CN109935798A - A kind of preparation method of lithium ion battery nickel manganese lithium composite material - Google Patents
A kind of preparation method of lithium ion battery nickel manganese lithium composite material Download PDFInfo
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- CN109935798A CN109935798A CN201711377915.4A CN201711377915A CN109935798A CN 109935798 A CN109935798 A CN 109935798A CN 201711377915 A CN201711377915 A CN 201711377915A CN 109935798 A CN109935798 A CN 109935798A
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Abstract
The invention discloses a kind of lithium ion battery preparation method of nickel manganese lithium composite material, include the following steps: that nickel chloride, lithium oxalate, manganese sulfate, yttrium nitrate and zirconium chloride and water are formed mixed solution by (1)；The mixed solution is slowly added dropwise with precipitant solution, is stirred to react to obtain presoma；Precursor is sintered, the LiNi of rare earth doped yttrium and zirconium is obtained0.5Mn1.5O4；(2) by the LiNi of rare earth doped yttrium0.5Mn1.5O4, carbon black, glucose be added ball mill in, ball milling is sintered in air atmosphere, obtain it is carbon-coated doping yttrium and zirconium nickel manganese lithium composite material.Lithium ion battery prepared by the present invention nickel manganese lithium composite material, using wet process doping process, improve the cyclical stability of material, it is when being used for lithium ion battery, electric conductivity with higher and good cyclical stability, so that lithium ion battery has high specific capacity and longer service life.
Description
Technical field
The present invention relates to lithium ion battery manufacturing field more particularly to a kind of lithium ion battery nickel manganese lithium composite material
Preparation method.
Background technique
Rechargeable type high-energy battery of the lithium ion secondary battery as a new generation, have operating voltage is high, energy density is big,
It has a safety feature, have extended cycle life and many merits such as self discharge is low, be widely used in mobile phone, laptop
In many portable electronic instrument equipment such as instrument and meter, meanwhile, in electric car, electric tool and energy storage peak shaving power station etc.
Field also has a good application prospect.
In recent years, with energy environment issues get worse and the requirement of electronic product lightness, people to lithium from
The research of sub- battery deepens continuously.Currently used commercialized anode material for lithium-ion batteries LiCoO2Price is high, toxic,
Old friends make great efforts finding its substitute always.LiMn2O4 (LiMn2O4) be concerned by people due to cheap, nontoxic,
And nickel is added into LiMn2O4, Li-Ni-Mn-O (LiNi can be obtained0.5Mn1.5O4Material LiNi0.5Mn1.5O4The charge and discharge process of material
In be primarily present the platform of 4.7V, theoretical capacity is up to 146.7mAh/g, energy density with higher, higher specific power,
Thus become the hot spot of current anode material for lithium-ion batteries research.
LiNi0.5Mn1.5O4Voltage is up to 5V or so in charge and discharge process, so that the electrolyte of electrode surface is ceaselessly by oxygen
Change and decompose, be deposited on electrode surface, hinder the deintercalation of lithium ion, so that its cycle performance is deteriorated, capacity attenuation, limit its business
Change application.In order to solve this problem, improve chemical property, many researchers carry out surface modification treatment to it, i.e., main
If carrying out cladding processing using other metals or nonmetallic oxide, keep apart positive electrode and electrolyte, from
And reducing electrolyte in charge and discharge process influences the dissolution of material, erosion etc..
Summary of the invention
The present invention provides a kind of preparation method of lithium ion battery nickel manganese lithium composite material, just using this method preparation
Pole material has good electrochemistry cycle performance.
To achieve the above object, the invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of preparation method of lithium ion battery nickel manganese lithium composite material, including
Following steps:
(1) LiNi of rare earth doped yttrium and zirconium is prepared0.5Mn1.5O4
It is 0.5:1:(1.45-1.48 by nickel, lithium, manganese, yttrium and zirconium molar ratio): (0.01-0.03): (0.01-0.02's)
Nickel chloride, lithium oxalate, manganese sulfate, yttrium nitrate and zirconium chloride are mixed with water, and it is 1- that stirring and dissolving, which uniformly obtains concentration of metal ions,
The mixed solution of 1.5mol/L；
By bicarbonate diammonium stirring and dissolving soluble in water, the precipitant solution that concentration is 1-2mol/L is obtained, it will be described mixed
It closes solution to be slowly added dropwise with precipitant solution, rate of addition 5-10ml/min obtains reaction solution, and the pH value for adjusting reaction solution is
9-11 is stirred to react, and is then aged, and refilters to obtain sediment, cleans sediment with detergent, and the sediment after cleaning is dropped
Temperature freezes 2-5h, is then dried in vacuo, obtains presoma to-15-- 20 DEG C；
In air atmosphere by the precursor, it is sintered with 700-800 DEG C of temperature of stabilization, time 6-8h, i.e.,
Obtain the LiNi of rare earth doped yttrium and zirconium0.5Mn1.5O4；
(2) LiNi of carbon coating rare earth doped yttrium and zirconium0.5Mn1.5O4
By the LiNi of above-mentioned rare earth doped yttrium0.5Mn1.5O4, carbon black, glucose, according to mass ratio 100:(1-3):
(3-5) is added in ball mill, with the revolving speed ball milling 6-8h of 400-500r/min, is uniformly mixed, is sintered in air atmosphere, natural
It is cooled to the nickel manganese lithium composite material that carbon-coated doping yttrium and zirconium are arrived after room temperature.
