CN107293718B - R2-xMxEMnO6Modified lithium nickel manganese oxide material, preparation and application - Google Patents
R2-xMxEMnO6Modified lithium nickel manganese oxide material, preparation and application Download PDFInfo
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- 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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- H01M4/525—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 a compound R2‑xMxEMnO6The preparation method comprises the following steps of mixing rare earth metal salt, alkaline earth metal salt, iron series metal salt and manganese salt according to a molar ratio of 2-x: x: 1: 1 adding the mixture into a solvent to dissolve the mixture to obtain a mixed solution; adding a complexing agent into the mixed solution, adding lithium nickel manganese oxide or a lithium nickel manganese oxide precursor, uniformly stirring, heating and evaporating to obtain gel; drying and calcining the gel to obtain R2‑xMxEMnO6A modified lithium nickel manganese oxide material. The invention adopts R with a double perovskite structure2‑ xMxEMnO6The material has good electronic conductivity and good ionic conductivity, improves the first efficiency and rate capability of the lithium nickel manganese oxide material, and simultaneously has the R of a double perovskite structure2‑xMxEMnO6The material has a stable structure, effectively prevents the lithium nickel manganese oxide anode material from contacting with electrolyte, and prolongs the cycle life of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a lithium ion battery anode material2-xMxEMnO6Modified lithium nickel manganese oxide material and preparation and application thereof.
Background
The performance of commercial lithium ion batteries has been greatly improved since the 90 s in the 20 th century, but the commercial consumer electronics electrode material still uses lithium cobaltate LiCoO to date2Mainly comprises the following steps.Despite the LiCoO2The safety of the lithium ion battery with the anode made of the carbon material and the cathode made of the carbon material is greatly improved, but the cost and the safety of the high-capacity and high-power lithium ion battery are the core problems to be solved in the first place. Due to LiCoO2The cost is high, the overcharge resistance is poor, the material is not suitable for being used as a positive electrode material of a power lithium ion battery, and Co element is very expensive and has certain toxicity, so that the development of a more reasonable new electrode material is urgently needed. Among a series of newly developed electrode materials, lithium nickel manganese has attracted great interest of extensive researchers, and LiNi0.5Mn1.5O2Low price, high voltage platform, large charge-discharge capacity and safety, etc., so that it can replace LiCoO2The electrode material is ideal and can be used as the anode material of the power type power battery.
LiNi0.5Mn1.5O2Although the lithium manganate has higher specific capacity, the structural stability is poor, the nickel-doped lithium manganate has higher corresponding energy density due to higher voltage platform, but the cycle performance is poor, and particularly under the high temperature condition, Mn is easy to dissolve in electrolyte in the charging and discharging process, so LiNi is caused0.5Mn1.5O2The structure is unstable, resulting in poor cycle.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides a R2-xMxEMnO6Modified lithium nickel manganese oxide material, preparation and application thereof, and preparation method and application thereof by adopting double perovskite structure R2-xMxEMnO6The material has a stable structure, has good electronic conductivity and good ionic conductivity, can be well used as a coating material of the lithium nickel manganese oxide, prevents the lithium nickel manganese oxide from contacting with electrolyte, does not block the migration of electrons and the ionic conductivity, and realizes the improvement of the cycle life, the first efficiency and the rate capability of the lithium ion battery.
The invention provides a compound R2-xMxEMnO6The modified lithium nickel manganese oxide material comprises lithium nickel manganese oxide and R which is coated on the outer side of the lithium nickel manganese oxide and has a double perovskite structure2-xMxEMnO6Wherein x is more than or equal to 0 and less than or equal to 0.5.
Preferably, R is a rare earth metal.
Preferably, R is an Nd element, a Pm element, an Eu element, a Gd element, a Tb element, a Dy element, or a Yb element.
Preferably, M is an alkaline earth metal.
Preferably, M is Ca element or Ba element.
Preferably, E is an iron-based metal.
Preferably, E is an Ni element or a Co element.
The invention also provides a preparation method of the compound2-xMxEMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, mixing rare earth metal salt, alkaline earth metal salt, iron series metal salt and manganese salt according to the molar ratio of 2-x: x: 1: 1 adding the mixture into a solvent to dissolve the mixture to obtain a mixed solution;
s2, adding a complexing agent into the mixed solution, adding lithium nickel manganese oxide or a lithium nickel manganese oxide precursor, uniformly stirring, and heating and evaporating to obtain gel; drying and calcining the gel to obtain R2-xMxEMnO6A modified lithium nickel manganese oxide material.
