CN110364701A - Rodlike LiNi0.8Co0.1Mn0.1O2Preparation and method for coating and its lithium electricity anode in application - Google Patents
Rodlike LiNi0.8Co0.1Mn0.1O2Preparation and method for coating and its lithium electricity anode in application Download PDFInfo
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- CN110364701A CN110364701A CN201910497213.2A CN201910497213A CN110364701A CN 110364701 A CN110364701 A CN 110364701A CN 201910497213 A CN201910497213 A CN 201910497213A CN 110364701 A CN110364701 A CN 110364701A
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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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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- 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
The invention discloses rodlike LiNi0.8Co0.1Mn0.1O2Preparation and method for coating and its lithium electricity anode in application.First using the rodlike presoma of acid Co deposited synthesis, recycles solvent-thermal method that the crystallization water in rodlike presoma is hydrolyzed with the source Ti and react, form uniform clad on the surface of the material.The present invention and tradition utilize alkaline coprecipitation preparation LiNi0.8Co0.1Mn0.1O2Method compare, do not have to control pH and inert gas shielding not only, device is simple, is easy to largely prepare.And clad obtained by method for coating of the invention is thin and uniform, and embedded type cladding is formed after high-temperature process, and the stability of clad is high.LiNi after being coated with Li-Ti-O0.8Co0.1Mn0.1O2For the lithium ion battery of active material assembling, capacity retention ratio is 94.9% after 2.8-4.4V, 0.5C, 30 DEG C, 50 circles.
Description
Technical field
The present invention relates to the positive fields of lithium electricity, and in particular to rodlike LiNi0.8Co0.1Mn0.1O2Preparation and method for coating and
Its application in lithium electricity anode.
Background technique
Rich nickel tertiary cathode material LiNi0.8Co0.1Mn0.1O2It is considered as most potential substitution LiCoO2Positive electrode,
In addition, rich nickel tertiary cathode material is used for the positive electrode of lithium ion battery due to height ratio capacity and low cost.Tradition preparation
LiNi0.8Co0.1Mn0.1O2Method be alkaline coprecipitation, this method needs strict control pH, temperature and needs in inertia
It is carried out under environment, operates extremely inconvenient and required equipment costly.Here, proposing that acid coprecipitation is used for
LiNi0.8Co0.1Mn0.1O2Preparation, acid coprecipitation do not have to control pH without inert gas shielding, can grasp under room temperature
Make and can largely prepare.In addition, rich nickel tertiary cathode material is since first circle coulombic efficiency is low, and poor circulation, bad storage
Characteristic is deposited, high thermal instability leads to the unstability between electrode and electrolyte, is difficult commercial applications.Surface cladding is most
Widely used method improves rich nickel tertiary cathode material chemical property.However, the material of cladding is usually detrimental to just
The lithium ion conduction of pole material and the interfacial charge transfer of electrode, are not only isolated lithium ion conduction, also increase lithium ion diffusion length
Degree causes chemical property to deteriorate.Therefore, researcher has studied the material for improving lithium ion conduction and wraps as surface
Coating, for improving the cycle performance and thermal stability of rich nickel tertiary cathode material.In addition, preparing Li-Ti- using solvent-thermal method
The LiNi of O cladding0.8Co0.1Mn0.1O2, possess good chemical property.
Summary of the invention
The object of the invention is in order to solve LiNi0.8Co0.1Mn0.1O2Preparation and coat there are the problem of with defect and
There is provided a kind of simple to operation, the high preparation method of repeatability utilizes water of the crystallization water in predecessor during solvent heat
Solution reaction forms thin and uniform clad in rodlike oxide surface, and the Li- of embedded cladding is obtained using high-temperature calcination
Ti-O coats rodlike LiNi0.8Co0.1Mn0.1O2Positive electrode, and be successfully applied in lithium ion battery.
The purpose of the present invention is achieved through the following technical solutions.
