CN107834027A - A kind of combination electrode material and technique for adulterating aluminium element - Google Patents
A kind of combination electrode material and technique for adulterating aluminium element Download PDFInfo
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- CN107834027A CN107834027A CN201710578231.4A CN201710578231A CN107834027A CN 107834027 A CN107834027 A CN 107834027A CN 201710578231 A CN201710578231 A CN 201710578231A CN 107834027 A CN107834027 A CN 107834027A
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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
- H01M4/364—Composites as mixtures
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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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- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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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- 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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- Inorganic Chemistry (AREA)
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- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of combination electrode material and technique for adulterating aluminium element.Using LiOH as lithium source, with FeC2O4・2H2O is as source of iron, NH4H2PO4As source of phosphoric acid, and Nd powder and Al (OH)3Powder is as doped raw material, according to Li1‑xNd xFe1‑yAlyPO4（0.02≤x≤0.1,0. 2≤y≤0.4）Atomic ratio dispensing obtain slurry through mechanical ball mill; resulting slurry is dried, obtains precursor powder, then precursor powder is heat-treated under hot conditions under inert atmosphere protection; room temperature is finally naturally cooled under inert atmosphere protection, that is, obtains combination electrode material powder.
Description
Technical field
The present invention relates to a kind of li-ion electrode materials and its preparation technology, more particularly to a kind of addition rare earth and aluminium element
Li-ion electrode materials and preparation method thereof, belong to battery electrode material field.
Background technology
With mobile phone, notebook, LEV, hybrid electric vehicle, telecommunications developing rapidly for fields such as electricity, lithium ion
Battery is widely used.Lithium ion battery is a kind of efficiently fine and close energy storage device, with LiFePO4For the poly- of representative
Anion structure phosphate material, due to spies such as the security of its protrusion, overlength cycle life, wide electrochemical window, low costs
Point receives extensive concern.LiFePO4With the hexagonal closs packing arrangement architecture somewhat distorted, belong to rhombic system, space group
For Pnma.In the a-c planes where lithium atom, include PO4Tetrahedron, which limits the mobile sky of lithium ion
Between, cause lithium ion mobility speed and electronic conductivity relatively low, this is LiFePO4The inherent defect of material, this shortcoming one
Directly constrain LiFePO4The application of lithium battery.
In order to improve LiFePO4Performance, rare earth element is often added in actual fabrication process, rare earth element is metal
" vitamin " of material, there play the role of to the performance for improving metal material to be special.Rare earth element can instead of Li position, very
Good is dissolved into olivine structural.But rare earth element is only added, to LiFePO4Conductance performance improvement unobvious,
LiFePO4The application of electrode material cannot be lifted further.
The content of the invention
The present invention prepares a kind of Li by ball-milling technology and high temperature solid-state method1-xNd xFe1-yAlyPO4Combination electrode material,
By adding rare earth Nd powder and Al (OH) during utilizing ball-milling technology and high temperature solid-state method in tradition3Powder, it is former to adulterate Nd and Al
Son, prepare Li1-xNdxFe1-yAlyPO4Combination electrode material, make up LiFePO4Deficiency, improve LiFePO4Conduction and charge and discharge
Electrical property.The method technique is simple, and presoma mixability is good, and production cost is low.The preparation technology of the electrode material powder
Comprise the following steps：
(1) using LiOH as lithium source, with FeC2O4・2H2O is as source of iron, NH4H2PO4As source of phosphoric acid, and Nd powder and Al (OH)3Powder
End is used as doped raw material, according to Li1-xNd xFe1-yAlyPO4（0.02≤x≤0.1, 0. 2≤y≤0.4）Atomic ratio dispensing,
Then add certain steel ball and obtain slurry after ball-milling medium progress mechanical ball mill 10-15 hours；
(2) resulting slurry is dried, obtains precursor powder；
(3) the precursor powder obtained by sintering step (2) carries out heat treatment 6- under inert atmosphere protection under conditions of 500 DEG C
8h；
(4) temperature is increased to 700 DEG C again, constant temperature heat treatment 10-15h；
(5) products therefrom naturally cools to room temperature under inert atmosphere protection, that is, obtains Li1-xNd xFe1-yAlyPO4Combination electrode
Material powder.
Preferentially, step (1) in, ball-milling medium is absolute alcohol or acetone.
Preferentially, step (2) in, the drying means of the presoma is spray drying.
Preferentially, step (3) in, described inert gas is the mixed gas of nitrogen, argon gas or both.
Embodiment one：
Using LiOH as lithium source, with FeC2O4・2H2O is as source of iron, NH4H2PO4As source of phosphoric acid, and Nd powder and Al (OH)3Powder
As doped raw material, according to Li0.98Nd0.02Fe0.8Al0.2PO4Atom ratio dispensing 5g mixture, the mixture that will be prepared
Raw material poured into together in ball grinder after tentatively mixing, then is situated between toward appropriate steel ball and absolute alcohol ball milling is added in ball grinder
Matter, then cover ball grinder lid and tighten screw, then put it into planetary ball mill and carry out ball milling 10 hours, remove ball
After grinding jar stands a period of time, ball grinder is opened, alloy powder slurry in ball grinder is taken out and carries out being spray-dried to obtain presoma
Powder, then powder carried out under the protective condition of nitrogen to be heated at high temperature to 500 DEG C, constant temperature 6 hours, then raise temperature extremely
700 DEG C, constant temperature 10 hours, products therefrom naturally cools to room temperature under inert atmosphere protection, collects powder and produces product.
