CN107293718A - R2‑xMxEMnO6Modified Nickel lithium manganate material and preparation, application - Google Patents
R2‑xMxEMnO6Modified Nickel lithium manganate material and preparation, application Download PDFInfo
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- CN107293718A CN107293718A CN201710495102.9A CN201710495102A CN107293718A CN 107293718 A CN107293718 A CN 107293718A CN 201710495102 A CN201710495102 A CN 201710495102A CN 107293718 A CN107293718 A CN 107293718A
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
The invention discloses a kind of R2‑xMxEMnO6Modified Nickel lithium manganate material and preparation, application, belong to field of material technology, and rare earth metal salt, alkali salt, Ferrious material salt and manganese salt are 2 x in molar ratio by the preparation method：x：1：Dissolving obtains mixed solution in 1 addition solvent；Complexing agent is added into mixed solution, nickel ion doped is added or nickel ion doped presoma stirs, heating evaporation obtains gel；By gel drying, calcining obtains R2‑xMxEMnO6Modified Nickel lithium manganate material.The present invention uses the R of structure of double perovskite2‑ xMxEMnO6Material has the ionic conductivity that good electronic conductivity is become reconciled, and nickel ion doped material efficiency, high rate performance first is improved, while the R of structure of double perovskite2‑xMxEMnO6Material structure is stable, the effective contact for preventing nickel lithium manganate cathode material with electrolyte, realizes the cycle life for improving lithium ion battery.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, more particularly to a kind of R2-xMxEMnO6Modified Nickel mangaic acid
Lithium material and its preparation, application.
Background technology
Since 1990s, commercialized performance of lithium ion battery there has been very big raising, but up to the present,
Cell electrodes material is still with cobalt acid lithium LiCoO in commercialization consumption2Based on.Although LiCoO2It is negative pole for positive pole, Carbon Materials
Lithium ion battery security, which has, largely to be improved, but for high power capacity, high-power power-type lithium ion battery,
Its cost and security are the key problems primarily solved.Due to LiCoO2Cost is high, overcharge resistance performance is poor, is not suitable for power
Type anode material for lithium-ion batteries, and Co elements are very expensive, and have certain toxicity, so in the urgent need to exploitation is more closed
The new electrode material of reason.In a series of electrode materials newly developed, nickel ion doped causes the great interest of numerous researchers,
LiNi0.5Mn1.5O2Cheap, higher voltage platform, charge/discharge capacity be big and the advantages of security, it is substituted LiCoO2
Ideal electrode material, and can as power-type electrokinetic cell positive electrode.
LiNi0.5Mn1.5O2Although with higher specific capacity, structural stability is poor, and the LiMn2O4 of nickel doping is because of tool
There is higher voltage platform, corresponding energy density is higher, but its cycle performance is poor, especially under the high temperature conditions, discharge and recharge
During Mn be soluble in electrolyte, cause LiNi0.5Mn1.5O2Structure it is unstable, cause circulation be deteriorated.
The content of the invention
The technical problem existed based on background technology, the present invention proposes a kind of R2-xMxEMnO6Modified Nickel lithium manganate material
And its prepare, apply, using the R of structure of double perovskite2-xMxEMnO6Material structure is stable, and with good electronic conductivity
The ionic conductivity become reconciled, can prevent contact of the nickel ion doped with electrolyte well as the covering material of nickel ion doped, and
The migration of electronics and the conductance of ion are not hindered, realize cycle life, first efficiency and the high rate performance for improving lithium ion battery.
A kind of R proposed by the present invention2-xMxEMnO6Modified Nickel lithium manganate material, including nickel ion doped, and it is coated on nickel mangaic acid
Lithium outside and the R with structure of double perovskite2-xMxEMnO6Material, wherein 0≤x≤0.5.
Preferably, R is rare earth metal.
Preferably, R is Nd elements, Pm elements, Eu elements, Gd elements, Tb elements, Dy elements or Yb elements.
Preferably, M is alkaline-earth metal.
Preferably, M is Ca elements or Ba elements.
Preferably, E is Ferrious material.
Preferably, E is Ni elements or Co elements.
A kind of R that the present invention is also proposed2-xMxEMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by rare earth metal salt, alkali salt, Ferrious material salt and manganese salt in molar ratio be 2-x：x：1：1 addition is molten
Dissolving obtains mixed solution in agent；
S2, complexing agent is added into mixed solution, add nickel ion doped or nickel ion doped presoma stirs, heated
Evaporation obtains gel；By gel drying, calcining obtains R2-xMxEMnO6Modified Nickel lithium manganate material.