Further, preparation method of the lithium ion battery with nickel manganese lithium composite material the step of in (1), institute
The molar ratio for stating nickel chloride, lithium oxalate, manganese sulfate, nickel in yttrium nitrate and zirconium chloride, lithium, manganese, yttrium and zirconium is 0.5:1:1.47:
0.02:0.02.
Further, preparation method of the lithium ion battery with nickel manganese lithium composite material the step of in (1), step
Suddenly in (1), the mixing time of the mixed solution is 2-4h, and solution temperature is 40-50 DEG C.
Further, preparation method of the lithium ion battery with nickel manganese lithium composite material the step of in (1), step
Suddenly in (1), the sintering temperature of the precursor in air atmosphere is 740-760 DEG C, sintering time 6.5h.
Further, preparation method of the lithium ion battery with nickel manganese lithium composite material the step of in (1), step
Suddenly in (2), the LiNi of the rare earth doped yttrium0.5Mn1.5O4, carbon black, glucose mass ratio be 100:2.5:4.3.
Further, preparation method of the lithium ion battery with nickel manganese lithium composite material the step of in (1), step
Suddenly in (2), the sintering process are as follows: keep the temperature 2-3 hours after being warming up to 400-500 DEG C with 5-10 DEG C/min heating rate, then
It is warming up to 700-800 DEG C with the heating rate of 10-15 DEG C/min, 4-5h is kept the temperature, makes its carbonization, finally with 15-20 DEG C/min's
Cooling rate is down to 400-600 DEG C of annealing 5-10h.
The lithium ion battery that the second aspect of the invention is to provide a kind of method preparation described above is compound with nickel manganese lithium
Material.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
Lithium ion battery prepared by the present invention nickel manganese lithium composite material, uses wet process doping process, and preparation doping is dilute
The LiNi of earth elements yttrium and zirconium0.5Mn1.5O4, the stable circulation performance of material is improved, and using special process on its surface
Film closely coat with one layer of carbon, therefore the composite material be used for lithium ion battery when, electric conductivity with higher
With good cyclical stability so that lithium ion battery have high specific capacity and longer service life.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
The preparation of 1 lithium ion battery of embodiment nickel manganese lithium composite material
(1) LiNi of rare earth doped yttrium and zirconium is prepared0.5Mn1.5O4
By nickel, lithium, manganese, yttrium and zirconium molar ratio be the nickel chloride of 0.5:1:1.45:0.03:0.02, lithium oxalate, manganese sulfate,
Yttrium nitrate, zirconium chloride are mixed with water, and stirring and dissolving uniformly obtains the mixed solution that concentration of metal ions is 1mol/L, wherein mixing
The mixing time for closing solution is 4h, and solution temperature is 40 DEG C.
By bicarbonate diammonium stirring and dissolving soluble in water, the precipitant solution that concentration is 1mol/L is obtained, by the mixing
Solution is slowly added dropwise with precipitant solution, and rate of addition 50ml/min obtains reaction solution, and the pH value for adjusting reaction solution is 9, stirs
Reaction is mixed, is then aged, refilters to obtain sediment, cleans sediment with detergent, the sediment after cleaning is cooled to -15
DEG C, 5h is freezed, is then dried in vacuo, obtains presoma.
In air atmosphere by the precursor, it is sintered with 700 DEG C of temperature of stabilization, the time is 8h to get to mixing
The LiNi of miscellaneous rare earth element yttrium0.5Mn1.5O4。
(2) LiNi of carbon coating rare earth doped yttrium and zirconium0.5Mn1.5O4
By the LiNi of above-mentioned rare earth doped yttrium and zirconium0.5Mn1.5O4, carbon black, glucose, according to mass ratio 100:1:3
It is added in ball mill, with the revolving speed ball milling 8h of 400r/min, is uniformly mixed, is sintered in air atmosphere, heated up with 5 DEG C/min fast
Rate keeps the temperature 3h after being warming up to 400 DEG C, be then warming up to 700 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 5h hours, makes its carbon
Change, 600 DEG C of annealing 10h are finally down to the cooling rate of 15 DEG C/min, is naturally cooling to after room temperature carbon-coated to get arriving
Adulterate the nickel manganese lithium composite material of yttrium and zirconium.
