CN105609718B - The rich lithium material Li of Spinel cladding1.87Mn0.94Ni0.19O3, its preparation method and application - Google Patents

The rich lithium material Li of Spinel cladding1.87Mn0.94Ni0.19O3, its preparation method and application Download PDF

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CN105609718B
CN105609718B CN201510975426.3A CN201510975426A CN105609718B CN 105609718 B CN105609718 B CN 105609718B CN 201510975426 A CN201510975426 A CN 201510975426A CN 105609718 B CN105609718 B CN 105609718B
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rich lithium
spinel
lithium material
manganese
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CN105609718A (en
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王云鹤
左斌
雷军
田占军
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Laoling Shengli New Energy Co ltd
Shandong Baoli Biomass Energy Co ltd
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LELING SHENGLI NEW ENERGY Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/366Composites as layered products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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Abstract

The invention discloses a kind of rich lithium material Li1.87Mn0.94Ni0.19O3, its preparation method and its application, belong to electrochemical technology field.The invention discloses a kind of new material as lithium ion cell positive, i.e. the rich lithium material Li of Spinel cladding1.87Mn0.94Ni0.19O3, its preparation method is simple.Lithium coin cells 1C can be lifted during positive electrode of the material as lithium coin cells(250 milliamperes every gram)Cyclical stability under high magnification, while ensure higher specific capacity.Stable circulation performance has been brought up to more than 200 times under 1C multiplying powers at present, while keeps capacity in every gram or so of 180 MAH.