Preferably, in S1, rare earth metal salt and alkali salt is in villaumite, alkoxide, nitrate, carbonate or acetates
It is at least one.
Preferably, in S1, solvent is distilled water or ethanol.
Preferably, in S2, the amount of metal ion total material is a in mixed solution, and the amount of complexing agent material is b, a：B=1：
2-3。
Preferably, in S2, complexing agent is citric acid.
Preferably, in S2, nickel ion doped or nickel ion doped presoma and R2-xMxEMnO6The mass ratio of material is 100：0.5-
1, wherein the quality of nickel ion doped presoma is based on gained nickel ion doped.
Preferably, in S2, calcination environment is pure oxygen atmosphere or air atmosphere, and calcining heat is 750-1000 DEG C.
Preferably, in S2 calcination process, there is following relation in calcining heat T and heating-up time t：T=t × lgt+750；
Wherein T for calcining temperature value, unit for DEG C, t is that, from room temperature to calcining heat T time, unit is min, 1≤t≤
120。
The invention also provides a kind of R2-xMxEMnO6Modified Nickel lithium manganate material answering in anode material for lithium-ion batteries
With.
The beneficial effects of the invention are as follows：
(1) R of structure of double perovskite2-xMxEMnO6With good electronic conductivity and ionic conductivity, using double calcium titaniums
The R of ore deposit structure2-xMxEMnO6Cladding nickel lithium manganate cathode material can effectively improve nickel ion doped material efficiency, forthright again first
Energy；
(2) R of structure of double perovskite2-xMxEMnO6Stability Analysis of Structures, uses the R of structure of double perovskite2-xMxEMnO6Coat nickel
LiMn2O4 can effectively prevent contact of the nickel ion doped with electrolyte as anode material of lithium battery, realize and improve lithium ion battery
Cycle life；
(3) in calcination process, there is following relation in calcining heat with the heating-up time：T=t × lgt+750, makes R2- xMxEMnO6In nickel ion doped surface uniform fold, strengthen the R of structure of double perovskite2-xMxEMnO6Stabilization on nickel ion doped surface
Property, the battery performance of nickel ion doped material can be further lifted, battery cycle life is improved.
Brief description of the drawings
Fig. 1 is the gained Dy of the embodiment of the present invention 11.5Ca0.5NiMnO6The circulation of Modified Nickel lithium manganate material and nickel ion doped
Charging and discharging curve figure.
Fig. 2 is the gained Dy of the embodiment of the present invention 11.5Ca0.5NiMnO6Modified Nickel lithium manganate material is with nickel ion doped in difference
Discharge curve under multiplying power.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of R2-xMxEMnO6Modified Nickel lithium manganate material, including nickel ion doped, and be coated on the outside of nickel ion doped and have
The R of structure of double perovskite2CoMnO6Material.
Embodiment 2
A kind of R2-xMxEMnO6Modified Nickel lithium manganate material, including nickel ion doped, and be coated on the outside of nickel ion doped and have
The R of structure of double perovskite1.5M0.5NiMnO6Material.
Embodiment 3
A kind of R2-xMxEMnO6Modified Nickel lithium manganate material, including nickel ion doped, and be coated on the outside of nickel ion doped and have
The R of structure of double perovskite1.5M0.5CoMnO6Material.
Wherein R is Nd elements, Pm elements, Eu elements, Gd elements, Tb elements, Dy elements or Yb elements；M be Ca elements or
Ba elements.
Embodiment 4
Dy1.5Ca0.5NiMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by Dy (NO3)3·6H2O、Ca(NO3)2·6H2O、Ni(NO3)2·6H2O and Mn (NO3)2·6H2O is in molar ratio
For 1.5：0.5：1：Dissolving obtains mixed solution in 1 addition distilled water；
S2, added into mixed solution the total material of metal ion in citric acid, mixed solution amount be a, citric acid
The amount of material is b, a：B=1：2, add nickel ion doped and stir, nickel ion doped and Dy1.5Ca0.5NiMnO6The matter of material
Amount is than being 100：0.5；Heating evaporation obtains gel；By gel drying, under pure oxygen atmosphere, 850 DEG C of calcinings are obtained
Dy1.5Ca0.5NiMnO6Modified Nickel lithium manganate material.