The preparation of 2 lithium ion battery of embodiment nickel manganese lithium composite material
(1) LiNi of rare earth doped yttrium and zirconium is prepared0.5Mn1.5O4
By nickel, lithium, manganese, yttrium and zirconium molar ratio be the nickel chloride of 0.5:1:1.48:0.01:0.01, lithium oxalate, manganese sulfate,
Yttrium nitrate and zirconium chloride are mixed with water, and stirring and dissolving uniformly obtains the mixed solution that concentration of metal ions is 1.5mol/L, wherein
The mixing time of mixed solution is 2h, and solution temperature is 50 DEG C.
By bicarbonate diammonium stirring and dissolving soluble in water, the precipitant solution that concentration is 2mol/L is obtained, by the mixing
Solution is slowly added dropwise with precipitant solution, and rate of addition 10ml/min obtains reaction solution, and the pH value for adjusting reaction solution is 11,
It is stirred to react, is then aged, refilter to obtain sediment, clean sediment with detergent, the sediment after cleaning is cooled to-
20 DEG C, 2h is freezed, is then dried in vacuo, obtains presoma.
In air atmosphere by the precursor, it is sintered with 800 DEG C of temperature of stabilization, the time is 6h to get to mixing
The LiNi of miscellaneous rare earth element yttrium and zirconium0.5Mn1.5O4。
(2) LiNi of carbon coating rare earth doped yttrium and zirconium0.5Mn1.5O4
By the LiNi of above-mentioned rare earth doped yttrium and zirconium0.5Mn1.5O4, carbon black, glucose, according to mass ratio 100:3:5
It is added in ball mill, with the revolving speed ball milling 6h of 500r/min, is uniformly mixed, is sintered in air atmosphere, with 10 DEG C/min heating
Rate keeps the temperature 2h after being warming up to 500 DEG C, be then warming up to 800 DEG C with the heating rate of 15 DEG C/min, heat preservation 4h makes its carbonization, most
400 DEG C of annealing 5h are down to the cooling rate of 20 DEG C/min afterwards, be naturally cooling to after room temperature to get to carbon-coated doping yttrium with
The nickel manganese lithium composite material of zirconium.
Comparative example
(1) by the manganese acetate of the nickel acetate of 0.005mol, the cobalt acetate of 0.005mol and 0.02mol be dissolved in 100ml go from
In sub- water, magnetic agitation 4h forms it into homogeneous mixed solution at 30 DEG C, wherein the mass ratio of the material of Ni2+:Co2+:Mn2+
For 1:1:4.Lithium hydroxide is dissolved in stirring and dissolving in deionized water and obtains the clear lithium hydroxide solution of 60ml, wherein hydroxide
The concentration of lithium is 1.25mol/L；
(2) mixed solution is added dropwise in lithium hydroxide solution with the speed of 3ml/min and is mixed to get reaction solution, use ammonium hydroxide
The pH value for adjusting reaction solution is 11.0, and places reaction liquid into 50 DEG C of water-baths and be stirred to react 3h with the speed of 120rmp, then is old
Change 4h, suction filtration obtains sediment, and 3 times wash with distilled water, the sediment after being cleaned；Sediment after cleaning is put into cold
In trap, -90 DEG C are cooled to together with cold-trap, rate of temperature fall is 2 DEG C/min, after freezing 3h, by the sediment of freezing in vacuum degree
It is dried in vacuo under≤10.0Pa for 24 hours, obtains precursor；
(3) precursor is mixed with lithium hydroxide, wherein the mass ratio of the material of Li:Ni:Co:Mn is 9:1:1:4, with grinding
Alms bowl grinding is uniformly mixed it, obtains mixture, and mixture is cooled to room temperature tabletting first in 480 DEG C of pre-burning 8h with Muffle furnace,
Then in 900 DEG C of sintering 3h, product is obtained.
