CN108203118A - A kind of novel LiMn2O4Electrode material and its preparation process - Google Patents
A kind of novel LiMn2O4Electrode material and its preparation process Download PDFInfo
- Publication number
- CN108203118A CN108203118A CN201611172384.0A CN201611172384A CN108203118A CN 108203118 A CN108203118 A CN 108203118A CN 201611172384 A CN201611172384 A CN 201611172384A CN 108203118 A CN108203118 A CN 108203118A
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- China
- Prior art keywords
- limn
- novel
- electrode material
- ball
- lidy
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1242—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]-, e.g. LiMn2O4, Li[MxMn2-x]O4
-
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of novel LiMn2O4Electrode material and its preparation process.The material is in LiMn with rare earth dysprosium doped2O4In, preparation process is to take acetic acid dysprosium, lithium carbonate, manganese dioxide feedstock, according to LiDyxMn2‑xO4Atomic ratio dispensing, then raw material is subjected to ball-milling treatment, ball milling micro mist is dried, then completely cuts off air calcination, LiDy is prepared by sinteringxMn2‑xO4Electrode material.
Description
Technical field
The present invention relates to a kind of li-ion electrode materials and its preparation process, more particularly to a kind of LiMn for adding rare earth2O4
Li-ion electrode materials and its preparation process belong to battery electrode material field.
Background technology
With being widely used for portable digital product, the use of special mobile phone, laptop, portable, capacitance
The lithium ion battery of high, recyclable charging is just used widely with excellent performance in this kind of product.Initial lithium electricity
Pond be it is a kind of by lithium metal or lithium alloy be negative material, the battery using non-aqueous electrolytic solution.Due to the chemistry of lithium metal
Characteristic is very active so that processing, preservation, the use of lithium metal, it is very high to environmental requirement, and so lithium battery production will be in spy
It is carried out under different environmental condition, use condition is very harsh.Later, Sony Corporation of Japan had been invented using Carbon Materials as cathode, with
Compound containing lithium makees the lithium battery of anode, in charge and discharge process, exists without lithium metal, only lithium ion, here it is lithiums
Ion battery.
Anode material for lithium-ion batteries common at present mainly has the phosphoric acid of the cobalt acid lithium and olivine structural of layer structure
Iron lithium etc..Wherein LiCoO2The overcharge resistant ability of material is poor, declines rapidly in higher charging voltage specific capacity；LiFePO4
There are discharge voltage is low, tap density is low etc., shortcomings all constrain the further application of itself, LiMn2O4Material is as a new generation
Li-ion electrode materials be just widely studied, there is document to point out, to LiMn2O4The rare earth doped element of ingredient, can effectively improve and follow
Ring performance slows down the increase of electrode impedance.The present invention is raw material through ball milling work using lithium carbonate, electrolytic manganese dioxide, acetic acid dysprosium
Skill is worn into alloy powder, then passes through calcine technology Solid phase synthesis LiDyxMn2-xO4 Material, the LiDy after dopingxMn2- xO4 The comprehensive performance of electrode material will further improve.
Invention content
The object of the present invention is to provide a kind of novel LiMn for adulterating Dy2O4Electrode material and its preparation process, the preparation work
Skill includes the following steps：
(1) appropriate chemical pure acetic acid dysprosium, lithium carbonate, electrolytic manganese dioxide are taken as raw material, according to LiDyxMn2-xO4（0.01≤
X≤0.1）Atomic ratio dispensing；
(2) a ball grinder is taken, the raw mixture prepared is poured into wherein together, and adds suitable steel ball, is carried out with ball mill
Ball milling；
(3) the alloy powder of ball milling is dried；
(4) the high-temperature calcination under the conditions of starvation by the alloy powder after drying；
(5) after calcining, powder is collected up to product.
Preferentially, step (1) in, according to LiDyxMn2-xO4（0.03≤X≤0.05）Atomic ratio dispensing.
Preferentially, step (2) in, ratio of grinding media to material 15-20.
Preferentially, step (2) in, ball mill carry out ball milling time be 30-40h.
Step (2) in, acetone can also be changed into gasoline or alcohol.
Preferentially, step (4) in, high-temperature calcination temperature be 700-900 DEG C, time control is in 10-20h.
The present invention has following advantages and characteristic：
(1) the electrode material conductivity prepared is high；
(2) preparation process is simple, and flow is short.
Embodiment one：
Appropriate chemical pure acetic acid dysprosium, lithium carbonate, electrolytic manganese dioxide are taken as raw material, according to LiDy0.01Mn1.99O4Atom
Ratio dispensing 5g, the mixture material prepared is poured into ball grinder together, and puts into the steel ball of 100g, then to pour into acetone molten
After submerging ball grinder, cover is covered tightly for liquid, is put into planetary ball mill and is carried out ball milling, after ball milling 40h, alloy powder is taken out,
It is put into a smooth container and dries, then the powder dried is fitted into quartz glass tube, in the case of continuous pumping, carry out
Vacuum sealing will verify air-tightness in the quartz glass tube input water of sealing, if bubble-free, can assert that its leakproofness is good,
Quartz glass tube is taken out again, dries to be put into 700 DEG C of high temperature furnace after moisture and be calcined, after calcining 20h, processing will be passed through
Quartz glass tube take out, smash quartz glass tube after cooling, collect powder up to product.
