CN106410186B - A kind of preparation method and application of lithium-rich oxide anode material - Google Patents
A kind of preparation method and application of lithium-rich oxide anode material Download PDFInfo
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- 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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Abstract
A kind of preparation method of lithium-rich oxide anode material, the chemical molecular formula of the lithium-rich oxide anode material are Li [Li(1‑2x)/3Nix‑yM2yMn2/3‑x/3‑y]O2, in formula: the mixture of 0 < x < 0.5,0 < y < x, one or more of M Fe, Co, Al and Cr arbitrary proportion；Preparation method is: preparing the Li of M doping using high temperature solid-state method first2MnO3Material, then it is mixed with the source Li, the source Ni and Mn source material, baking mixed 5-15h, obtains object under the conditions of 700-950 DEG C.Material prepared by the present invention has many advantages, such as that stable structure, condition are easily controllable, lot stability is good, is suitable for large-scale production；Have many advantages, such as that first charge-discharge efficiency is high, voltage attenuation is small, cyclicity is good using the button cell that prepared lithium-rich oxide anode material is assembled into.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, specifically a kind of lithium-rich oxide anode material
Preparation method and application.
Background technique
With popularizing for portable electronic product, hybrid vehicle and pure electric automobile, lithium ion battery is also obtained
More and more extensive use.In recent years, it is the lithium ion battery for developing high-energy density, is developed many high-energy densities
Positive electrode.Wherein discharge capacity is high, voltage platform is wide, environmentally protective etc. excellent because having for lithium-rich oxide anode material
It puts and causes further investigation.The expression formula of lithium-rich oxide material is Li (Li1/3-2x/3NixMn2/3-x/3)O2(0<x<1/
2) it, can regard Li as2MnO3(stratified material is represented by Li [Li1/3Mn2/3]O2) material and LiNi1/2Mn1/2O2Material
The solid solution of formation, therefore, lithium-rich oxide material Li (Li1/3-2x/3NixMn2/3-x/3)O2Expression formula can also write a
[yLi2MnO3·(1-y)LiNi1/2Mn1/2O2], wherein a=2 (1+x)/3, y=(1-2x)/(1+x).
According to a large amount of document report, to Li (Li1/3-2x/3NixMn2/3-x/3)O2Material, which carries out metal ion mixing, to be had
Effect improves its chemical property.For lithium-rich oxide anode material and the modified lithium-rich oxidation of metal M ion
The preparation method of object positive electrode mainly has coprecipitation, sol-gal process and combustion method etc..Coprecipitation: Li et al. people report
It is a kind of that the Acetate Solution of Mn, Ni and Co and LiOH are prepared into hydroxide precursor by coprecipitation reaction, by washing
After dry and LiOH mixing and ball milling is uniform, Li (Li is prepared by high-temperature roasting0.2Mn0.56Ni0.16Co0.08)O2The method of material
(Journal of Power Sources,2011,196,4821).Sol-gal process: Zheng et al. is first by Ni (NO3)2·
6H2O、Co(NO3)2·6H2O and Mn (NO3)2Wiring solution-forming, then by LiNO3It is slowly added to the mixed solution of appropriate citric acid
Into the mixed solution of above-mentioned transition metal, then with ammonium hydroxide adjust the mixed solution of above two solution pH value be 7.0~
8.0, by two-step thermal processing and quenching after being evaporated, obtain designed Li (Li0.20Ni0.13Co0.13Mn0.54)O2Positive electrode
(Electrochimica Acta,2011,56,3071)；Ma et al. is prepared for Li also by similar method
[Li0.2Ni0.11Co0.11Mn0.54Al0.04]O2Material (Journal of Power Sources, 2015,277,393).2.Burning
Method: Hong et al. is configured to solution according to stoichiometric ratio, is filled using the acetate of Li, Ni and Mn and nitrate as raw material
Gained xerogel is lighted after dividing drying, carries out high-temperature heat treatment and quenching again finally to get required Li is arrived
(Li0.2Ni0.2Mn0.6)O2With Li (Li0.27Co0.20Mn0.53)O2Material (Solid State Ionics, 2005,176,1035).
