35 DEG C of stirring 2h, diluted sample is added in 1000mL deionized water and is being stirred
25mL hydrogen peroxide, 25mL concentrated hydrochloric acid and 225mL deionized water are sequentially added under conditions of mixing, and continue to staticly settle after stirring 0.5h
Layering, pours out supernatant, dialyses sample to neutrality and obtain carbon base body-grapheme material in 40 DEG C of vacuum drying.
Further preferably, the detailed process of step S3 are as follows: by the nickel cobalt lithium aluminate anode of the obtained cerium dopping of 1g step S1
Material is scattered in 10mL deionized water and ultrasound 1h is uniformly mixed and obtains mixed liquor A, the carbon base body-that 0.1g step S2 is obtained
Grapheme material is scattered in 5mL deionized water and ultrasound 1h is uniformly mixed and obtains mixed liquid B, and mixed liquor A and mixed liquid B are mixed
It closes and ball milling in spheroidal graphite tank is added, then the good mixture of ball milling is taken out to and is added the pH to 9~11 that ammonium hydroxide adjusts mixed system, so
It is placed in ptfe autoclave in 150 DEG C of hydro-thermal reaction 5h, is cooled to room temperature, take out filtration washing and be dried to obtain cerium
Nickel cobalt lithium aluminate/grapheme composite positive electrode material of doping.
The present invention effectively inhibits the side reaction between positive electrode and electrolyte by cerium dopping, and then improves lithium-ion electric
The cyclical stability in pond；It can be improved the electronic conductivity and ion transmission efficiency of positive electrode by carbon base body-graphene coated,
And then improve the high rate performance of lithium ion battery.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment
The detailed process of step S1 are as follows: by 2.2023g nickel cobalt hydroxide precursor Ni0.84Co0.16(OH)2、1.054g
LiOH·H2O、0.0382g Al2O3With 0.2182g Ce (NO3)3·6H2O ball milling 2h obtains a homogeneous mixture material, then will mixing
Material is transferred in tube furnace, is warming up to 550 DEG C of pretreatment 4h under oxygen atmosphere with the heating rate of 1.67 DEG C/min, then rise
Temperature obtains the nickel cobalt lithium aluminate cathode material of cerium dopping to 750 DEG C of sintering 7h；
The detailed process of step S2 are as follows: by 6g natural graphite, 5g K2S2O5With 5g P2O5It is added to the dense H of 24mL2SO4In simultaneously
It is uniformly mixed, then is placed in be scattered in 700mL deionized water after stirring 5h in 80 DEG C of oil bath and obtains dilute sample, then
By dilute sample filtering and washing to neutrality and be stored at room temperature 35h obtain pre-oxidation raw material, will pre-oxidation raw material in 0 DEG C of condition of ice bath
The dense H of lower addition 240mL2SO4And be uniformly mixed, 27.5g potassium permanganate is added under stirring conditions, is stirred then at 35 DEG C
The dilution of 500mL deionized water is added after 2h, diluted sample is added in 1000mL deionized water and under stirring conditions
25mL hydrogen peroxide, 25mL concentrated hydrochloric acid and 225mL deionized water are sequentially added, continues to staticly settle layering after stirring 0.5h, pour out
Supernatant dialyses to neutrality to sample and obtains carbon base body-grapheme material in 40 DEG C of vacuum drying；
The detailed process of step S3 are as follows: disperse the nickel cobalt lithium aluminate cathode material of the obtained cerium dopping of 1g step S1 in
In 10mL deionized water and ultrasound 1h is uniformly mixed and obtains mixed liquor A, carbon base body-grapheme material that 0.1g step S2 is obtained
It is scattered in 5mL deionized water and ultrasound 1h is uniformly mixed and obtains mixed liquid B, mixed liquor A and mixed liquid B are mixed, spheroidal graphite is added
Ball milling in tank, then the good mixture of ball milling is taken out to and is added the pH to 9~11 that ammonium hydroxide adjusts mixed system, it is subsequently placed in poly- four
In 150 DEG C of hydro-thermal reaction 5h in vinyl fluoride reaction kettle, it is cooled to room temperature, takes out the nickel cobalt that filtration washing is dried to obtain cerium dopping
Lithium aluminate/grapheme composite positive electrode material.