Embodiment two：
Appropriate chemical pure acetic acid dysprosium, lithium carbonate, electrolytic manganese dioxide are taken as raw material, according to LiDy0.1Mn1.9O4Atomic ratio
Example dispensing 10g, the mixture material prepared is poured into ball grinder together, and put into the steel ball of 150g, then pour into acetone soln,
After submerging ball grinder, cover is covered tightly, planetary ball mill is put into and carries out ball milling, after ball milling 30h, alloy powder is taken out, is put
Enter and dried in a smooth container, then the powder dried is fitted into quartz glass tube, in the case of continuous pumping, carry out true
Sky sealing will verify air-tightness in the quartz glass tube input water of sealing, if bubble-free, can assert that its leakproofness is good, then
Quartz glass tube is taken out, dries to be put into 800 DEG C of high temperature furnace after moisture and be calcined, it, will be treated after calcining 15h
Quartz glass tube takes out, and quartz glass tube is smashed after cooling, collects powder up to product.
Embodiment three：
Appropriate chemical pure acetic acid dysprosium, lithium carbonate, electrolytic manganese dioxide are taken as raw material, according to LiDy0.05Mn1.95O4Atom
Ratio dispensing 20g, the mixture material prepared is poured into ball grinder together, and puts into the steel ball of 300g, then to pour into acetone molten
After submerging ball grinder, cover is covered tightly for liquid, is put into planetary ball mill and is carried out ball milling, after ball milling 30h, alloy powder is taken out,
It is put into a smooth container and dries, then the powder dried is fitted into quartz glass tube, in the case of continuous pumping, carry out
Vacuum sealing will verify air-tightness in the quartz glass tube input water of sealing, if bubble-free, can assert that its leakproofness is good,
Quartz glass tube is taken out again, dries to be put into 900 DEG C of high temperature furnace after moisture and be calcined, after calcining 10h, processing will be passed through
Quartz glass tube take out, smash quartz glass tube after cooling, collect powder up to product.
Claims (6)
1. a kind of novel LiMn2O4Electrode material, it is characterised in that the preparation method of the material carries out as follows：
(1) appropriate chemical pure acetic acid dysprosium, lithium carbonate, electrolytic manganese dioxide are taken as raw material, according to LiDyxMn2-xO4（0.01≤X
≤0.1）Atomic ratio dispensing；
(2) a ball grinder is taken, the raw mixture prepared is poured into wherein together, and adds suitable steel ball, is carried out with ball mill
Ball milling；
(3) the alloy powder of ball milling is dried；
(4) the high-temperature calcination under the conditions of starvation by the alloy powder after drying；
(5) after calcining, powder is collected up to product.
2. a kind of novel LiMn as shown in claim 12O4Electrode material, which is characterized in that step (1) in, according to
LiDyxMn2-xO4（0.03≤X≤0.05）Atomic ratio dispensing.
3. a kind of novel LiMn as shown in claim 12O4Electrode material, which is characterized in that step (2) in, ratio of grinding media to material is
15-20。
4. a kind of novel LiMn as shown in claim 12O4Electrode material, which is characterized in that step (2) in, ball mill into
The time of row ball milling is 30-40h.
5. a kind of novel LiMn as shown in claim 12O4Electrode material, which is characterized in that step (2) in, can also will
Acetone changes gasoline or alcohol into.
6. a kind of novel LiMn as shown in claim 12O4Electrode material, which is characterized in that step (4) in, high-temperature calcination
Temperature is 700-900 DEG C, and time control is in 10-20h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611172384.0A CN108203118A (en) | 2016-12-17 | 2016-12-17 | A kind of novel LiMn2O4Electrode material and its preparation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611172384.0A CN108203118A (en) | 2016-12-17 | 2016-12-17 | A kind of novel LiMn2O4Electrode material and its preparation process |
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|---|---|
| CN108203118A true CN108203118A (en) | 2018-06-26 |
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| CN201611172384.0A Pending CN108203118A (en) | 2016-12-17 | 2016-12-17 | A kind of novel LiMn2O4Electrode material and its preparation process |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1447466A (en) * | 2003-04-04 | 2003-10-08 | 清华大学 | Method for preparing anode material of spherical lithium manganate applicable to lithium ion batteries |
| CN101780983A (en) * | 2009-01-16 | 2010-07-21 | 比亚迪股份有限公司 | Spinel Li1+xMyMn2-x-yO4, preparation method thereof and lithium-ion secondary battery |
| CN102195042A (en) * | 2010-03-09 | 2011-09-21 | 中国科学院过程工程研究所 | High performance lithium ion battery anode material lithium manganate and preparation method thereof |
| CN103441264A (en) * | 2013-09-09 | 2013-12-11 | 齐鲁工业大学 | Method for reducing dissolution of manganese in lithium manganate in electrolyte solution |
| CN105591103A (en) * | 2015-12-21 | 2016-05-18 | 李梦思 | Modification process of lithium ion battery cathode material |
-
2016
- 2016-12-17 CN CN201611172384.0A patent/CN108203118A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1447466A (en) * | 2003-04-04 | 2003-10-08 | 清华大学 | Method for preparing anode material of spherical lithium manganate applicable to lithium ion batteries |
| CN101780983A (en) * | 2009-01-16 | 2010-07-21 | 比亚迪股份有限公司 | Spinel Li1+xMyMn2-x-yO4, preparation method thereof and lithium-ion secondary battery |
| CN102195042A (en) * | 2010-03-09 | 2011-09-21 | 中国科学院过程工程研究所 | High performance lithium ion battery anode material lithium manganate and preparation method thereof |
| CN103441264A (en) * | 2013-09-09 | 2013-12-11 | 齐鲁工业大学 | Method for reducing dissolution of manganese in lithium manganate in electrolyte solution |
| CN105591103A (en) * | 2015-12-21 | 2016-05-18 | 李梦思 | Modification process of lithium ion battery cathode material |
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Application publication date: 20180626 |