Above-described preparation method all uses to reach the uniform mixing of metal ion by metal ion Ni, Mn
It is added simultaneously with M and is made into homogeneous solution or uniformly mixed method, lithium-rich oxide material prepared by these methods
Specific discharge capacity with higher, but its that there is also material structures is unstable, part layer structure is to sharp brilliant in cyclic process
Stone structure transformation voltage because caused by declines and the problems such as capacity attenuation, constrains its reality in lithium ion battery and answers
With.The present invention is by dopant M ion modification Li2MnO3Phase, then pass through modified Li2MnO3Phase and the source Li, the source Ni and the source Mn
A kind of baking mixed preparation method to prepare lithium-rich oxide of material.By retrieval, for doped lithium-rich
Oxide anode material Li [Li(1-2x)/3Nix-yM2yMn2/3-x/3-y]O2(one in 0 < x < 0.5,0 < y < x, M Fe, Co, Al and Cr
Kind is several), it is not yet found that similar report.
Summary of the invention
Object of the present invention is to overcome the above problem of the existing technology, a kind of lithium-rich oxide anode material is provided
Preparation method and application.
Technical solution of the present invention:
A kind of preparation method of lithium-rich oxide anode material, the chemistry of the lithium-rich oxide anode material
Molecular formula is Li [Li(1-2x)/3Nix-yM2yMn2/3-x/3-y]O2, in formula: one in 0 < x < 0.5,0 < y < x, M Fe, Co, Al and Cr
The mixture of kind or two or more arbitrary proportions；
Preparation methods steps are as follows:
1) source Li, the source Mn and M source metal are uniformly mixed, obtain mixture；
2) said mixture is roasted under conditions of 400-750 DEG C 5-80h, obtains the metal-doped Li of M2MnO3Material；
3) Li that above-mentioned M is metal-doped2MnO3Material and the source Li, the source Ni and the source Mn are sufficiently mixed uniformly, obtain mixing material
Material；
4) above-mentioned mixing material is roasted into 5-15h at 700-950 DEG C；
5) it is cooled to room temperature, obtains lithium-rich oxide anode material Li [Li(1-2x)/3Nix-yM2yMn2/3-x/3-y]O2。
The source Li is that one or more of lithium carbonate, lithium hydroxide, lithium nitrate and lithium acetate are appointed in the step 1)
The mixture of meaning ratio；The source Mn is oxidation (Asia) manganese, hydroxide (Asia) manganese, hydroxyl manganese oxide, manganese carbonate, manganese nitrate and manganese acetate
One of two or more arbitrary proportions mixture；M source metal is carbonate, hydroxide, nitrate and the acetic acid of M metal
The mixture of one or more of salt arbitrary proportion；The molar ratio in the source Li, the source Mn and M source metal is (2-4x): (1-
2x-3y): 3y, in formula: 0 < x < 0.5,0 < y < x.
The source Li is that one or more of lithium carbonate, lithium hydroxide, lithium nitrate and lithium acetate are appointed in the step 3)
The mixture of meaning ratio；The source Ni is oxidation (Asia) nickel, hydroxide (Asia) nickel, hydroxy nickel oxide, nickelous carbonate, nickel nitrate and nickel acetate
One or more of arbitrary proportion mixture；The source Mn be oxidation (Asia) manganese, hydroxide (Asia) manganese, hydroxyl manganese oxide,
The mixture of the two or more arbitrary proportions of one of manganese carbonate, manganese nitrate and manganese acetate；M metal-doped Li2MnO3Material with
The molar ratio of Li, Ni and Mn for being added are (1-2x): 3x:(3x-3y)/2:(3x+3y)/2, in formula: 0 < x < 0.5,0 < y < x.
A kind of application of lithium-rich oxide anode material, is used to prepare the positive material of height ratio capacity lithium ion battery
Material.
The beneficial effects of the present invention are:
The lithium-rich oxide anode material of this method preparation will be modified M ion doping to Li2MnO3Xiang Zhong, effectively
The structure of material is stabilized, then with modified Li2MnO3Based on material, lithium-rich oxide anode material is prepared, is inhibited
The structure transformation of prepared lithium-rich oxide anode material in cyclic process, thus effectively reduce material and exist
Oxygen amount of precipitation during initial charge, improves the first charge-discharge efficiency of material, reduces material in cyclic process
Voltage drop improves the circulation volume conservation rate of material；The material preparation process controllability is good, and extensive manufacturing cost is low
It is honest and clean, process repeatability is high, lot stability is good, be suitable for large-scale production, can satisfy in the market to high voltage, height ratio capacity lithium
The demand of ion battery positive electrode.
Detailed description of the invention
Fig. 1 is lithium-rich oxide anode material Li [Li prepared by embodiment 10.28Ni0.06Fe0.04Mn0.62]O2(x=
1/12, M=Fe, y=0.02) SEM figure.
