CN108615856A - A kind of li-ion electrode materials and its preparation process of addition dysprosium element - Google Patents
A kind of li-ion electrode materials and its preparation process of addition dysprosium element Download PDFInfo
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- CN108615856A CN108615856A CN201611133989.9A CN201611133989A CN108615856A CN 108615856 A CN108615856 A CN 108615856A CN 201611133989 A CN201611133989 A CN 201611133989A CN 108615856 A CN108615856 A CN 108615856A
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- glass tube
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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
- 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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- 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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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of li-ion electrode materials and its preparation process of addition dysprosium element.Its preparation process is：Suitable chemistry pure Dy, FeC are weighed first, in accordance with certain proportion2O4・2H2O 、Li2CO3、NH4H2PO4、Cr2O3Powder, it is put into ball grinder after acetone soln cleans, suitable sucrose is added again, fluid-tight is carried out with acetone soln, it places into and carries out ball milling in planetary ball mill, dried after ball milling, the powder under vacuum dried is sealed in quartz glass tube, then the quartz glass tube equipped with sample powder is put into high temperature furnace and carries out high-temperature calcination, powder is taken out after calcining up to product.
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 electrode of addition Dy elements
Material and its preparation process belong to battery electrode material field.
Background technology
It by lithium metal or lithium alloy is negative material, using the battery of non-aqueous electrolytic solution that lithium battery, which is a kind of,.At present
Common anode material for lithium-ion batteries mainly has the cobalt acid lithium of layer structure and the LiFePO4 of olivine structural etc..Wherein,
LiFePO4Belong to newer positive electrode, it is safe, cost is relatively low, but that there are room-temperature conductivities is low, and discharge voltage is low
（3.4V）, tap density it is low, actual capacity only has the shortcomings of 114mAh/g, all constrains the further application of itself, because
This, exploitation composite positive pole is at one of research direction of anode material for lithium-ion batteries.
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, therefore it
Conductivity Ratio others lamellar compound is low.There is document to point out, rare earth element can be well dissolved into instead of the position of Li
In olivine structural, and it can change and improve LiFePO4Conductivity.
The present invention by by ball-milling technology, the rare earth doped element Dy of high temperature solid-state method and Cr elements, preparing a kind of again
Li1-xFe0.9Cr0.1Dy xPO4Composite lithium ion cell composite positive pole makes up the deficiency of LiFePO4.
Invention content
The object of the present invention is to provide a kind of li-ion electrode materials and its preparation process of addition dysprosium element.The preparation work
Skill includes the following steps：
(1) the FeC for taking appropriate chemistry pure2O4・2H2O 、Li2CO3、NH4H2PO4、Cr2O3With metal Dy powder as raw material, according to
Li1-xFe0.9Cr0.1DyxPO4（0.01≤X≤0.1）Atomic ratio dispensing；
(2) the raw material prepared is poured into together in acetone soln and cleaned and filtered；
(3) the raw mixture being collected by filtration is poured into ball grinder together again, and add suitable sucrose and steel ball, in acetone
Protection under, carry out ball milling with planetary ball mill；
Ball milling for a period of time after, alloy powder is taken out and is dried；
(5) the powder dried is fitted into quartz glass tube, carries out vacuum sealing；
(6) glass tube is put into water, if bubble-free, its leakproofness can be examined good；
(7) glass tube is taken out again, be put into high temperature furnace, calcined after drying moisture；
(8) treated glass tube is taken out, glass tube is smashed after cooling, collect powder up to product.
Preferentially, step (1) in, according to Li1-xFe0.9Cr0.1DyxPO4（0.03≤X≤0.05）Atomic ratio dispensing.
Preferentially, step (3) in, ratio of grinding media to material 15-20, planetary ball mill speed control 250-350 r/min fortune
Row.
Preferentially, step (4) in, the time that ball milling is carried out with planetary ball mill is 20-40h.
Preferentially, step (7) in, high-temperature calcination temperature be 600-800 DEG C, time control is in 10-15h.