Description

The rich lithium material Li of Spinel cladding1.87Mn0.94Ni0.19O3, its preparation method and Using
Technical field
The present invention relates to electrochemical technology field, more particularly to a kind of rich lithium material of Spinel cladding Li1.87Mn0.94Ni0.19O3, its preparation method and its application.
Background technology
In recent years, with the getting worse of energy environment issues, and the requirement of electronic product lightness, people to lithium from The research of sub- battery deepens continuously.
At present, the positive electrode of lithium-ion-power cell mainly uses LiMn2O4, LiFePO4 or multivariant oxide positive pole Material, but material gram volume is low, cyclical stability is poor under high magnification, storge quality is poor, it is also necessary to continues to improve.
The content of the invention
In order to make up the deficiencies in the prior art, the invention provides a kind of rich lithium material of Spinel cladding Li1.87Mn0.94Ni0.19O3, its preparation method and its application.
The technical scheme is that:
A kind of surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3, including rich lithium material and be coated on The Spinel clad of rich lithium material outer layer;The rich lithium material is made up of Li elements, Mn elements, Ni elements and O elements, institute The mol ratio for stating Li elements, Mn elements, Ni elements and O elements is 1.87:0.94:0.19:3;The Spinel clad is Galaxite.
Preferably, the thickness of the Spinel clad is 2-2.5nm.
The surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3Preparation method, including step:
1)The mol ratio of the mixed solution of preparation manganese nitrate and nickel nitrate, manganese nitrate and nickel nitrate is 4.9-5.1:1, mixing The total concentration of manganese ion and nickel ion is 0.2-0.25mol/L in solution;
2)It is gradually added into sodium carbonate liquor into mixture, the concentration of sodium carbonate liquor is 0.2-0.25mol/L, added carbon The molal quantity of carbonate is equal with manganese ion and nickel ion molal quantity summation in acid solution;
3)15-25 hours are stirred, obtain the mixed carbonate sediment of nickel and manganese;
4)Mixed carbonate sediment is isolated, 20-28 hours are dried at 105-120 DEG C, then in air atmosphere, 4-6 hours are sintered at 470-530 DEG C, obtain the mixed oxide of nickel and manganese;
5)By the mixed oxide of nickel and manganese and lithium hydroxide according to mass ratio 1:1.078-1.122 is uniformly mixed, then At 850-950 DEG C, 11-13 hours are sintered in air atmosphere, obtain rich lithium material Li1.87Mn0.94Ni0.19O3
6)Manganese acetate and rich lithium material Li1.87Mn0.94Ni0.19O3Mix in ethanol, ultrasonic 20-40 minutes;Wherein acetic acid Manganese and rich lithium material Li1.87Mn0.94Ni0.19O3Mol ratio be 1:14-16;
7)Mill-drying, then proceed to add ethanol, then mill-drying, circulate 8-12 times according to this;
8)In air atmosphere, 4-6 hours are sintered at 700-800 DEG C, obtain the surface coated rich lithium material of Spinel Li1.87Mn0.94Ni0.19O3
Preferably, step 1)In, the mol ratio of manganese nitrate and nickel nitrate is 5:1.
Preferably, step 2)In, the concentration of sodium carbonate liquor is equal with the total concentration of manganese ion and nickel ion.
Preferably, step 4)In, in air atmosphere, sintered 5 hours at 500 DEG C.
Preferably, step 5)In, in air atmosphere, sintered 12 hours at 900 DEG C.
Preferably, step 6)In, manganese acetate and rich lithium material Li1.87Mn0.94Ni0.19O3Mol ratio be 1:15.
Preferably, step 8)In, in air atmosphere, sintered 5 hours at 750 DEG C.
The surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3As anode material for lithium-ion batteries Application.
Beneficial effects of the present invention are:
The invention provides a kind of new material as lithium battery anode, i.e. the surface coated rich lithium material of Spinel Li1.87Mn0.94Ni0.19O3.The preparation method of the material is simple, and mild condition is controllable, is evenly coated, and cladding thickness is received for 2-2.5 Rice.
The Spinel superficial layer that the present invention obtains can effectively slow down electrolyte and the direct of lithium-rich anode material connects Touch, destruction of the electrolyte to rich lithium material surface is reduced, so as to improve cyclical stability of the material under 1C high magnifications.
The surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3During as positive electrode, can further it carry Rise lithium coin cells 1C(250 milliamperes every gram)Stability under high magnification, while ensure higher specific capacity.1C multiplying powers at present Lower stable circulation performance has been brought up to more than 200 times, while keeps capacity in every gram or so of 180 MAH.
In addition, the surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3During as positive electrode, button lithium Under battery 0.1C multiplying powers, first circulation specific discharge capacity is 105 every gram of MAHs;And uncoated rich lithium material Li1.87Mn0.94Ni0.19O3During as positive electrode, under 0.1C multiplying powers, first circulation specific discharge capacity is lithium coin cells 76 every gram of MAHs;The former first discharge specific capacity is high.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also To obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is the surface coated rich lithium material Li of Spinel of the present invention1.87Mn0.94Ni0.19O3Transmission electron microscope(TEM) Figure;
Fig. 2 is the surface coated rich lithium material Li of Spinel of the present invention1.87Mn0.94Ni0.19O3Another transmission electron microscope (TEM)Figure;
Fig. 3 is the surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3During as positive electrode, button lithium Battery is in 0.1C and 1C, the graph of a relation of cycle-index and specific discharge capacity.
Embodiment
Embodiment 1
A kind of surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3, including rich lithium material and be coated on The Spinel clad of rich lithium material outer layer;The rich lithium material is made up of Li elements, Mn elements, Ni elements and O elements, institute The mol ratio for stating Li elements, Mn elements, Ni elements and O elements is 1.87:0.94:0.19:3;The Spinel clad is Galaxite.
The surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3Preparation method, including step:
1)The mol ratio of the mixed solution 100ml of preparation manganese nitrate and nickel nitrate, manganese nitrate and nickel nitrate is 5:1, mixing The total concentration of manganese ion and nickel ion is 0.2mol/L in solution;
2)100ml sodium carbonate liquors are gradually added into mixture, the concentration of sodium carbonate liquor is 0.2mol/L;
3)Stirring 20 hours, obtains the mixed carbonate sediment of nickel and manganese;
4)Mixed carbonate sediment is isolated, is dried 24 hours at 110 DEG C, then in air atmosphere, at 500 DEG C Sintering 5 hours, obtains the mixed oxide of nickel and manganese;
5)By the mixed oxide of nickel and manganese and lithium hydroxide according to mass ratio 1:1.1 uniformly mixing, then in 900 DEG C Under, sintered 12 hours in air atmosphere, obtain rich lithium material Li1.87Mn0.94Ni0.19O3
6)Manganese acetate and rich lithium material Li1.87Mn0.94Ni0.19O3Mix in ethanol, ultrasound 30 minutes;Wherein manganese acetate With rich lithium material Li1.87Mn0.94Ni0.19O3Mol ratio be 1:15;
7)Mill-drying, then proceed to add ethanol, then mill-drying, circulate 10 times according to this;
8)In air atmosphere, sintered 5 hours at 750 DEG C, obtain the surface coated rich lithium material of Spinel Li1.87Mn0.94Ni0.19O3
Wherein, step 5)In, lithium is excessive, to supplement the volatilization under its high temperature.
As shown in Figure 1 and Figure 2, a layer crystal of material surface about 2-2.5 nanometer thickness is can see along different crystal faces Body, the lattice arrangement and interplanar distance of its lattice and body phase have significant difference, that is to say, that surface Spinel clad Thickness is about 2-2.5 nanometers.
With the surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3As positive electrode, lithium ion knob is made Battery is detained, and carries out performance test.
As shown in figure 3, the surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3, can during as positive electrode Further to lift lithium coin cells 1C(250 milliamperes every gram)Stability under high magnification, while keep higher electric discharge to hold Amount.Stable circulation performance has been brought up to more than 200 times under 1C multiplying powers at present, while keeps capacity on every gram of left side of 180 MAH It is right;Under 0.1C multiplying powers, first circulation specific discharge capacity is 105 every gram of MAHs.
With uncoated rich lithium material Li1.87Mn0.94Ni0.19O3As positive electrode, lithium ion button shape cell is made, and Carry out performance test.
Embodiment 2
A kind of surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3, including rich lithium material and be coated on The Spinel clad of rich lithium material outer layer;The rich lithium material is made up of Li elements, Mn elements, Ni elements and O elements, institute The mol ratio for stating Li elements, Mn elements, Ni elements and O elements is 1.87:0.94:0.19:3;The Spinel clad is Galaxite.
The surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3Preparation method, including step:
1)The mol ratio of the mixed solution 100ml of preparation manganese nitrate and nickel nitrate, manganese nitrate and nickel nitrate is 4.9:1, mix It is 0.25mol/L to close the total concentration of manganese ion and nickel ion in solution;
2)100ml sodium carbonate liquors are gradually added into mixture, the concentration of sodium carbonate liquor is 0.25mol/L;
3)Stirring 20 hours, obtains the mixed carbonate sediment of nickel and manganese;
4)Mixed carbonate sediment is isolated, is dried 24 hours at 110 DEG C, then in air atmosphere, at 500 DEG C Sintering 5 hours, obtains the mixed oxide of nickel and manganese;
5)By the mixed oxide of nickel and manganese and lithium hydroxide according to mass ratio 1:1.078 uniformly mixing, then in 900 DEG C Under, sintered 12 hours in air atmosphere, obtain rich lithium material Li1.87Mn0.94Ni0.19O3
6)Manganese acetate and rich lithium material Li1.87Mn0.94Ni0.19O3Mix in ethanol, ultrasound 40 minutes;Wherein manganese acetate With rich lithium material Li1.87Mn0.94Ni0.19O3Mol ratio be 1:16;
7)Mill-drying, then proceed to add ethanol, then mill-drying, circulate 12 times according to this;
8)In air atmosphere, sintered 6 hours at 700 DEG C, obtain the surface coated rich lithium material of Spinel Li1.87Mn0.94Ni0.19O3
Wherein, step 5)In, lithium is excessive, to supplement the volatilization under its high temperature.
Embodiment 3
A kind of surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3, including rich lithium material and be coated on The Spinel clad of rich lithium material outer layer;The rich lithium material is made up of Li elements, Mn elements, Ni elements and O elements, institute The mol ratio for stating Li elements, Mn elements, Ni elements and O elements is 1.87:0.94:0.19:3;The Spinel clad is Galaxite.
The surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3Preparation method, including step:
1)The mol ratio of the mixed solution 100ml of preparation manganese nitrate and nickel nitrate, manganese nitrate and nickel nitrate is 5.1:1, mix It is 0.2mol/L to close the total concentration of manganese ion and nickel ion in solution;
2)100ml sodium carbonate liquors are gradually added into mixture, the concentration of sodium carbonate liquor is 0.2mol/L;
3)Stirring 20 hours, obtains the mixed carbonate sediment of nickel and manganese;
4)Mixed carbonate sediment is isolated, is dried 24 hours at 110 DEG C, then in air atmosphere, at 500 DEG C Sintering 5 hours, obtains the mixed oxide of nickel and manganese;
5)By the mixed oxide of nickel and manganese and lithium hydroxide according to mass ratio 1:1.122 uniformly mixing, then in 900 DEG C Under, sintered 12 hours in air atmosphere, obtain rich lithium material Li1.87Mn0.94Ni0.19O3
6)Manganese acetate and rich lithium material Li1.87Mn0.94Ni0.19O3Mix in ethanol, ultrasonic 20-40 minutes;Wherein acetic acid Manganese and rich lithium material Li1.87Mn0.94Ni0.19O3Mol ratio be 1:14;
7)Mill-drying, then proceed to add ethanol, then mill-drying, circulate 8 times according to this;
8)In air atmosphere, sintered 4 hours at 800 DEG C, obtain the surface coated rich lithium material of Spinel Li1.87Mn0.94Ni0.19O3
Wherein, step 5)In, lithium is excessive, to supplement the volatilization under its high temperature.