Preferably, in S1, the rare earth metal salt and the alkaline earth metal salt are at least one of chloride, alkoxide, nitrate, carbonate or acetate.
Preferably, in S1, the solvent is distilled water or ethanol.
Preferably, in S2, the total amount of metal ions in the mixed solution is a, the amount of the complexing agent substance is b, a: b is 1: 2-3.
Preferably, in S2, the complexing agent is citric acid.
Preferably, in S2, lithium nickel manganese oxide or lithium nickel manganese oxide precursor is reacted with R2-xMxEMnO6The mass ratio of the materials is 100: 0.5-1, wherein the mass of the lithium nickel manganese oxide precursor is calculated according to the obtained lithium nickel manganese oxide.
Preferably, in S2, the calcination environment is pure oxygen atmosphere or air atmosphere, and the calcination temperature is 750-1000 ℃.
Preferably, in the calcination process of S2, the calcination temperature T and the temperature rise time T have the following relationship: t × lgt + 750; wherein T is the temperature value of calcination, the unit is DEG C, T is the time for heating from room temperature to the calcination temperature T, the unit is min, and T is more than or equal to 1 and less than or equal to 120.
The invention also provides a method for preparing the compound2-xMxEMnO6The modified lithium nickel manganese oxide material is applied to the anode material of the lithium ion battery.
The invention has the beneficial effects that:
(1) r of double perovskite structure2-xMxEMnO6Has good electronic conductivity and ionic conductivity, and adopts R with double perovskite structure2-xMxEMnO6The coated lithium nickel manganese oxide positive electrode material can effectively improve the first efficiency and rate performance of the lithium nickel manganese oxide material;
(2) r of double perovskite structure2-xMxEMnO6Stable structure, R using double perovskite structure2-xMxEMnO6The coated lithium nickel manganese oxide can effectively prevent the lithium nickel manganese oxide from contacting with electrolyte when being used as a lithium battery anode material, so that the cycle life of the lithium ion battery is prolonged;
(3) in the calcining process, the calcining temperature and the temperature rise time have the following relationship: t is T × lgt +750, and R is2- xMxEMnO6Uniformly covering the surface of the lithium nickel manganese oxide to enhance the R of a double perovskite structure2-xMxEMnO6The stability on the surface of the lithium nickel manganese oxide can further improve the battery performance of the lithium nickel manganese oxide material and prolong the cycle life of the battery.
Drawings
FIG. 1 shows Dy obtained in example 4 of the present invention1.5Ca0.5NiMnO6And (3) a cyclic charge-discharge curve diagram of the modified lithium nickel manganese oxide material and lithium nickel manganese oxide.
FIG. 2 shows Dy obtained in example 4 of the present invention1.5Ca0.5NiMnO6And (3) a discharge curve diagram of the modified lithium nickel manganese oxide material and the lithium nickel manganese oxide under different multiplying powers.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
R2-xMxEMnO6The modified lithium nickel manganese oxide material comprises lithium nickel manganese oxide and R which is coated on the outer side of the lithium nickel manganese oxide and has a double perovskite structure2CoMnO6A material.
Example 2
R2-xMxEMnO6The modified lithium nickel manganese oxide material comprises lithium nickel manganese oxide and R which is coated on the outer side of the lithium nickel manganese oxide and has a double perovskite structure1.5M0.5NiMnO6A material.
Example 3
R2-xMxEMnO6The modified lithium nickel manganese oxide material comprises lithium nickel manganese oxide and R which is coated on the outer side of the lithium nickel manganese oxide and has a double perovskite structure1.5M0.5CoMnO6A material.
Wherein R is Nd element, Pm element, Eu element, Gd element, Tb element, Dy element or Yb element; m is Ca element or Ba element.
Example 4
Dy1.5Ca0.5NiMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, adding Dy (NO)3)3·6H2O、Ca(NO3)2·6H2O、Ni(NO3)2·6H2O and Mn (NO)3)2·6H2O is added according to a molar ratio of 1.5: 0.5: 1: 1, adding distilled water to dissolve to obtain a mixed solution;
s2, adding citric acid into the mixed solution, wherein the total substance amount of the metal ions in the mixed solution is a, the substance amount of the citric acid is b, a: b is 1: 2, adding the lithium nickel manganese oxide and stirring uniformly, wherein the lithium nickel manganese oxide and Dy1.5Ca0.5NiMnO6The mass ratio of the materials is 100: 0.5; heating and evaporating to obtain gel; drying the gel, calcining at 850 ℃ in pure oxygen atmosphere to obtain Dy1.5Ca0.5NiMnO6A modified lithium nickel manganese oxide material.