Embodiment 5
Dy2NiMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by Dy (NO3)3·6H2O、Ni(NO3)2·6H2O and Mn (NO3)2·6H2O is 2 in molar ratio：1：1 adds steaming
Dissolving obtains mixed solution in distilled water；
S2, added into mixed solution the total material of metal ion in citric acid, mixed solution amount be a, citric acid
The amount of material is b, a：B=1：2, add nickel ion doped and stir, nickel ion doped and Dy2NiMnO6The mass ratio of material is
100：1；Heating evaporation obtains gel；By gel drying, under pure oxygen atmosphere, 850 DEG C of calcinings obtain Dy2NiMnO6Modified Nickel mangaic acid
Lithium material.
Embodiment 6
Dy1.5Ca0.5NiMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by Dy (NO3)3·6H2O、Ca(NO3)2·6H2O、Ni(NO3)2·6H2O and Mn (NO3)2·6H2O is in molar ratio
For 1.5：0.5：1：Dissolving obtains mixed solution in 1 addition distilled water；
S2, added into mixed solution the total material of metal ion in citric acid, mixed solution amount be a, citric acid
The amount of material is b, a：B=1：3, add nickel ion doped presoma and stir；Nickel ion doped presoma is pressed into gained nickel manganese
Sour lithium meter, then nickel ion doped presoma and Dy1.5Ca0.5NiMnO6The mass ratio of material is 100：0.5；Heating evaporation is coagulated
Glue；By gel drying, under pure oxygen atmosphere, 850 DEG C of calcinings obtain Dy1.5Ca0.5NiMnO6Modified Nickel lithium manganate material.
Embodiment 7
Eu1.5Ba0.5CoMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by Eu (NO3)3·6H2O、Ba(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO3)2·6H2O is in molar ratio
For 1.5：0.5：1：Dissolving obtains mixed solution in 1 addition absolute ethyl alcohol；
S2, added into mixed solution the total material of metal ion in citric acid, mixed solution amount be a, citric acid
The amount of material is b, a：B=1：2, add nickel ion doped and stir, nickel ion doped and Eu1.5Ba0.5CoMnO6The matter of material
Amount is than being 100：0.5；Heating evaporation obtains gel；By gel drying, under pure oxygen atmosphere, 750 DEG C of calcinings are obtained
Eu1.5Ba0.5CoMnO6Modified Nickel lithium manganate material.
Embodiment 8
Eu1.5Ba0.5CoMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by Eu (NO3)3·6H2O、Ba(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO3)2·6H2O is in molar ratio
For 1.5：0.5：1：Dissolving obtains mixed solution in 1 addition absolute ethyl alcohol；
S2, added into mixed solution the total material of metal ion in citric acid, mixed solution amount be a, citric acid
The amount of material is b, a：B=1：2, add nickel ion doped and stir, nickel ion doped and Eu1.5Ba0.5CoMnO6The matter of material
Amount is than being 100：0.5；Heating evaporation obtains gel；By gel drying, under pure oxygen atmosphere, 1000 DEG C of calcinings are obtained
Eu1.5Ba0.5CoMnO6Modified Nickel lithium manganate material.
Embodiment 9
Dy1.5Ca0.5NiMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by Dy (NO3)3·6H2O、Ca(NO3)2·6H2O、Ni(NO3)2·6H2O and Mn (NO3)2·6H2O is in molar ratio
For 1.5：0.5：1：Dissolving obtains mixed solution in 1 addition distilled water；
S2, added into mixed solution the total material of metal ion in complexing agent, mixed solution amount be a, complexing agent
The amount of material is b, a：B=1：2, add nickel ion doped and stir, nickel ion doped and Dy1.5Ca0.5NiMnO6The matter of material
Amount is than being 100：0.5；Heating evaporation obtains gel；By gel drying, under pure oxygen atmosphere, from room temperature to 750 DEG C of calcinings, rise
The warm time is 1min, obtains Dy1.5Ca0.5NiMnO6Modified Nickel lithium manganate material.
Embodiment 10
Dy2NiMnO6The preparation method of Modified Nickel lithium manganate material, comprises the following steps：
S1, by Dy (NO3)3·6H2O、Ni(NO3)2·6H2O and Mn (NO3)2·6H2O is 2 in molar ratio：1：1 adds steaming
Dissolving obtains mixed solution in distilled water；
S2, added into mixed solution the total material of metal ion in complexing agent, mixed solution amount be a, complexing agent
The amount of material is b, a：B=1：2.5, add nickel ion doped and stir, nickel ion doped and Dy2NiMnO6The mass ratio of material
For 100：0.8；Heating evaporation obtains gel；By gel drying, under pure oxygen atmosphere, from room temperature to 1000 DEG C of calcinings, heating
Time is 120min, obtains Dy2NiMnO6Modified Nickel lithium manganate material.