Fig. 2 is lithium-rich oxide anode material Li [Li prepared by embodiment 10.28Ni0.06Fe0.04Mn0.62]O2(x=
1/12, M=Fe, y=0.02) cycle performance figure.
Fig. 3 is lithium-rich oxide anode material Li [Li prepared by embodiment 20.2Ni0.1Co0.2Mn0.5]O2(x=1/
5, M=Co, y=0.1) SEM figure.
Fig. 4 is lithium-rich oxide anode material Li [Li prepared by embodiment 20.2Ni0.1Co0.2Mn0.5]O2(x=1/
5, M=Co, y=0.1) cycle performance figure.
Fig. 5 is lithium-rich oxide anode material Li [Li prepared by embodiment 30.11Ni0.28Al0.1Mn0.51]O2(x=
1/3, M=Al, y=0.05) SEM figure.
Fig. 6 is lithium-rich oxide anode material Li [Li prepared by embodiment 30.11Ni0.28Al0.1Mn0.51]O2(x=
1/3, M=Al, y=0.05) cycle performance figure.
Fig. 7 is lithium-rich oxide anode material Li [Li prepared by embodiment 40.03Ni0.43Cr0.04Mn0.50]O2(x=
9/20, M=Cr, y=0.02) SEM figure.
Fig. 8 is lithium-rich oxide anode material Li [Li prepared by embodiment 40.03Ni0.43Cr0.04Mn0.50]O2(x=
9/20, M=Cr, y=0.02) cycle performance figure.
Specific embodiment
Detailed process of the invention is told about by the following examples, providing embodiment is the convenience for understanding, rather than
The limitation present invention.
Embodiment 1:
A kind of preparation method of lithium-rich oxide anode material, the chemistry of the lithium-rich oxide anode material
Molecular formula is Li [Li0.28Ni0.06Fe0.04Mn0.62]O2(x=1/12, M=Fe, y=0.02), preparation methods steps are as follows:
1) 87.14g MnSO is weighed4·H2O and 16.16g Fe (NO3)3·9H2O preparing metal ion concentration is 1mol/L
Solution；
2) under lasting stirring condition, it is slowly added to the mixed solution of ammonium hydroxide and sodium carbonate into above-mentioned solution, mixes molten
In liquid ammonia concn be 0.2mol/L, concentration of sodium carbonate 2mol/L, with control reacting liquid pH value be 10, carry out precipitation reaction,
Sediment is filtered, washed and dried, the MnCO of Fe doping is obtained3Material；
3) 41.05g Li is weighed2CO3, and the MnCO for the Fe doping that it is obtained with step 2)3Material is mixed evenly, and is placed in
It is roasted in Muffle furnace, maturing temperature is 400 DEG C, calcining time 80h, obtains the Li of Fe doping2MnO3Material；
4) by 17.00gCH3COOLi·2H2O、18.42g Ni(NO3)2·6H2O and 25.33g Mn (CH3COO)2·4H2O
Mixing obtains mixed solution, and metal ion total concentration is 2mol/L, the Li for the Fe doping that step 3) is obtained2MnO3Material is put into
Suspension is obtained in mixed solution, is under stirring conditions evaporated suspension, obtains persursor material；
5) persursor material for obtaining step 4) is placed in Muffle furnace and roasts, and maturing temperature is 950 DEG C, when roasting
Between be 5h, obtain 80.70g lithium-rich oxide anode material Li [Li0.28Ni0.08Mn0.64]O2。
Fig. 1 is lithium-rich oxide anode material Li [Li prepared by embodiment 10.28Ni0.06Fe0.04Mn0.62]O2SEM
Figure.
Prepared lithium-rich oxide anode material is used to prepare the positive electrode of height ratio capacity lithium ion battery.
Fig. 2 is lithium-rich oxide anode material Li [Li prepared by embodiment 10.28Ni0.06Fe0.04Mn0.62]O2Assembly
At the cycle performance figure of button cell.Show in figure using Li [Li prepared by this method0.28Ni0.06Fe0.04Mn0.62]O2Material
Specific discharge capacity with higher and good cycle performance.