Example 5
Dy2NiMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, adding Dy (NO)3)3·6H2O、Ni(NO3)2·6H2O and Mn (NO)3)2·6H2O is prepared according to the molar ratio of 2: 1: 1, adding distilled water to dissolve to obtain a mixed solution;
s2, adding citric acid into the mixed solution, wherein the total substance amount of the metal ions in the mixed solution is a, the substance amount of the citric acid is b, a: b is 1: 2, adding the lithium nickel manganese oxide and stirring uniformly, wherein the lithium nickel manganese oxide and Dy2NiMnO6The mass ratio of the materials is 100: 1; heating and evaporating to obtain gel; drying the gel, calcining at 850 ℃ in pure oxygen atmosphere to obtain Dy2NiMnO6A modified lithium nickel manganese oxide material.
Example 6
Dy1.5Ca0.5NiMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, adding Dy (NO)3)3·6H2O、Ca(NO3)2·6H2O、Ni(NO3)2·6H2O and Mn (NO)3)2·6H2O is added according to a molar ratio of 1.5: 0.5: 1: 1, adding distilled water to dissolve to obtain a mixed solution;
s2, adding citric acid into the mixed solution, wherein the total substance amount of the metal ions in the mixed solution is a, the substance amount of the citric acid is b, a: b is 1: 3, adding the lithium nickel manganese oxide precursor and uniformly stirring; counting the nickel lithium manganate precursor according to the obtained nickel lithium manganate to obtain the nickel lithium manganate precursor and Dy1.5Ca0.5NiMnO6The mass ratio of the materials is 100: 0.5; heating and evaporating to obtain gel; drying the gel, calcining at 850 ℃ in pure oxygen atmosphere to obtain Dy1.5Ca0.5NiMnO6A modified lithium nickel manganese oxide material.
Example 7
Eu1.5Ba0.5CoMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, adding Eu (NO)3)3·6H2O、Ba(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO)3)2·6H2O is added according to a molar ratio of 1.5: 0.5: 1: 1, adding the mixture into absolute ethyl alcohol to dissolve the mixture to obtain a mixed solution;
s2, adding citric acid into the mixed solution, wherein the total substance amount of the metal ions in the mixed solution is a, the substance amount of the citric acid is b, a: b is 1: 2, adding the lithium nickel manganese oxide, uniformly stirring, and mixing the lithium nickel manganese oxide and Eu1.5Ba0.5CoMnO6The mass ratio of the materials is 100: 0.5; heating and evaporating to obtain gel; drying the gel, calcining at 750 ℃ in pure oxygen atmosphere to obtain Eu1.5Ba0.5CoMnO6A modified lithium nickel manganese oxide material.
Example 8
Eu1.5Ba0.5CoMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, adding Eu (NO)3)3·6H2O、Ba(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO)3)2·6H2O is added according to a molar ratio of 1.5: 0.5: 1: 1, adding the mixture into absolute ethyl alcohol to dissolve the mixture to obtain a mixed solution;
s2, adding citric acid into the mixed solution, wherein the total substance amount of the metal ions in the mixed solution is a, the substance amount of the citric acid is b, a: b is 1: 2, adding the lithium nickel manganese oxide, uniformly stirring, and mixing the lithium nickel manganese oxide and Eu1.5Ba0.5CoMnO6The mass ratio of the materials is 100: 0.5; heating and evaporating to obtain gel; drying the gel, calcining at 1000 ℃ in pure oxygen atmosphere to obtain Eu1.5Ba0.5CoMnO6A modified lithium nickel manganese oxide material.
Example 9
Dy1.5Ca0.5NiMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, adding Dy (NO)3)3·6H2O、Ca(NO3)2·6H2O、Ni(NO3)2·6H2O and Mn (NO)3)2·6H2O is added according to a molar ratio of 1.5: 0.5: 1: 1, adding distilled water to dissolve to obtain a mixed solution;
s2, adding a complexing agent into the mixed solution, wherein the total amount of metal ions in the mixed solution is a, the amount of the complexing agent is b, and a: b is 1: 2, adding the lithium nickel manganese oxide and stirring uniformly, wherein the lithium nickel manganese oxide and Dy1.5Ca0.5NiMnO6The mass ratio of the materials is 100: 0.5; heating and evaporating to obtain gel; drying the gel, heating from room temperature to 750 ℃ in pure oxygen atmosphere, and calcining for 1min to obtain Dy1.5Ca0.5NiMnO6A modified lithium nickel manganese oxide material.