R described in embodiment 1-102-xMxEMnO6Modified Nickel lithium manganate material can be used for preparing anode material for lithium-ion batteries.
Using the gained Dy of embodiment 11.5Ca0.5NiMnO6Modified Nickel lithium manganate material and nickel ion doped are respectively as lithium ion
Cell positive material carries out electrical property detection, as depicted in figs. 1 and 2, and Fig. 1 is the gained R of the embodiment of the present invention 12-xMxEMnO6It is modified
The cycle charge-discharge curve map of nickel ion doped material and nickel ion doped, Fig. 2 is the gained R of the embodiment of the present invention 12-xMxEMnO6It is modified
Nickel ion doped material and discharge curve of the nickel ion doped under different multiplying.From Fig. 1 and Fig. 2, present invention gained R2- xMxEMnO6Modified Nickel lithium manganate material can improve the cycle life of lithium ion battery, the specific discharge capacity under different multiplying
It is bigger.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of R2-xMxEMnO6Modified Nickel lithium manganate material, it is characterised in that including nickel ion doped, and it is coated on nickel ion doped
Outside and the R with structure of double perovskite2-xMxEMnO6Material, wherein 0≤x≤0.5.
2. R according to claim 12-xMxEMnO6Modified Nickel lithium manganate material, it is characterised in that R is rare earth metal；It is preferred that
Ground, R is Nd elements, Pm elements, Eu elements, Gd elements, Tb elements, Dy elements or Yb elements.
3. R according to claim 12-xMxEMnO6Modified Nickel lithium manganate material, it is characterised in that M is alkaline-earth metal；It is preferred that
Ground, M is Ca elements or Ba elements.
4. R according to claim 12-xMxEMnO6Modified Nickel lithium manganate material, it is characterised in that E is Ferrious material；It is preferred that
Ground, E is Ni elements or Co elements.
5. one kind R as described in claim any one of 1-42-xMxEMnO6The preparation method of Modified Nickel lithium manganate material, its feature exists
In comprising the following steps：
S1, by rare earth metal salt, alkali salt, Ferrious material salt and manganese salt in molar ratio be 2-x：x：1：1 adds in solvent
Dissolving obtains mixed solution；
S2, complexing agent is added into mixed solution, add nickel ion doped or nickel ion doped presoma stirs, heating evaporation
Obtain gel；By gel drying, calcining obtains R2-xMxEMnO6Modified Nickel lithium manganate material.
6. R according to claim 52-xMxEMnO6The preparation method of Modified Nickel lithium manganate material, it is characterised in that in S1, it is dilute
Earth metal salt and alkali salt are at least one of villaumite, alkoxide, nitrate, carbonate or acetate；Preferably, in S1,
Solvent is distilled water or ethanol.
7. R according to claim 52-xMxEMnO6The preparation method of Modified Nickel lithium manganate material, it is characterised in that in S2, is mixed
The amount for closing metal ion in solution total material is a, and the amount of complexing agent material is b, a：B=1：2-3；Preferably, complexing agent is lemon
Lemon acid.
8. R according to claim 52-xMxEMnO6The preparation method of Modified Nickel lithium manganate material, it is characterised in that in S2, nickel
LiMn2O4 or nickel ion doped presoma and R2-xMxEMnO6The mass ratio of material is 100：0.5-1's, wherein nickel ion doped presoma
Quality is based on gained nickel ion doped.
9. according to any one of the claim 1-8 R2-xMxEMnO6The preparation method of Modified Nickel lithium manganate material, its feature exists
In in S2, calcination environment is pure oxygen atmosphere or air atmosphere, and calcining heat is 750-1000 DEG C；Preferably, S2 calcination process
In, there is following relation in calcining heat T and heating-up time t：T=t × lgt+750；Wherein T is the temperature value of calcining, and unit is
DEG C, t is that unit is min, 1≤t≤120 from room temperature to calcining heat T time.
10. one kind R as described in claim any one of 1-52-xMxEMnO6Modified Nickel lithium manganate material is in lithium ion cell positive material
Application in material.
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| CN107293718B (en) | 2020-05-26 |
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