Rodlike LiNi0.8Co0.1Mn0.1O2Preparation method, comprising the following steps:
(1) oxalic acid is subjected to acid coprecipitation reaction with the transition metal ion solution stoichiometrically mixed, filtered,
Washing, obtains rodlike oxalic acid presoma MC after drying2O4·2H2O, wherein M=Ni, Co, Mn；
(2) rodlike oxalic acid presoma obtained by step (1) is mixed with lithium salts, high-temperature calcination obtain it is rodlike
LiNi0.8Co0.1Mn0.1O2Positive electrode.
Further, the stoichiometric ratio is to be added in the ratio of Ni:Co:Mn=8:1:1.
Further, the transition metal ion solution refers to nickel sulfate, cobaltous sulfate, the mixed solution of manganese sulfate；It is described
Lithium salts be LiOH, Li2CO3And LiNO3One of or it is a variety of.
Further, the rate being vigorously stirred is 800rpm, time 10h.
Rodlike LiNi0.8Co0.1Mn0.1O2The method for coating of positive electrode, comprising the following steps:
The source Ti that can be hydrolyzed and oxalic acid presoma are subjected to solvent thermal reaction, then will be filtered, washing, the product after drying
It is mixed with lithium salts, then carries out high-temperature calcination and obtain the embedded cladding LiNi of Li-Ti-O0.8Co0.1Mn0.1O2Positive electrode；It is described
Oxalic acid presoma is MC2O4·2H2O, wherein M=Ni, Co, Mn.
Further, the source Ti is C16H36O4Ti；The lithium salts is LiOH.
Further, the solvent of the solvent thermal reaction is dehydrated alcohol, and temperature is 120-180 DEG C, further preferably
150 DEG C, time 4-8h, further preferably 6h.
Further, the atmosphere of the high-temperature calcination be oxygen atmosphere, temperature be 750-850 DEG C, further preferably 800
DEG C, time 10-12h, further preferably 12h, heating rate are 5-10 DEG C/min, further preferably 5 DEG C/min.
Further, the temperature of the drying is 80-100 DEG C, further preferably 80 DEG C.
Further, cladding ratio of the Li-Ti-O in positive electrode is 1mol%, 3mol%, 5mol%.
Further, a certain amount of oxalic acid is first reacted with the cobaltous sulfate of half, is vigorously stirred, forms rodlike cobalt oxalate, after
(nickel oxalate, cobalt oxalate, the content of manganese oxalate is according to stoichiometry for oxalic acid and nickel sulfate, manganese sulfate and the reaction of remaining cobaltous sulfate
Than being added) form oxalic acid presoma MC2O4·2H2O (M=Ni, Co, Mn), by drug and oxalic acid presoma MC2O4·2H2O (M=
Ni, Co, Mn) for a period of time, filtering, the product after washing and drying mixes hydro-thermal reaction with lithium salts at a certain temperature, then into
Row high-temperature calcination obtains the LiNi of different proportion cladding Li-Ti-O0.8Co0.1Mn0.1O2Positive electrode.
Further, it is vigorously stirred as 800rpm, time 10h, solvent is water, and the drug is C16H36O4Ti,
The solvent heat time is 4-8h, further preferably 6h；Solvent is dehydrated alcohol, and the drug is C16H36O4Ti, when solvent heat
Between be 4-8h, further preferably 6h；The lithium salts is LiOH.
Further, the stoichiometric ratio is Ni:Co:Mn=8:1:1, and the high-temperature calcination is 750-850
DEG C, further preferably 800 DEG C, calcination time 10-12h, further preferably 12h, the high-temperature calcination atmosphere is oxygen
Gas atmosphere, rate are 5-10 DEG C/min, and further preferably 5 DEG C/min, the drying temperature is 80-100 DEG C, further excellent
It is selected as 80 DEG C.