Embodiment two：
Using LiOH as lithium source, with FeC2O4・2H2O is as source of iron, NH4H2PO4As source of phosphoric acid, and Nd powder and Al (OH)3Powder
As doped raw material, according to Li0.95Nd0.05Fe0.7Al0.3PO4Atom ratio dispensing 20g mixture, the mixture that will be prepared
Raw material poured into together in ball grinder after tentatively mixing, then is situated between toward appropriate steel ball and absolute alcohol ball milling is added in ball grinder
Matter, then cover ball grinder lid and tighten screw, then put it into planetary ball mill and carry out ball milling 12 hours, remove ball
After grinding jar stands a period of time, ball grinder is opened, alloy powder slurry in ball grinder is taken out and carries out being spray-dried to obtain presoma
Powder, then powder carried out under the protective condition of nitrogen to be heated at high temperature to 500 DEG C, constant temperature 7 hours, then raise temperature extremely
700 DEG C, constant temperature 12 hours, products therefrom naturally cools to room temperature under inert atmosphere protection, collects powder and produces product.
Embodiment three：
Using LiOH as lithium source, with FeC2O4・2H2O is as source of iron, NH4H2PO4As source of phosphoric acid, and Nd powder and Al (OH)3Powder
As doped raw material, according to Li0.9Nd0.1Fe0.6Al0.4PO4Atom ratio dispensing 50g mixture, the mixture that will be prepared
Raw material poured into together in ball grinder after tentatively mixing, then is situated between toward appropriate steel ball and absolute alcohol ball milling is added in ball grinder
Matter, then cover ball grinder lid and tighten screw, then put it into planetary ball mill and carry out ball milling 15 hours, remove ball
After grinding jar stands a period of time, ball grinder is opened, alloy powder slurry in ball grinder is taken out and carries out being spray-dried to obtain presoma
Powder, then precursor powder is fitted into the quartz glass tube of an end closure, inside full of appropriate nitrogen, then melted with thermal-flame
The fused silica tube opening other end makes its sealing, will verify air-tightness in the quartz glass tube input water of sealing, can if bubble-free
Assert that its sealing is good, will carry out being heated at high temperature to 500 DEG C under protective condition of the powder in nitrogen, constant temperature 8 hours, then
Temperature is raised to 700 DEG C, constant temperature 15 hours, products therefrom naturally cools to room temperature under inert atmosphere protection, collects powder and is
Obtain product.
Claims (4)
1. a kind of lithium ion combination electrode material, it is characterised in that the preparation method of the combination electrode material is entered as follows
OK：
(1) using LiOH as lithium source, with FeC2O4・2H2O is as source of iron, NH4H2PO4As source of phosphoric acid, and Nd powder and Al (OH)3Powder
End is used as doped raw material, according to Li1-xNd xFe1-yAlyPO4（0.02≤x≤0.1, 0. 2≤y≤0.4）Atomic ratio dispensing,
Then add certain steel ball and obtain slurry after ball-milling medium progress mechanical ball mill 10-15 hours；
(2) resulting slurry is dried, obtains precursor powder；
(3) the precursor powder obtained by sintering step (2) carries out heat treatment 6- under inert atmosphere protection under conditions of 500 DEG C
8h；
(4) temperature is increased to 700 DEG C again, constant temperature heat treatment 10-15h；
(5) products therefrom naturally cools to room temperature under inert atmosphere protection, that is, obtains Li1-xNd xFe1-yAlyPO4Combination electrode material
Feed powder body.
2. a kind of lithium ion combination electrode material as claimed in claim 1, it is characterised in that prepared by material the step of (1)
In, ball-milling medium is absolute alcohol or acetone.
3. a kind of lithium ion combination electrode material as described in claim 1 or 2, it is characterised in that in step prepared by material
Suddenly (2) in, the drying means of the presoma is spray drying.
4. a kind of lithium ion combination electrode material as described in claim 1 or 2, it is characterised in that in step prepared by material
Suddenly (3) in, described inert gas is the mixed gas of nitrogen, argon gas or both.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710578231.4A CN107834027A (en) | 2017-07-16 | 2017-07-16 | A kind of combination electrode material and technique for adulterating aluminium element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710578231.4A CN107834027A (en) | 2017-07-16 | 2017-07-16 | A kind of combination electrode material and technique for adulterating aluminium element |
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| Publication Number | Publication Date |
|---|---|
| CN107834027A true CN107834027A (en) | 2018-03-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710578231.4A Withdrawn CN107834027A (en) | 2017-07-16 | 2017-07-16 | A kind of combination electrode material and technique for adulterating aluminium element |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837033A (en) * | 2006-03-24 | 2006-09-27 | 山东科技大学 | Process for synthesizing LiFePO4 as positive electrode materials of lithium ion cell |
| CN101339994A (en) * | 2008-09-01 | 2009-01-07 | 罗绍华 | Preparation of multi-position doped lithium iron phosphate positive electrode material and application thereof |
| CN101800315A (en) * | 2010-04-09 | 2010-08-11 | 曲阜毅威能源股份有限公司 | Multielement-doped lithium iron phosphate positive electrode material and preparation method thereof |
-
2017
- 2017-07-16 CN CN201710578231.4A patent/CN107834027A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837033A (en) * | 2006-03-24 | 2006-09-27 | 山东科技大学 | Process for synthesizing LiFePO4 as positive electrode materials of lithium ion cell |
| CN101339994A (en) * | 2008-09-01 | 2009-01-07 | 罗绍华 | Preparation of multi-position doped lithium iron phosphate positive electrode material and application thereof |
| CN101800315A (en) * | 2010-04-09 | 2010-08-11 | 曲阜毅威能源股份有限公司 | Multielement-doped lithium iron phosphate positive electrode material and preparation method thereof |
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Application publication date: 20180323 |