CN108609597A - A kind of li-ion electrode materials of rare earth doped terbium, dysprosium - Google Patents
A kind of li-ion electrode materials of rare earth doped terbium, dysprosium Download PDFInfo
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- CN108609597A CN108609597A CN201611141268.2A CN201611141268A CN108609597A CN 108609597 A CN108609597 A CN 108609597A CN 201611141268 A CN201611141268 A CN 201611141268A CN 108609597 A CN108609597 A CN 108609597A
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- dysprosium
- rare earth
- ion electrode
- electrode materials
- earth doped
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
Abstract
The invention discloses the li-ion electrode materials and its technique of a kind of rare earth doped terbium, dysprosium.The technique is with FeC2O4・2H2O is as the sources Fe, with Li2CO3As the sources Li, with NH4H2PO4As PO4Source, with rare earth terbium (Tb）, dysprosium (Dy）Foreign atom.It first by it according to certain atomic ratio dispensing, then cleans through acetone, ball milling is then carried out under the protection of gasoline; ball-milled powder dries; it is then charged into the quartz glass tube full of argon gas, and seals, finally carry out high temperature sintering up to the li-ion electrode materials of a kind of rare earth doped terbium, dysprosium.The electrode material powder electricity rate is high, capacity is big, and preparation flow is controllable, easy to operate, has larger application prospect.
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 lithium of rare earth doped element
Ion electrode materials and its preparation process belong to battery electrode material field.
Background technology
Lithium ion battery is higher than energy with it, operating voltage is high, have extended cycle life, memory-less effect, it is pollution-free the advantages that,
Be widely used in portable electronics and new traffic tool, wherein common LiFePO 4 material belong to newer lithium from
Sub- cell positive material, it is safe, cost is relatively low.
LiFePO4With the hexagonal closs packing arrangement architecture slightly distorted, belong to rhombic system, space group Pnma.
Include PO in a-c planes where lithium atom4Tetrahedron, which limits the mobile spaces of lithium ion.LiFePO4
That there are room-temperature conductivities is low for electrode material, and discharge voltage is low（3.4V）, actual capacity only has the shortcomings of 114mAh/g, all makes
About itself further application, therefore, exploitation composite positive pole at anode material for lithium-ion batteries research direction it
One.
There is document to point out, rare earth element can be dissolved into olivine structural, and can well instead of the position of Li
Change and improves LiFePO4Conductivity.The present invention passes through ball-milling technology, the rare earth doped terbium (Tb of high temperature solid-state method）, dysprosium (Dy）Atom,
A kind of anode material for compound lithium ion battery is prepared, the chemical property performance of the modified electrode material of this method is excellent, tool
There is good application prospect.
Invention content
The object of the present invention is to provide the li-ion electrode materials and its preparation process of a kind of rare earth doped terbium, dysprosium.The system
Standby technique includes the following steps：
(1) the FeC for taking appropriate chemistry pure2O4・2H2O 、Li2CO3、NH4H2PO4With terbium (Tb）, dysprosium (Dy）Metal powder is as former
Material, according to Li1-（x+y）FeTbxDyyPO4（0.01≤x+y≤0.1）Atomic ratio dispensing；
(2) by the raw material prepared acetone soln soaking and washing；
(3) the raw mixture after cleaning is further risen in input ball grinder, and add suitable sucrose and steel ball, in gasoline
Under protection, ball milling is carried out with ball mill；
(4) the alloy powder after ball milling is taken out and dried, be reloaded into the quartz glass tube full of argon gas, and seal；
(5) quartz glass tube of the sealing equipped with sample is put into high temperature furnace again and is sintered, it is to be cooled after sintering, it takes out in pipe
Powder is up to a kind of compound lithium ion electrode material.
Preferentially, step (3) in, the adding proportion of sucrose and raw material is 0.2-0.3, ratio of grinding media to material 10-20.
Preferentially, step (3) in, ball mill speed control 250-350 r/min operation.
Preferentially, step (3) in, ball mill carry out ball milling time be 20-50h.
Preferentially, step (5) in, sintering temperature be 600-800 DEG C, time control is in 10-15h.
The present invention has following advantages and characteristic：
(1) the electrode material powder electricity rate prepared is high, and capacity is big；
(2) favorable reproducibility, condition are easy to control；
(3) flow is short, easy to operate.
Specific implementation mode
Embodiment one：
The FeC for taking appropriate chemistry pure2O4・2H2O 、Li2CO3、NH4H2PO4With rare earth metal Tb (Tb）, dysprosium (Dy）Powder is as former
Material, according to Li0.9FeTb0.01Dy0.09PO4Atomic ratio dispensing 5g raw material, the raw material prepared is poured into acetone soln together
In, soaking and washing is carried out, the raw material after cleaning further rises in input ball grinder, and adds 1.5g sucrose and 100g steel balls, in vapour
Under the protection of oil, ball milling is carried out with ball mill, ball milling speed is arranged 250 r/min, after ball milling 50h, simultaneously alloy powder taking-up
It dries, the powder dried is fitted into the quartz glass tube full of argon gas and is sealed, quartz glass tube is then put into 600 DEG C of height
15h is sintered in warm stove, taking-up powder in tube to be cooled is up to a kind of compound lithium ion electrode material after sintering.