Further, the oxalic acid first and the cobaltous sulfate of half react to be formed rodlike cobalt oxalate mainly formed it is rodlike
Cobalt oxalate template, so as to the rodlike LiNi of subsequent synthesis0.8Co0.1Mn0.1O2。
Further, the capacity is largely provided by Ni, and the Li-Ti-O clad that solvent-thermal method obtains stablizes knot
Structure improves stability.
Further, different proportion Li-Ti-O cladding is 1mol%, 3mol%, 5mol%.
Further, clad 1-2nm.
The embedded cladding LiNi of Li-Ti-O prepared by the process described above0.8Co0.1Mn0.1O2Positive electrode.
The above-described embedded cladding LiNi of Li-Ti-O0.8Co0.1Mn0.1O2Positive electrode answering in lithium electricity anode
With by the embedded cladding LiNi of the Li-Ti-O0.8Co0.1Mn0.1O2Positive electrode and conductive additive, binder are mixed with
Positive electrode is applied in lithium ion battery.
Compared with prior art, the invention has the advantages that and effect:
(1) LiNi is prepared with tradition0.8Co0.1Mn0.1O2Alkaline coprecipitation compare, acid coprecipitation of the invention
Do not have to control pH not only can be operated, and device is simple without inert gas shielding under room temperature, be easy to largely prepare.
(2) LiNi is coated with tradition0.8Co0.1Mn0.1O2Method compare, solvent-thermal method of the invention is not only easy to operate,
It is repeated high, and the clad, thin and uniform of 1-2nm thickness is obtained, be conducive to the promotion of circulating battery stability.
(3) the embedded cladding LiNi of Li-Ti-O that the present invention is prepared0.8Co0.1Mn0.1O2Positive electrode is put with height
The features such as capacitance, high rate capability, good circulation stability.Applied to showing excellent electrochemistry in lithium ion battery
Energy.With the embedded cladding LiNi of Li-Ti-O0.8Co0.1Mn0.1O2Positive electrode is active material, and conductive black is conductive agent, is gathered
Vinylidene is binder, and three kinds of materials are uniformly mixed, and is coated on aluminium foil, and using lithium piece as cathode, diaphragm is PP diaphragm, carbon
Acid propylene ester is electrolyte, assembles lithium ion battery in argon gas glove box.The capacity after 2.8-4.4V, 0.5C, 30 DEG C, 50 circles
Conservation rate is 94.9%.
Detailed description of the invention
Fig. 1 is that 3mol%Li-Ti-O prepared by embodiment 3 coats LiNi0.8Co0.1Mn0.1O2The XRD diagram of positive electrode.
Fig. 2 is that 3mol%Li-Ti-O prepared by embodiment 3 coats LiNi0.8Co0.1Mn0.1O2The SEM of positive electrode schemes.
Fig. 3 is that 3mol%Li-Ti-O prepared by embodiment 3 coats LiNi0.8Co0.1Mn0.1O2Appearance of the positive electrode in 0.5C
Measure conservation rate curve graph.
Specific embodiment
Specific implementation of the invention is further described below in conjunction with example and attached drawing, but embodiments of the present invention
It is without being limited thereto.
Embodiment 1
When preparing rodlike LiNi0.8Co0.1Mn0.1O2When, stoichiometrically 200mL oxalic acid is first mixed with 1.54g cobaltous sulfate
Stirring, reaction 1h obtain rodlike cobalt oxalate, and afterwards with 20.50g nickel sulfate, 1.54g cobaltous sulfate, 1.66g manganese sulfate mixed solution is total
Precipitation reaction, room temperature, 800rpm/min are vigorously stirred 10h, filter, washing, dry at 80 DEG C, obtain oxalic acid presoma MC2O4·
2H2O (M=Ni, Co, Mn).Take 2.279g MC2O4·2H2O (M=Ni, Co, Mn) and 0.552g LiOH, mixed grinding, 500
DEG C calcining 6h, 800 DEG C of calcining 12h.Membrane and assembled battery are carried out afterwards.Capacity retention ratio is 86.5% after 50 circles.