Above-described embodiment 1, embodiment 2 and comparative example products therefrom and conductive agent acetylene black, binder PVDF is (poly-
Vinylidene) it is uniformly mixed according to mass ratio 8: 1: 1, the modulation of this mixture is slurried with NMP (1-Methyl-2-Pyrrolidone)
Material, is evenly applied on aluminium foil, is put into baking oven, 80-120 DEG C of drying 1h, and taking-up is washed into pole piece, and 85 DEG C of vacuum drying 12 are small
When, tabletting is carried out, 85 DEG C are dried in vacuo 12 hours, obtained experimental cell pole piece.It is to electrode with lithium piece, electrolyte is
1.5mol/L LiPF6EC (ethyl carbonate ester)+DMC (dimethyl carbonate) (volume ratio 1: 1) solution, diaphragm is
Celgard2400 film is assembled into CR2025 type button cell in the glove box full of argon atmosphere, and charge and discharge are by voltage
3.5~4.9V.Electric performance test is carried out at being 25 DEG C in test temperature, after tested the material and comparative example of the embodiment one and two
Product compare, specific capacity improves 45-55%, and service life improves 2 times or more.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (7)
1. a kind of lithium ion battery preparation method of nickel manganese lithium composite material, which comprises the steps of:
(1) LiNi of rare earth doped yttrium and zirconium is prepared0.5Mn1.5O4
It is 0.5:1:(1.45-1.48 by nickel, lithium, manganese, yttrium and zirconium molar ratio): (0.01-0.03): the chlorination of (0.01-0.02)
Nickel, lithium oxalate, manganese sulfate, yttrium nitrate and zirconium chloride are mixed with water, and it is 1- that stirring and dissolving, which uniformly obtains concentration of metal ions,
The mixed solution of 1.5mol/L；
By bicarbonate diammonium stirring and dissolving soluble in water, the precipitant solution that concentration is 1-2mol/L is obtained, the mixing is molten
Liquid is slowly added dropwise with precipitant solution, and rate of addition 5-10ml/min obtains reaction solution, and the pH value for adjusting reaction solution is 9-
11, it is stirred to react, is then aged, refilter to obtain sediment, clean sediment with detergent, the sediment after cleaning is cooled down
To-15-- 20 DEG C, 2-5h is freezed, is then dried in vacuo, obtains presoma；
In air atmosphere by the precursor, it is sintered with 700-800 DEG C of temperature of stabilization, the time is 6-8h to get arriving
The LiNi of rare earth doped yttrium and zirconium0.5Mn1.5O4；
(2) LiNi of carbon coating rare earth doped yttrium and zirconium0.5Mn1.5O4
By the LiNi of above-mentioned rare earth doped yttrium0.5Mn1.5O4, carbon black, glucose, according to mass ratio 100:(1-3): (3-5) plus
Enter in ball mill, with the revolving speed ball milling 6-8h of 400-500r/min, is uniformly mixed, is sintered, is naturally cooling in air atmosphere
The nickel manganese lithium composite material of carbon-coated doping yttrium and zirconium is arrived after room temperature.
2. the lithium ion battery according to claim 1 preparation method of nickel manganese lithium composite material, which is characterized in that step
(1) in, nickel in the nickel chloride, lithium oxalate, manganese sulfate, yttrium nitrate and zirconium chloride, lithium, manganese, yttrium and zirconium molar ratio be 0.5:
1:1.47:0.02:0.02.
3. the lithium ion battery according to claim 1 preparation method of nickel manganese lithium composite material, which is characterized in that step
(1) in, the mixing time of the mixed solution is 2-4h, and solution temperature is 40-50 DEG C.
4. the lithium ion battery according to claim 1 preparation method of nickel manganese lithium composite material, which is characterized in that step
(1) in, the sintering temperature of the precursor in air atmosphere is 740-760 DEG C, sintering time 6.5h.
5. the lithium ion battery according to claim 1 preparation method of nickel manganese lithium composite material, which is characterized in that step
(2) in, the LiNi of the rare earth doped yttrium0.5Mn1.5O4, carbon black, glucose mass ratio be 100:2.5:4.3.
6. the lithium ion battery according to claim 1 preparation method of nickel manganese lithium composite material, which is characterized in that step
(2) in, the sintering process are as follows: keep the temperature 2-3 hours after being warming up to 400-500 DEG C with 5-10 DEG C/min heating rate, then with
The heating rate of 10-15 DEG C/min is warming up to 700-800 DEG C, keeps the temperature 4-5h, makes its carbonization, finally with the drop of 15-20 DEG C/min
Warm speed is down to 400-600 DEG C of annealing 5-10h.
7. a kind of lithium ion battery nickel manganese lithium composite material prepared such as any one of claim 1-6 the method.
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Cited By (1)
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| CN113830845A (en) * | 2021-10-14 | 2021-12-24 | 浙江帕瓦新能源股份有限公司 | Preparation method of carbon and yttrium oxide double-coated nickel-manganese zirconium-doped binary anode material |
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Application publication date: 20190625 |