Respectively just to the nickel cobalt lithium aluminate of cerium dopping made from nickel cobalt lithium aluminate cathode material (sample number into spectrum 1), embodiment
Nickel cobalt lithium aluminate/grapheme composite positive electrode material (sample number into spectrum of cerium dopping made from pole material (sample number into spectrum 2) and embodiment
3) conductivity, cycle performance and high rate performance is measured.
Using the nickel cobalt lithium aluminate cathode material and embodiment of cerium dopping made from nickel cobalt lithium aluminate cathode material, embodiment
Nickel cobalt lithium aluminate/grapheme composite positive electrode material that cerium dopping is made prepares positive plate respectively, then uses and be prepared just
Pole piece prepares half-cell.Cycle performance test is half-cell test under conditions of charge-discharge magnification is 1C, charge and discharge electricity
Press range: 2.75-4.3V；High rate performance tests half electricity under the conditions of charge-discharge magnification is 0.2C, 0.5C, 1C, 2C, 5C respectively
Pond test, charging/discharging voltage range: 2.75-4.3V, measurement result are shown in Table 1~3.
The cycle performance test result (charge-discharge magnification 1C) of battery is made in the different samples of table 1
The different positive electrodes of table 2 be made battery high rate performance test result (charge-discharge magnification 0.2C, 0.5C, 1C,
2C、5C)
The conductivity test result of battery is made in nickel cobalt lithium aluminate/grapheme composite positive electrode material of 3 cerium dopping of table
| Sample number into spectrum | Conductivity (S/cm) | 1C recycles 100 weeks conservation rates |
| 1 | 8.14*10-5 | 77.98% |
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (5)
1. a kind of nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping, it is characterised in that specific steps
Are as follows:
Step S1: by the nickel cobalt hydroxide precursor Ni of 2 ~ 3 parts by weight0.84Co0.16(OH)2, 0.5 ~ 2 parts by weight LiOH
H2O, the Al of 0.03 ~ 0.04 parts by weight2O3With the Ce (NO of 0.1 ~ 0.4 parts by weight3)3·6H21 ~ 3h of O ball milling is obtained a homogeneous mixture
Material, then mixed material is transferred in tube furnace, 500 ~ 600 are warming up under oxygen atmosphere with the heating rate of 1 ~ 2 DEG C/min
DEG C 3 ~ 5h of pretreatment, then is warming up to 700 ~ 800 DEG C of 6 ~ 8h of sintering and obtains the nickel cobalt lithium aluminate cathode material of cerium dopping；
Step S2: by the natural graphite of 5 ~ 7 parts by weight, the K of 4 ~ 6 parts by weight2S2O5With the P of 4 ~ 6 parts by weight2O5It is added to dense H2SO4
In and be uniformly mixed, then be placed in 80 DEG C of oil bath stir 4 ~ 6h after be scattered in deionized water and obtain dilute sample, so
Dilute sample filtering and washing to neutrality and being stored at room temperature is obtained into pre-oxidation raw material afterwards, will pre-oxidation raw material in 0 DEG C of condition of ice bath
It is lower that dense H is added2SO4And be uniformly mixed, the potassium permanganate of 25 ~ 30 parts by weight is added under stirring conditions, then at 30 ~ 40
Deionized water dilution is added after DEG C 1 ~ 3h of stirring, diluted sample is add to deionized water and under stirring conditions successively
Hydrogen peroxide, concentrated hydrochloric acid and deionized water is added, staticly settles layering after continuing 0.5 ~ 1h of stirring, pours out supernatant, to sample into
Row dialysis obtains carbon base body-grapheme material to neutrality and in 40 ~ 50 DEG C of vacuum drying；
Step S3: deionization is dispersed by the nickel cobalt lithium aluminate cathode material of the obtained cerium dopping of the step S1 of 0.5 ~ 2 parts by weight
In water and ultrasonic mixing uniformly obtains mixed liquor A, carbon base body-grapheme material that the step S2 of 0.05 ~ 0.2 parts by weight is obtained
It is scattered in deionized water and ultrasonic mixing uniformly obtains mixed liquid B, mixed liquor A and mixed liquid B are mixed and are added in spheroidal graphite tank
Ball milling, then the good mixture of ball milling is taken out to and is added the pH to 9 ~ 11 that ammonium hydroxide adjusts mixed system, it is subsequently placed in polytetrafluoroethyl-ne
In 140 ~ 160 DEG C of 4 ~ 6h of hydro-thermal reaction in alkene reaction kettle, it is cooled to room temperature, filtration washing is dried to obtain cerium dopping after taking-up
Nickel cobalt lithium aluminate/grapheme composite positive electrode material.
2. nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping according to claim 1, special
Sign is: O in the entire calcination process of step S12Intake be 60mL/min.
3. nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping according to claim 1, special
Sign is the detailed process of step S1 are as follows: by 2.2023g nickel cobalt hydroxide precursor Ni0.84Co0.16(OH)2、1.054g
LiOH·H2O、0.0382g Al2O3With 0.2182g Ce (NO3)3·6H2O ball milling 2h obtains a homogeneous mixture material, then will mixing
Material is transferred in tube furnace, is warming up to 550 DEG C of pretreatment 4h under oxygen atmosphere with the heating rate of 1.67 DEG C/min, then rise
Temperature obtains the nickel cobalt lithium aluminate cathode material of cerium dopping to 750 DEG C of sintering 7h.
4. nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping according to claim 1, special
Sign is the detailed process of step S2 are as follows: by 6g natural graphite, 5g K2S2O5With 5g P2O5It is added to the dense H of 24mL2SO4In and stir
Mix it is uniformly mixed, then be placed in 80 DEG C of oil bath stir 5h after be scattered in 700mL deionized water and obtain dilute sample, then will
Dilute sample filtering and washing to neutrality and be stored at room temperature 35h obtain pre-oxidation raw material, will pre-oxidation raw material under 0 DEG C of condition of ice bath
The dense H of 240mL is added2SO4And be uniformly mixed, 27.5g potassium permanganate is added under stirring conditions, then at 35 DEG C of stirring 2h
Afterwards be added 500mL deionized water dilution, diluted sample is added in 1000mL deionized water and under stirring conditions according to
Secondary addition 25mL hydrogen peroxide, 25mL concentrated hydrochloric acid and 225mL deionized water continue to staticly settle layering after stirring 0.5h, pour out
Clear liquid dialyses to neutrality to sample and obtains carbon base body-grapheme material in 40 DEG C of vacuum drying.
5. nickel cobalt lithium aluminate/grapheme composite positive electrode material preparation method of cerium dopping according to claim 1, special
Sign is the detailed process of step S3 are as follows: disperses 10mL for the nickel cobalt lithium aluminate cathode material of the obtained cerium dopping of 1g step S1
In deionized water and ultrasound 1h is uniformly mixed and obtains mixed liquor A, the carbon base body that 0.1g step S2 is obtained-grapheme material dispersion
In 5mL deionized water and ultrasound 1h is uniformly mixed and obtains mixed liquid B, and mixed liquor A and mixed liquid B are mixed and are added in spheroidal graphite tank
Ball milling, then the good mixture of ball milling is taken out to and is added the pH to 9 ~ 11 that ammonium hydroxide adjusts mixed system, it is subsequently placed in polytetrafluoroethyl-ne
In 150 DEG C of hydro-thermal reaction 5h in alkene reaction kettle, it is cooled to room temperature, takes out the nickel cobalt aluminic acid that filtration washing is dried to obtain cerium dopping
Lithium/grapheme composite positive electrode material.
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Cited By (3)
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| CN111470547A (en) * | 2020-04-10 | 2020-07-31 | 广东墨睿科技有限公司 | NCM @ Al2O3Preparation method for modifying/rCO material |
| CN111477866A (en) * | 2020-05-13 | 2020-07-31 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Ternary cathode material nickel-cobalt-aluminum for lithium ion battery and preparation method thereof |
| CN115036605A (en) * | 2022-06-24 | 2022-09-09 | 云南云天化股份有限公司 | Method for regenerating composite cathode material of retired lithium battery |
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| CN115036605A (en) * | 2022-06-24 | 2022-09-09 | 云南云天化股份有限公司 | Method for regenerating composite cathode material of retired lithium battery |
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