Claims (8)

  1. A kind of 1. surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3, it is characterised in that:Including rich lithium material with And it is coated on the Spinel clad of rich lithium material outer layer;The rich lithium material is by Li elements, Mn elements, Ni elements and O members Element composition, the Li elements, Mn elements, the mol ratio of Ni elements and O elements are 1.87:0.94:0.19:3;The Spinel Clad is galaxite;
    The surface coated rich lithium material Li of Spinel1.87Mn0.94Ni0.19O3Preparation method, including step:
    1)The mol ratio of the mixed solution of preparation manganese nitrate and nickel nitrate, manganese nitrate and nickel nitrate is 4.9-5.1:1, mixed solution The total concentration of middle manganese ion and nickel ion is 0.2-0.25mol/L;
    2)Sodium carbonate liquor is gradually added into mixture, the concentration of sodium carbonate liquor is 0.2-0.25mol/L, and added carbonic acid is molten The molal quantity of carbonate is equal with manganese ion and nickel ion molal quantity summation in liquid;
    3)15-25 hours are stirred, obtain the mixed carbonate sediment of nickel and manganese;
    4)Mixed carbonate sediment is isolated, 20-28 hours, then in air atmosphere, 470- are dried at 105-120 DEG C 4-6 hours are sintered at 530 DEG C, obtain the mixed oxide of nickel and manganese;
    5)By the mixed oxide of nickel and manganese and lithium hydroxide according to mass ratio 1:1.078-1.122 is uniformly mixed, Ran Houyu At 850-950 DEG C, 11-13 hours are sintered in air atmosphere, obtain rich lithium material Li1.87Mn0.94Ni0.19O3
    6)Manganese acetate and rich lithium material Li1.87Mn0.94Ni0.19O3Mix in ethanol, ultrasonic 20-40 minutes;Wherein manganese acetate with Rich lithium material Li1.87Mn0.94Ni0.19O3Mol ratio be 1:14-16;
    7)Mill-drying, then proceed to add ethanol, then mill-drying, circulate 8-12 times according to this;
    8)In air atmosphere, 4-6 hours are sintered at 700-800 DEG C, obtain the surface coated rich lithium material of Spinel Li1.87Mn0.94Ni0.19O3
  2. 2. the surface coated rich lithium material Li of Spinel as claimed in claim 11.87Mn0.94Ni0.19O3, it is characterised in that:Institute The thickness for stating Spinel clad is 2-2.5nm.
  3. 3. the surface coated rich lithium material Li of Spinel as claimed in claim 11.87Mn0.94Ni0.19O3, it is characterised in that:Step Rapid 1)In, the mol ratio of manganese nitrate and nickel nitrate is 5:1.
  4. 4. the surface coated rich lithium material Li of Spinel as claimed in claim 11.87Mn0.94Ni0.19O3, it is characterised in that:Step Rapid 2)In, the concentration of sodium carbonate liquor is equal with the total concentration of manganese ion and nickel ion.
  5. 5. the surface coated rich lithium material Li of Spinel as claimed in claim 11.87Mn0.94Ni0.19O3, it is characterised in that:Step Rapid 4)In, in air atmosphere, sintered 5 hours at 500 DEG C.
  6. 6. the surface coated rich lithium material Li of Spinel as claimed in claim 11.87Mn0.94Ni0.19O3, it is characterised in that:Step Rapid 5)In, in air atmosphere, sintered 12 hours at 900 DEG C.
  7. 7. the surface coated rich lithium material Li of Spinel as claimed in claim 11.87Mn0.94Ni0.19O3, it is characterised in that:Step Rapid 6)In, manganese acetate and rich lithium material Li1.87Mn0.94Ni0.19O3Mol ratio be 1:15.
  8. 8. the surface coated rich lithium material Li of Spinel as claimed in claim 11.87Mn0.94Ni0.19O3, it is characterised in that:Step Rapid 8)In, in air atmosphere, sintered 5 hours at 750 DEG C.
CN201510975426.3A 2015-12-23 2015-12-23 The rich lithium material Li of Spinel cladding1.87Mn0.94Ni0.19O3, its preparation method and application Expired - Fee Related CN105609718B (en)

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US20180114982A1 (en) * 2016-10-24 2018-04-26 Nano And Advanced Materials Institute Limited Lithium manganese oxide spinel and manufacturing method therefor
CN107394156A (en) * 2017-07-19 2017-11-24 长沙矿冶研究院有限责任公司 A kind of method of modifying and its modified anode material of the lithium-rich manganese-based anode material for lithium-ion batteries based on organic matter ammoniacal liquor
US11495796B2 (en) 2018-11-14 2022-11-08 Samsung Sdi Co., Ltd. Positive active material for rechargeable lithium battery, method of preparing the same and rechargeable lithium battery including the same
CN111193025B (en) * 2018-11-15 2023-10-20 三星Sdi株式会社 Positive active material for rechargeable lithium battery, method of preparing the same, and rechargeable lithium battery including the same
KR102363371B1 (en) 2019-02-01 2022-02-14 삼성에스디아이 주식회사 Positive active material for rechargeable lithium battery, method of preparing the same and rechargeable lithium battery incluidng the same
CN112803022B (en) * 2020-12-31 2022-05-06 国联汽车动力电池研究院有限责任公司 Surface structure spinel-rock salt phase integrated lithium-rich material and preparation method thereof

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