Example 10
Dy2NiMnO6The preparation method of the modified lithium nickel manganese oxide material comprises the following steps:
s1, adding Dy (NO)3)3·6H2O、Ni(NO3)2·6H2O and Mn (NO)3)2·6H2O is prepared according to the molar ratio of 2: 1: 1, adding distilled water to dissolve to obtain a mixed solution;
s2, adding a complexing agent into the mixed solution, wherein the total amount of metal ions in the mixed solution is a, the amount of the complexing agent is b, and a: b is 1: 2.5, adding the lithium nickel manganese oxide, and uniformly stirring to obtain the lithium nickel manganese oxide and Dy2NiMnO6The mass ratio of the materials is 100: 0.8; heating and evaporating to obtain gel; drying the gel, heating from room temperature to 1000 ℃ in pure oxygen atmosphere, and calcining for 120min to obtain Dy2NiMnO6A modified lithium nickel manganese oxide material.
Examples 1 to 10R2-xMxEMnO6The modified lithium nickel manganese oxide material can be used for preparing a lithium ion battery anode material.
Dy obtained in example 1 was used1.5Ca0.5NiMnO6Modified lithium nickel manganese oxide material and lithium nickel manganese oxide are respectively used asFor testing electrical properties of the lithium ion battery positive electrode material, as shown in fig. 1 and 2, fig. 1 shows R obtained in example 1 of the present invention2-xMxEMnO6FIG. 2 is a graph showing the charge-discharge cycle curves of modified lithium nickel manganese oxide material and lithium nickel manganese oxide, wherein R is obtained in example 1 of the present invention2-xMxEMnO6And (3) a discharge curve diagram of the modified lithium nickel manganese oxide material and the lithium nickel manganese oxide under different multiplying powers. As can be seen from FIGS. 1 and 2, R obtained in the present invention2- xMxEMnO6The modified lithium nickel manganese oxide material can prolong the cycle life of the lithium ion battery, and has larger discharge specific capacity under different multiplying powers.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. R2-xMxEMnO6The preparation method of the modified lithium nickel manganese oxide material is characterized by comprising the following steps:
s1, mixing rare earth metal salt, alkaline earth metal salt, iron series metal salt and manganese salt according to the molar ratio of 2-x: x: 1: 1 adding the mixture into a solvent to dissolve the mixture to obtain a mixed solution;
s2, adding a complexing agent into the mixed solution, adding lithium nickel manganese oxide or a lithium nickel manganese oxide precursor, uniformly stirring, and heating and evaporating to obtain gel; drying and calcining the gel to obtain R2-xMxEMnO6Modifying a lithium nickel manganese oxide material;
wherein in S2, the calcination environment is pure oxygen atmosphere or air atmosphere, and the calcination temperature is 750-1000 ℃; in the calcination process of S2, the calcination temperature T and the temperature rise time T have the following relationship: t × lgt + 750; wherein T is the temperature value of calcination, the unit is DEG C, T is the time for heating from room temperature to the calcination temperature T, the unit is min, and T is more than or equal to 1 and less than or equal to 120;
wherein in S2, R which is coated outside the lithium nickel manganese oxide and has a double perovskite structure2-xMxEMnO6The material, wherein x is more than or equal to 0 and less than or equal to 0.5;
wherein in S1 and S2, R is rare earth metal, and R is Nd element, Pm element, Eu element, Gd element, Tb element, Dy element or Yb element; m is alkaline earth metal, and M is Ca element or Ba element; e is iron metal, E is Ni element or Co element;
wherein in S2, lithium nickel manganese oxide or lithium nickel manganese oxide precursor and R2-xMxEMnO6The mass ratio of the materials is 100: 0.5-1, wherein the mass of the lithium nickel manganese oxide precursor is calculated according to the obtained lithium nickel manganese oxide.
2. R according to claim 12-xMxEMnO6The preparation method of the modified lithium nickel manganese oxide material is characterized in that in S1, the rare earth metal salt and the alkaline earth metal salt are at least one of chloride, alkoxide, nitrate, carbonate or acetate; in S1, the solvent is distilled water or ethanol.
3. R according to claim 12-xMxEMnO6The preparation method of the modified lithium nickel manganese oxide material is characterized in that in S2, the total amount of metal ions in the mixed solution is a, the amount of the complexing agent is b, and a: b is 1: 2-3; the complexing agent is citric acid.
4. A compound as claimed in any one of claims 1 to 32-xMxEMnO6The modified lithium nickel manganese oxide material is applied to the anode material of the lithium ion battery.
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