Embodiment two：
The FeC for taking appropriate chemistry pure2O4・2H2O 、Li2CO3、NH4H2PO4With rare earth metal Tb (Tb）, dysprosium (Dy）Powder is as former
Material, according to Li0.9FeTb0.09Dy0.01PO4Atomic ratio dispensing 10g raw material, the raw material prepared is poured into acetone soln together
In, soaking and washing is carried out, the raw material after cleaning further rises in input ball grinder, and adds 3g sucrose and 150g steel balls, in gasoline
Protection under, carry out ball milling with ball mill, ball milling speed is arranged 300 r/min, after ball milling 30h, alloy powder is taken out and is dried in the air
It is dry, the powder dried is fitted into the quartz glass tube full of argon gas and is sealed, quartz glass tube is then put into 700 DEG C of high temperature
13h is sintered in stove, taking-up powder in tube to be cooled is up to a kind of compound lithium ion electrode material after sintering.
Embodiment three：
The FeC for taking appropriate chemistry pure2O4・2H2O 、Li2CO3、NH4H2PO4With rare earth metal Tb (Tb）, dysprosium (Dy）Powder is as former
Material, according to Li0.9FeTb0.05Dy0.05PO4Atomic ratio dispensing 20g raw material, the raw material prepared is poured into acetone soln together
In, soaking and washing is carried out, the raw material after cleaning further rises in input ball grinder, and adds 4g sucrose and 200g steel balls, in gasoline
Protection under, carry out ball milling with ball mill, ball milling speed is arranged 350 r/min, after ball milling 20h, alloy powder is taken out and is dried in the air
It is dry, the powder dried is fitted into the quartz glass tube full of argon gas and is sealed, quartz glass tube is then put into 800 DEG C of high temperature
10h is sintered in stove, taking-up powder in tube to be cooled is up to a kind of compound lithium ion electrode material after sintering.
Claims (5)
1. the li-ion electrode materials of a kind of rare earth doped terbium, dysprosium, it is characterised in that the preparation process of the electrode material is by as follows
Step carries out：
(1) the FeC for taking appropriate chemistry pure2O4・2H2O 、Li2CO3、NH4H2PO4With terbium (Tb）, dysprosium (Dy）Metal powder as raw material,
According to Li1-（x+y）FeTbxDyyPO4（0.01≤x+y≤0.1）Atomic ratio dispensing；
(2) by the raw material prepared acetone soln soaking and washing；
(3) the raw mixture after cleaning is further risen in input ball grinder, and add suitable sucrose and steel ball, in gasoline
Under protection, ball milling is carried out with ball mill；
(4) the alloy powder after ball milling is taken out and dried, be reloaded into the quartz glass tube full of argon gas, and seal；
(5) quartz glass tube of the sealing equipped with sample is put into high temperature furnace again and is sintered, it is to be cooled after sintering, it takes out in pipe
Powder is up to a kind of compound lithium ion electrode material.
2. the li-ion electrode materials of a kind of rare earth doped terbium as shown in claim 1, dysprosium, which is characterized in that step (3)
In, the adding proportion of sucrose and raw material is 0.2-0.3, ratio of grinding media to material 10-20.
3. the li-ion electrode materials of a kind of rare earth doped terbium as shown in claim 1, dysprosium, which is characterized in that step (3)
In, ball mill speed control 250-350 r/min operations.
4. the li-ion electrode materials of a kind of rare earth doped terbium as shown in claim 1, dysprosium, which is characterized in that step (3)
In, the time that ball mill carries out ball milling is 20-50h.
5. the li-ion electrode materials of a kind of rare earth doped terbium as shown in claim 1, dysprosium, which is characterized in that step (5)
In, sintering temperature is 600-800 DEG C, and time control is in 10-15h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611141268.2A CN108609597A (en) | 2016-12-12 | 2016-12-12 | A kind of li-ion electrode materials of rare earth doped terbium, dysprosium |
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| CN201611141268.2A CN108609597A (en) | 2016-12-12 | 2016-12-12 | A kind of li-ion electrode materials of rare earth doped terbium, dysprosium |
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| CN108609597A true CN108609597A (en) | 2018-10-02 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105428652A (en) * | 2015-12-23 | 2016-03-23 | 郑春燕 | Novel rare-earth-lithium iron phosphate composite electrode material and preparation method thereof |
| CN105514428A (en) * | 2015-12-23 | 2016-04-20 | 邬石根 | Composite electrode material and preparation technology thereof |
| CN105609763A (en) * | 2015-12-23 | 2016-05-25 | 郑春燕 | Rare earth Y doped lithium iron phosphate electrode material and preparation method thereof |
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2016
- 2016-12-12 CN CN201611141268.2A patent/CN108609597A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105428652A (en) * | 2015-12-23 | 2016-03-23 | 郑春燕 | Novel rare-earth-lithium iron phosphate composite electrode material and preparation method thereof |
| CN105514428A (en) * | 2015-12-23 | 2016-04-20 | 邬石根 | Composite electrode material and preparation technology thereof |
| CN105609763A (en) * | 2015-12-23 | 2016-05-25 | 郑春燕 | Rare earth Y doped lithium iron phosphate electrode material and preparation method thereof |
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Application publication date: 20181002 |