Embodiment 2:
A kind of preparation method of lithium-rich oxide anode material, the chemistry of the lithium-rich oxide anode material
Molecular formula is Li [Li0.2Ni0.1Co0.2Mn0.5]O2(x=1/5, M=Co, y=0.1), preparation methods steps are as follows:
1) 27.58g LiNO is weighed respectively3·H2O,22.99gMnCO3And 16.05gCo3O4, it is uniformly mixed；
2) the resulting mixture of step 1) is placed in Muffle furnace and is roasted, maturing temperature is 750 DEG C, and calcining time is
5h obtains the Li of Co doping2MnO3Material；
3) 42.78g NiCl6H is prepared2O and 50.71g MnSO4·4H2The mixed solution of O, metal ion total concentration are
2.5mol/L；
4) under lasting stirring condition, the mixing that ammonium hydroxide and sodium hydroxide are slowly added into the resulting solution of step 3) is molten
Liquid, ammonia concn is 0.3mol/L, concentration of sodium carbonate 4mol/L in mixed solution, to control reacting liquid pH value as 10, carry out
Precipitation reaction obtains the mixed sediment of nickel hydroxide and manganous hydroxide, mixed sediment is filtered, washed and dried；
5) by the Li of the resulting Co doping of step 2)2MnO3Material, the resulting mixed sediment of step 4), and
27.58gLiNO3 is uniformly mixed, and is placed in Muffle furnace and is roasted, and maturing temperature is 850 DEG C, and calcining time 10h is obtained
85.45g lithium-rich oxide anode material Li [Li0.2Ni0.1Co0.2Mn0.5]O2。
Fig. 3 is lithium-rich oxide anode material Li [Li prepared by embodiment 20.2Ni0.1Co0.2Mn0.5]O2SEM
Figure.
Prepared lithium-rich oxide anode material is used to prepare the positive electrode of height ratio capacity lithium ion battery.
Fig. 4 is lithium-rich oxide anode material Li [Li prepared by embodiment 20.2Ni0.1Co0.2Mn0.5]O2It is assembled into
The cycle performance figure of button cell.Show the Li [Li prepared by this method in figure0.2Ni0.1Co0.2Mn0.5]O2Material have compared with
High specific discharge capacity and good cycle performance.
Embodiment 3:
A kind of preparation method of lithium-rich oxide anode material, the chemistry of the lithium-rich oxide anode material
Molecular formula is Li [Li0.11Ni0.28Al0.1Mn0.51]O2(x=1/3, M=Al, y=0.05), preparation methods steps are as follows:
1) 9.32g LiOH, 10.87gMn (OH) are weighed respectively2With 37.51gAl (NO3)3·9H2O is uniformly mixed；
2) the resulting mixture of step 1) is placed in Muffle furnace and is roasted, maturing temperature is 550 DEG C, and calcining time is
55h obtains the Li of Al doping2MnO3Material；
3) Li of the Al doping obtained step 2)2MnO3Material and 24.63g Li2CO3, 10.21gNiO and
44.06gMnCO3 is uniformly mixed, and obtains mixture；
4) the resulting mixture object of step 3) is placed in Muffle furnace and is roasted, maturing temperature is 700 DEG C, calcining time
For 15h, 86.85g lithium-rich oxide anode material Li [Li is obtained0.11Ni0.28Al0.1Mn0.51]O2。
Fig. 5 is lithium-rich oxide anode material Li [Li prepared by embodiment 20.11Ni0.28Al0.1Mn0.51]O2SEM
Figure.
Prepared lithium-rich oxide anode material is used to prepare the positive electrode of height ratio capacity lithium ion battery.
Fig. 6 is lithium-rich oxide anode material Li [Li prepared by embodiment 20.11Ni0.28Al0.1Mn0.51]O2Assembly
At the cycle performance figure of button cell.Show the Li [Li prepared by this method in figure0.11Ni0.28Al0.1Mn0.51]O2Material tool
There are higher specific discharge capacity and good cycle performance.
Embodiment 4:
A kind of preparation method of lithium-rich oxide anode material, the chemistry of the lithium-rich oxide anode material
Molecular formula is Li [Li0.03Ni0.43Cr0.04Mn0.50]O2(x=9/20, M=Cr, y=0.02), preparation methods steps are as follows:
1) 4.93g Li is weighed respectively2CO3,3.07gMnCO3With 16.01gCr (NO3)3·9H2O is uniformly mixed；
2) the resulting mixing material of step 1) is placed in Muffle furnace and is roasted, maturing temperature is 650 DEG C, calcining time
For 25h, the Li of Cr doping is obtained2MnO3Material；
3) Li of the Cr doping obtained step 2)2MnO3Material and 37.76gLiOH, 51.04gNiCO3With
54.03gMnCO3It is uniformly mixed, is placed in Muffle furnace and is roasted, maturing temperature is 800 DEG C, and calcining time 12h is obtained
93.94g lithium-rich oxide anode material Li [Li0.03Ni0.43Cr0.04Mn0.50]O2。
Fig. 7 is lithium-rich oxide anode material Li [Li prepared by embodiment 40.03Ni0.43Cr0.04Mn0.50]O2SEM
Figure.
