CN103915617A - Lithium-rich positive material and preparation method thereof - Google Patents
Lithium-rich positive material and preparation method thereof Download PDFInfo
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- CN103915617A CN103915617A CN201410158910.2A CN201410158910A CN103915617A CN 103915617 A CN103915617 A CN 103915617A CN 201410158910 A CN201410158910 A CN 201410158910A CN 103915617 A CN103915617 A CN 103915617A
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- lithium
- sodium
- anode material
- rich anode
- manganese
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to the technical field of a lithium ion battery, in particular to a lithium-rich positive material and a preparation method thereof. The chemical general formula of the lithium-rich positive material is mLi(2-x)NaxMnO3.nLi(1-y)NayMO2, wherein the sum of x and y is more than 0 and less than 1, the sum of m and n is equal to 1, and M is at least on of Mn, Ni and Co. Compared with an existing lithium-rich positive material, the lithium-rich positive material is not only good in cycling stability, but also excellent in rate performance and stable in voltage in a cycling process.
Description
Technical field
The present invention relates to technical field of lithium ion, particularly relate to a kind of lithium-rich anode material and preparation method thereof.
Background technology
The progress in modern epoch, the continuous miniaturization of consuming device, multifunction, also improving constantly for the requirement of battery accordingly.Lithium ion battery has many advantages: voltage platform is high, specific capacity is high, have extended cycle life, self discharge is low, memory-less effect etc., has huge application prospect on electric automobile and energy storage device.
At present, high-energy-density, durable, high magnification (fast charging and discharging ability), cheapness, safety have become the target that lithium ion battery development is pursued.LiCoO owing to having specific capacity
2the specific capacity of material twice, lithium-rich anode material is considered to the ideal material of high-energy electrokinetic cell of future generation.But its cyclical stability is poor, and in cyclic process, there is the problems such as voltage attenuation, be difficult to meet practical application.
Summary of the invention
In order to address the above problem, the object of the invention is to, a kind of good cycling stability is provided, high rate performance is good, voltage lithium-rich anode material stably in cyclic process.
Two of object of the present invention is to provide a kind of simple, the preparation method of described lithium-rich anode material.The present invention is achieved through the following technical solutions:
A kind of lithium-rich anode material, the chemical general formula of described lithium-rich anode material is mLi
2-xna
xmnO
3nLi
1-yna
ymO
2; Wherein 0<x+y<1, m+n=1; M is at least one in Mn, Ni, Co.
Prepare the method for described sodium doping lithium-rich anode material, elder generation obtains mixture I after weighing respectively lithium salts, sodium salt, nickel salt, cobalt salt, the mixing of manganese salt with mol ratio Li:Na:Ni:Co:Mn=2m+n-2x-2y:mx+ny:na:nb:n (1-a-b);
In said mixture I, add solvent adjustment to rheology phase (use Rheological Phase Method to prepare material, with respect to ball milling energy savings, reduce operation, heighten efficiency) again, obtain mixture II;
After then said mixture II being dried, putting into temperature and be the Muffle furnace of 700～1000 DEG C calcines after 8～48 hours and obtains described lithium-rich anode material; Mainly utilize airborne oxygen to originate as reactant, reactant need at high temperature with the abundant haptoreaction of oxygen.
Wherein: 0<x+y<1, m+n=1,0≤a≤1,0≤b≤1.
Wherein, rheology is a kind of process of preparing noval chemical compound by rheology hybrid system mutually.By suitably mixing, add suitable quantity of water or other solvent to be modulated into solids and evenly not stratified thick solid-liquid hybrid system-rheology phase system of liquid distribution reactant, then reaction obtains required product under proper condition.Material in rheology state generally chemically has complicated composition or structure; The character that demonstrates solid on mechanics demonstrates again the character of liquid, in other words conj.or perhaps like solid non-solid, like the non-liquid of liquid; On physical composition, be both to have comprised solid particle also to comprise liquid substance, can flow or the slow mobile uniform a kind of complication system of macroscopic view.
The homogeneous of solid particle and liquid substance is mixed to the advantage as rheological body: the surface area of solid particle can be effectively utilized, with fluid contact closely, evenly, heat exchange is good, there will not be local overheating phenomenon, temperature is easy to regulate.Many materials can show excess of export concentration phenomenon and new response characteristic in this state.Rheological phase reaction be a kind of energy-conservation, efficient, subtract dirty green chemical synthetic route.Specific practice of the present invention is: add appropriate solvent, control material viscosity at certain limit 3000～20000cp.