Embodiment 2
When Li-Ti-O cladding ratio is 1mol%, stoichiometrically 200mL oxalic acid is first mixed with 1.54g cobaltous sulfate
Stirring, reaction 1h obtain rodlike cobalt oxalate, and afterwards with 20.50g nickel sulfate, 1.54g cobaltous sulfate, 1.66g manganese sulfate mixed solution is total
Precipitation reaction, room temperature, 800rpm/min are vigorously stirred 10h, filter, washing, dry at 80 DEG C, obtain oxalic acid presoma MC2O4·
2H2O (M=Ni, Co, Mn).By 0.019g C16H36O4Ti and 1.000g oxalic acid presoma MC2O4·2H2O (M=Ni, Co, Mn)
Mixing is dissolved in 50mL dehydrated alcohol and is placed in water heating kettle, 120 DEG C of solvent thermal reaction 4h, filters, washing, dries at 100 DEG C, after
It is mixed with 0.235gLiOH, under oxygen atmosphere, 500 DEG C of calcinings 6h, 750 DEG C of calcining 10h are rear to carry out membrane and assembled battery.50
Capacity retention ratio is 89.4% after circle.
Embodiment 3
When Li-Ti-O cladding ratio is 3mol%, stoichiometrically 200mL oxalic acid is first mixed with 1.54g cobaltous sulfate
Stirring, reaction 1h obtain rodlike cobalt oxalate, and afterwards with 20.50g nickel sulfate, 1.54g cobaltous sulfate, 1.66g manganese sulfate mixed solution is total
Precipitation reaction, room temperature, 800rpm/min are vigorously stirred 10h, filter, washing, dry at 80 DEG C, obtain oxalic acid presoma MC2O4·
2H2O (M=Ni, Co, Mn).By 0.056g C16H36O4Ti and 1.000g oxalic acid presoma MC2O4·2H2O (M=Ni, Co, Mn)
Mixing is dissolved in 50mL dehydrated alcohol and is placed in water heating kettle, 150 DEG C of solvent thermal reaction 6h, filters, washing, dries at 80 DEG C, after
It is mixed with 0.244gLiOH, under oxygen atmosphere, 500 DEG C of calcinings 6h, 800 DEG C of calcining 12h are rear to carry out membrane and assembled battery.
3mol%Li-Ti-O manufactured in the present embodiment coats LiNi0.8Co0.1Mn0.1O2The XRD diagram of positive electrode is shown in Fig. 1,
The XRD diagram illustrates LiNi0.8Co0.1Mn0.1O2With six side a-NaFeO2Structure, R-3m space group, the obvious swarming of adjacent peak
((006)/(102) and (108)/(110)) show that all samples form orderly layer structure.
3mol%Li-Ti-O manufactured in the present embodiment coats LiNi0.8Co0.1Mn0.1O2The SEM figure of positive electrode is shown in Fig. 2.
The LiNi synthesized as seen from Figure 20.8Co0.1Mn0.1O2Club shaped structure is presented.
3mol%Li-Ti-O manufactured in the present embodiment coats LiNi0.8Co0.1Mn0.1O2Capacity of the positive electrode in 0.5C is protected
Holdup curve graph is shown in Fig. 3.It is 94.9% by the available capacity retention ratio of Fig. 3, shows LiNi0.8Co0.1Mn0.1O2With excellent
Cyclical stability.