Prepared lithium-rich oxide anode material is used to prepare the positive electrode of height ratio capacity lithium ion battery.
Fig. 8 is lithium-rich oxide anode material Li [Li prepared by embodiment 40.03Ni0.43Cr0.04Mn0.50]O2Assembly
At the cycle performance figure of button cell.Show prepared Li [Li in figure0.03Ni0.43Cr0.04Mn0.50]O2Material is with higher
Specific discharge capacity and good cycle performance.
In conclusion the lithium-rich oxide of this method preparation reduces the voltage attenuation of material, material is improved
Cycle performance.Therefore, the lithium-rich oxide anode material of the method preparation is hopeful to be able to satisfy in the market to high-performance lithium
Demand of the ion battery to height ratio capacity and Width funtion window positive electrode.
Although invention has been described for above-mentioned application example, the invention is not limited to above-mentioned specific implementations
Mode, the above mentioned embodiment is only schematical, rather than restrictive, and those skilled in the art are at this
Under the enlightenment of invention, without deviating from the spirit of the invention, many variations can also be made, these belong to of the invention
Within protection.
Claims (3)
1. a kind of preparation method of lithium-rich oxide anode material, it is characterised in that: the lithium-rich oxide anode
The chemical molecular formula of material is Li [Li(1-2x)/3Nix-yM2yMn2/3-x/3-y]O2, in formula: 0 < x < 0.5,0 < y < x, M Fe, Co, Al
With the mixture of one or more of Cr arbitrary proportion；
Preparation methods steps are as follows:
1) source Li, the source Mn and M source metal are uniformly mixed, obtain mixture；
2) said mixture is roasted under conditions of 400-750 DEG C 5-80h, obtains the metal-doped Li of M2MnO3Material；
3) Li that above-mentioned M is metal-doped2MnO3Material and the source Li, the source Ni and the source Mn are sufficiently mixed uniformly, obtain mixing material；
4) above-mentioned mixing material is roasted into 5-15h at 700-950 DEG C；
5) it is cooled to room temperature, obtains lithium-rich oxide anode material Li [Li(1-2x)/3Nix-yM2yMn2/3-x/3-y]O2。
2. the preparation method of lithium-rich oxide anode material according to claim 1, it is characterised in that: the step 1)
The middle source Li is the mixture of one or more of lithium carbonate, lithium hydroxide, lithium nitrate and lithium acetate arbitrary proportion；The source Mn
For one in manganese oxide, manganous oxide, manganous hydroxide, hydroxide manganese, hydroxyl manganese oxide, manganese carbonate, manganese nitrate and manganese acetate
The mixture of kind or two or more arbitrary proportions；M source metal is in carbonate, hydroxide, nitrate and the acetate of M metal
One or more kinds of arbitrary proportions mixture；The molar ratio in the source Li, the source Mn and M source metal is (2-4x): (1-2x-
3y): 3y, in formula: 0 < x < 0.5,0 < y < x.
3. the preparation method of lithium-rich oxide anode material according to claim 1, it is characterised in that: the step 3)
The middle source Li is the mixture of one or more of lithium carbonate, lithium hydroxide, lithium nitrate and lithium acetate arbitrary proportion；The source Ni
For one in nickel oxide, nickel protoxide, nickel hydroxide, hickelous nydroxide, hydroxy nickel oxide, nickelous carbonate, nickel nitrate and nickel acetate
The mixture of kind or two or more arbitrary proportions；The source Mn is manganese oxide, manganous oxide, manganous hydroxide, hydroxide manganese, hydroxyl oxygen
Change the mixture of one or more of manganese, manganese carbonate, manganese nitrate and manganese acetate arbitrary proportion；M is metal-doped
Li2MnO3Material is (1-2x): 3x:(3x-3y with the molar ratio of Li, Ni and Mn being added)/2:(3x+3y)/2, in formula: 0 < x
< 0.5,0 < y < x.
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| CN113097475A (en) * | 2021-04-02 | 2021-07-09 | 上海科技大学 | Lithium-rich layered cathode material, preparation method thereof, battery cathode formed by lithium-rich layered cathode material and battery |
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