Preferably, nickel salt is the one in nickel acetate, nickel oxalate, nickelous sulfate, nickel nitrate, nickel chloride.
Preferably, cobalt salt is the one in cobalt acetate, cobalt oxalate, cobaltous sulfate, cobalt nitrate, cobalt chloride.
Preferably, manganese salt is the one in manganese acetate, manganese oxalate, manganese sulfate, manganese nitrate, manganese chloride.
Preferably, lithium salts is the one in lithium nitrate, lithium carbonate, lithium oxalate, lithium acetate, lithium chloride.
The present invention tends to use lithium nitrate, because lithium nitrate, about the 200 DEG C first meltings of meeting, makes fully contact between raw material, reduces the reaction time, reduces reaction temperature, energy savings.
Preferably, sodium salt is the one in sodium nitrate, sodium carbonate, sodium acid carbonate, sodium acetate, sodium oxalate, sodium chloride.
Preferably, solvent is at least one in ethanol, deionized water, 1-METHYLPYRROLIDONE (NMP), acetone.
The present invention is mainly lithium position sodium-doped, uses part sodium to replace the elemental lithium in rich lithium.Its reason is: a. lithium and sodium belong to the first major element (the first major element sequence Li Na K ...), only have sodium ion radius to approach lithium ion radius most, if replace the elemental lithium in rich lithium material, sodium is first-selected.B. in rich lithium material, can there is nickel lithium mixing phenomenon, thereby make rich lithium material performance degradation; Existing bibliographical information uses sodium element doping can reduce nickel lithium mixing phenomenon, thereby improves material property.C. sodium metal, than lithium metal low price, is conducive to material cost and reduces.
The invention has the beneficial effects as follows:
(1), by the lithium position doping of sodium, can effectively reduce or eliminate voltage attenuation phenomenon in lithium-rich anode material cyclic process, improve the cycle performance (sodium ion radius is greater than lithium ion, can increase material layer spacing, is more conducive to comparatively speaking take off/embedding of lithium ion) of lithium-rich anode material.
(2), because sodium ion radius is greater than lithium ion radius, therefore, de-/embedding that lithium-rich anode material after sodium doping is more conducive to lithium ion, the adulterate high rate performance of rich lithium material of corresponding sodium also can get a promotion (because lithium ion battery is concentration cell, in charge and discharge process, can there is concentration polarization, and cause concentration difference plan reason to be take off/embedding speed of lithium ion.The present invention is adulterated and has been improved take off/embedding speed of lithium ion by sodium, thereby has reduced concentration polarization, has improved ion-conductance chemistry (multiplying power) performance).
(3), the present invention uses Rheological Phase Method to prepare sodium doping lithium-rich anode material.Rheological Phase Method is to use solvent by a kind of raw material furnishing state between liquid phase and solid phase, the method has the following advantages: with respect to liquid phase method, reduce solvent load, shorten time, the energy except desolventizing, thereby economize on resources the energy, improve material preparation efficiency; With respect to solid phase method, batch mixing is more even, and does not need the techniques such as ball milling, reduces energy consumption.
(4), because the present invention introduces low-cost sodium salt, reduced expensive lithium salts consumption, thereby reduced the cost of rich lithium material.
Brief description of the drawings
Fig. 1 is the specific capacity contrast of rich lithium material in the present invention and prior art.
concrete execution mode
Below in conjunction with embodiment, the present invention is described in further detail, understands the present invention to help those skilled in the art.
Embodiment 1:
Weigh respectively the nitrate of lithium, sodium, nickel, cobalt, manganese with mol ratio Li:Na:Ni:Co:Mn=1:0.2:0.13:0.13:0.54, add appropriate ethanol to regulate raw material to rheology phase, stirring at room temperature is calcined and within 16 hours, is obtained sodium doping lithium-rich anode material LiNa to putting into after dry at 800 DEG C of Muffle furnaces
0.2ni
0.13co
0.13mn
0.54o
2.