Embodiment 4
When Li-Ti-O cladding ratio is 5mol%, stoichiometrically 200mL oxalic acid is first mixed with 1.54g cobaltous sulfate
Stirring, reaction 1h obtain rodlike cobalt oxalate, and afterwards with 20.50g nickel sulfate, 1.54g cobaltous sulfate, 1.66g manganese sulfate mixed solution is total
Precipitation reaction, room temperature, 800rpm/min are vigorously stirred 10h, filter, washing, dry at 80 DEG C, by 0.115g C16H36O4Ti with
1.115g oxalic acid presoma MC2O4·2H2O (M=Ni, Co, Mn) mixing is dissolved in 50mL dehydrated alcohol and is placed in water heating kettle, and 180
DEG C solvent thermal reaction 8h is filtered, washing, is dried at 90 DEG C, mix afterwards with 0.266gLiOH, and under oxygen atmosphere, 500 DEG C are calcined
6h, 850 DEG C of calcining 11h, it is rear to carry out membrane and assembled battery.Capacity retention ratio is 90.9% after 50 circles.
Claims (10)
1. rodlike LiNi0.8Co0.1Mn0.1O2Preparation method, which comprises the following steps:
(1) oxalic acid is subjected to acid coprecipitation reaction with the transition metal ion solution stoichiometrically mixed, filtering is washed
It washs, rodlike oxalic acid presoma MC is obtained after drying2O4·2H2O, wherein M=Ni, Co, Mn；
(2) rodlike oxalic acid presoma obtained by step (1) is mixed with lithium salts, high-temperature calcination obtains rodlike LiNi0.8Co0.1Mn0.1O2
Positive electrode.
2. preparation method according to claim 1, which is characterized in that the stoichiometric ratio is by Ni:Co:Mn=8:
The ratio of 1:1 is added.
3. preparation method according to claim 1, which is characterized in that the transition metal ion solution refers to nickel sulfate,
Cobaltous sulfate, the mixed solution of manganese sulfate；The lithium salts is LiOH, Li2CO3And LiNO3One of or it is a variety of.
4. rodlike LiNi0.8Co0.1Mn0.1O2The method for coating of positive electrode, which comprises the following steps:
The source Ti that can be hydrolyzed and oxalic acid presoma are subjected to solvent thermal reaction, then will be filtered, washing, product and lithium after drying
Then salt mixing carries out high-temperature calcination and obtains the embedded cladding LiNi of Li-Ti-O0.8Co0.1Mn0.1O2Positive electrode；The oxalic acid
Presoma is MC2O4·2H2O, wherein M=Ni, Co, Mn.
5. method for coating according to claim 4, which is characterized in that the source Ti is C16H36O4Ti；The lithium salts is
LiOH。
6. method for coating according to claim 4, which is characterized in that the solvent of the solvent thermal reaction is dehydrated alcohol,
Temperature is 150-180 DEG C, time 4-8h.
7. method for coating according to claim 4, which is characterized in that the atmosphere of the high-temperature calcination is oxygen atmosphere, temperature
Degree is 750-850 DEG C, time 10-12h, and heating rate is 5-10 DEG C/min.
8. method for coating according to claim 4, which is characterized in that cladding ratio of the Li-Ti-O in positive electrode
Example is 1mol%, 3mol%, 5mol%.
9. by the embedded cladding LiNi of Li-Ti-O prepared by method according to any one of claims 80.8Co0.1Mn0.1O2Positive electrode.
10. the embedded cladding LiNi of Li-Ti-O as claimed in claim 90.8Co0.1Mn0.1O2Positive electrode is in lithium electricity anode
Using, which is characterized in that by the embedded cladding LiNi of the Li-Ti-O0.8Co0.1Mn0.1O2Positive electrode and conductive additive,
Binder is mixed with positive electrode, is applied in lithium ion battery.
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2019
- 2019-06-10 CN CN201910497213.2A patent/CN110364701A/en active Pending
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| CN103700834A (en) * | 2012-09-27 | 2014-04-02 | 清华大学 | Preparation method for lithium ion battery anode composite material |
| WO2016025866A1 (en) * | 2014-08-15 | 2016-02-18 | Quantumscape Corporation | Doped conversion materials for secondary battery cathodes |
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| CN106910874A (en) * | 2017-03-03 | 2017-06-30 | 北京理工大学 | A kind of Surface coating Li2TiO3With the high-nickel material and preparation method of top layer doping Ti |
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