Embodiment 2:
Weigh respectively the acetate of lithium, sodium, nickel, manganese with mol ratio Li:Na:Ni:Mn=1.1:0.1:0.13:0.67, add appropriate ethanol to regulate raw material to rheology phase, stirring at room temperature is calcined and within 16 hours, is obtained sodium doping lithium-rich anode material 0.5Li to putting into after dry at 800 DEG C of Muffle furnaces
1.85na
0.15mnO
30.5Li
0.9na
0.1(Ni
1/3mn
1/3) O
2.
Embodiment 3:
Weigh respectively the nitrate of lithium, sodium, nickel, manganese with mol ratio Li:Na:Ni:Mn=1.1:0.1:0.13:0.67, add appropriate amount of deionized water to regulate raw material to rheology phase, stirring at room temperature is calcined and within 24 hours, is obtained sodium doping lithium-rich anode material 0.5Li to putting into after dry at 900 DEG C of Muffle furnaces
1.85na
0.15mnO
30.5Li
0.9na
0.1(Ni
1/3mn
1/3) O
2.
Embodiment 4:
Weigh respectively the carbonate of lithium, sodium with mol ratio Li:Na:Ni:Co:Mn=1.3:0.2:0.35:0.14:0.51, the nitrate of nickel, cobalt, manganese, add proper amount of acetone to regulate raw material to rheology phase, stirring at room temperature is calcined and within 8 hours, is obtained sodium doping lithium-rich anode material 0.3Li to putting into after dry at 850 DEG C of Muffle furnaces
1.8na
0.2mnO
30.7Li (Ni
0.5co
0.2mn
0.3) O
2.
Above-described embodiment, is preferred embodiment of the present invention, is not used for limiting the scope of the present invention, and the equivalence of being done with the feature described in the claims in the present invention and principle therefore all changes or modifies, within all should being included in the claims in the present invention scope.
By finding out in Fig. 1, after rich lithium manganese material sodium contaminated, material polarization obviously reduces, and specific capacity is by the 222mAh g of doped samples not
-1increase to the 252mAh g after doping
-1.Illustrate that sodium is doped with helping promote rich lithium manganese material chemical property.
Claims (8)
1. a lithium-rich anode material, is characterized in that, the chemical general formula of described lithium-rich anode material is mLi
2-xna
xmnO
3nLi
1-yna
ymO
2; Wherein 0<x+y<1, m+n=1; M is at least one in Mn, Ni, Co.
2. the method for preparing lithium-rich anode material described in claim 1, is characterized in that,
After first weighing respectively lithium salts, sodium salt, nickel salt, cobalt salt, the mixing of manganese salt with mol ratio Li:Na:Ni:Co:Mn=2m+n-2x-2y:mx+ny:na:nb:n (1-a-b), obtain mixture I;
In said mixture I, add solvent adjustment to rheology phase again, obtain mixture II;
After then said mixture II being dried, putting into temperature and be the Muffle furnace of 700～1000 DEG C calcines after 8～48 hours and obtains described lithium-rich anode material;
Wherein: 0<x+y<1, m+n=1,0≤a≤1,0≤b≤1.
3. the preparation method of lithium-rich anode material described in claim 2, is characterized in that, nickel salt is the one in nickel acetate, nickel oxalate, nickelous sulfate, nickel nitrate, nickel chloride.
4. the preparation method of lithium-rich anode material described in claim 2, is characterized in that, cobalt salt is the one in cobalt acetate, cobalt oxalate, cobaltous sulfate, cobalt nitrate, cobalt chloride.
5. the preparation method of lithium-rich anode material described in claim 2, is characterized in that, manganese salt is the one in manganese acetate, manganese oxalate, manganese sulfate, manganese nitrate, manganese chloride.
6. the preparation method of lithium-rich anode material described in claim 2, is characterized in that, lithium salts is the one in lithium nitrate, lithium carbonate, lithium oxalate, lithium acetate, lithium chloride.
7. the preparation method of lithium-rich anode material described in claim 2, is characterized in that, sodium salt is the one in sodium nitrate, sodium carbonate, sodium acid carbonate, sodium acetate, sodium oxalate, sodium chloride.
8. the preparation method of lithium-rich anode material described in claim 2, is characterized in that, solvent is at least one in ethanol, deionized water, 1-METHYLPYRROLIDONE, acetone.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104733713A (en) * | 2015-03-25 | 2015-06-24 | 奇瑞汽车股份有限公司 | Lithium-rich manganese material, application thereof and preparation method |
| CN107591531A (en) * | 2017-09-25 | 2018-01-16 | 华南师范大学 | A kind of lithium/sodium double ion manganese-base oxide positive electrode and preparation method and application |
| DE102016214590A1 (en) | 2016-08-05 | 2018-02-08 | Evonik Degussa Gmbh | A method of making a cathode material having a low BET surface area and high tapped density and a special cathode material |
| CN107710461A (en) * | 2015-06-15 | 2018-02-16 | 罗伯特·博世有限公司 | Mix Na and mix Mb, W and/or Mo HE NCM |
| CN108023089A (en) * | 2017-12-13 | 2018-05-11 | 江南大学 | Anion F doping vario-property lithium-rich positive electrodes and preparation method |
| CN108023082A (en) * | 2017-12-04 | 2018-05-11 | 中南大学 | A kind of preparation method of the sodium-ion battery positive material with poly-phase composite layer shape structure |
| CN109244444A (en) * | 2018-08-29 | 2019-01-18 | 湘潭大学 | A kind of lithium-rich manganese-based layered oxide positive electrode and preparation method thereof of niobium doping |
| CN109860587A (en) * | 2019-02-28 | 2019-06-07 | 蜂巢能源科技有限公司 | Positive electrode of lithium ion battery and preparation method thereof, lithium ion battery |
| CN110112410A (en) * | 2019-05-29 | 2019-08-09 | 新乡学院 | A kind of modification lithium-ion battery anode material and preparation method thereof |
| CN115064674A (en) * | 2022-06-28 | 2022-09-16 | 天津巴莫科技有限责任公司 | High-rate long-cycle ternary cathode material, and preparation method and application thereof |
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| WEI HE,ET AL.: ""Enhanced high-rate capability and cycling stability of Na-stabilized layered Li1.2[Co0.13Ni0.13Mn0.54]O2 cathode material"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104733713A (en) * | 2015-03-25 | 2015-06-24 | 奇瑞汽车股份有限公司 | Lithium-rich manganese material, application thereof and preparation method |
| CN107710461A (en) * | 2015-06-15 | 2018-02-16 | 罗伯特·博世有限公司 | Mix Na and mix Mb, W and/or Mo HE NCM |
| DE102016214590A1 (en) | 2016-08-05 | 2018-02-08 | Evonik Degussa Gmbh | A method of making a cathode material having a low BET surface area and high tapped density and a special cathode material |
| WO2018024661A1 (en) | 2016-08-05 | 2018-02-08 | Evonik Degussa Gmbh | Method for producing a cathode material having a low bet surface area and a high tapped density, and a special cathode material |
| CN107591531A (en) * | 2017-09-25 | 2018-01-16 | 华南师范大学 | A kind of lithium/sodium double ion manganese-base oxide positive electrode and preparation method and application |
| CN108023082A (en) * | 2017-12-04 | 2018-05-11 | 中南大学 | A kind of preparation method of the sodium-ion battery positive material with poly-phase composite layer shape structure |
| CN108023082B (en) * | 2017-12-04 | 2021-04-16 | 中南大学 | Preparation method of sodium-ion battery positive electrode material with multiphase composite layered structure |
| CN108023089A (en) * | 2017-12-13 | 2018-05-11 | 江南大学 | Anion F doping vario-property lithium-rich positive electrodes and preparation method |
| CN109244444A (en) * | 2018-08-29 | 2019-01-18 | 湘潭大学 | A kind of lithium-rich manganese-based layered oxide positive electrode and preparation method thereof of niobium doping |
| CN109244444B (en) * | 2018-08-29 | 2021-06-18 | 湘潭大学 | Niobium-doped lithium-rich manganese-based layered oxide positive electrode material and preparation method thereof |
| CN109860587A (en) * | 2019-02-28 | 2019-06-07 | 蜂巢能源科技有限公司 | Positive electrode of lithium ion battery and preparation method thereof, lithium ion battery |
| CN110112410A (en) * | 2019-05-29 | 2019-08-09 | 新乡学院 | A kind of modification lithium-ion battery anode material and preparation method thereof |
| CN115064674A (en) * | 2022-06-28 | 2022-09-16 | 天津巴莫科技有限责任公司 | High-rate long-cycle ternary cathode material, and preparation method and application thereof |
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Application publication date: 20140709 |