The present invention has following advantages and characteristic：
(1) the electrode material conductivity prepared is high, and capacity is big；
(2) preparation process is simple, and flow is short；
Embodiment one：
First with the pure FeC of chemistry2O4・2H2O 、Li2CO3、NH4H2PO4、Cr2O3With metal Dy powder as raw material, according to
Li0.99Fe0.9Cr0.1Dy0.01PO4Atomic ratio dispensing 5g mixture, it is molten that the mixture material prepared is poured into acetone together
In liquid, cleaned and filtered, the raw mixture being collected by filtration is poured into ball grinder together again, and add 3g sucrose and
The steel ball of 100g, then acetone soln is poured into, after submerging ball grinder, cover is covered tightly, planetary ball mill is put into and carries out ball milling, ball
After grinding speed setting 250 r/min, ball milling 40h, alloy powder is taken out, is put into a smooth container and dries, then will dry
Powder be fitted into quartz glass tube, in the case of continuous pumping, carry out vacuum sealing, the quartz glass tube of sealing put into
Air-tightness is verified in water, if bubble-free, can be assert that its leakproofness is good, then quartz glass tube is taken out, be put after drying moisture
Enter and calcined in 600 DEG C of high temperature furnace, after calcining 15h, treated quartz glass tube is taken out, smashes quartz after cooling
Glass tube collects powder up to product.
Embodiment two：
First with the pure FeC of chemistry2O4・2H2O 、Li2CO3、NH4H2PO4、Cr2O3With metal Dy powder as raw material, according to
Li0.95Fe0.9Cr0.1Dy0.05PO4Atomic ratio dispensing 10g mixture, the mixture material prepared is poured into acetone together
It in solution, is cleaned and is filtered, the raw mixture being collected by filtration is poured into ball grinder together again, and add the sucrose of 4g
With the steel ball of 150g, then acetone soln is poured into, after submerging ball grinder, cover is covered tightly, is put into planetary ball mill and carry out ball milling,
After ball milling speed setting 300 r/min, ball milling 30h, alloy powder is taken out, is put into a smooth container and dries, then will dry in the air
Dry powder is fitted into quartz glass tube, in the case of continuous pumping, carries out vacuum sealing, the quartz glass tube of sealing is thrown
Enter and verify air-tightness in water, if bubble-free, can assert that its leakproofness is good, then quartz glass tube is taken out, after drying moisture
It is put into 700 DEG C of high temperature furnace and is calcined, after calcining 13h, treated quartz glass tube is taken out, smash stone after cooling
English glass tube collects powder up to product.
Embodiment three：
First with the pure FeC of chemistry2O4・2H2O 、Li2CO3、NH4H2PO4、Cr2O3With metal Dy powder as raw material, according to
Li0.9Fe0.9Cr0.1Dy0.1PO4Atomic ratio dispensing 20g mixture, it is molten that the mixture material prepared is poured into acetone together
In liquid, cleaned and filtered, the raw mixture being collected by filtration is poured into ball grinder together again, and add 5g sucrose and
The steel ball of 300g, then acetone soln is poured into, after submerging ball grinder, cover is covered tightly, planetary ball mill is put into and carries out ball milling, ball
After grinding speed setting 350 r/min, ball milling 20h, alloy powder is taken out, is put into a smooth container and dries, then will dry
Powder be fitted into quartz glass tube, in the case of continuous pumping, carry out vacuum sealing, the quartz glass tube of sealing put into
Air-tightness is verified in water, if bubble-free, can be assert that its leakproofness is good, then quartz glass tube is taken out, be put after drying moisture
Enter and calcined in 800 DEG C of high temperature furnace, after calcining 10h, treated quartz glass tube is taken out, smashes quartz after cooling
Glass tube collects powder up to product.
Claims (5)
1. a kind of preparation process of the li-ion electrode materials of addition dysprosium element, it is characterised in that the preparation method is as follows
It carries out：
(1) the FeC for taking appropriate chemistry pure2O4・2H2O 、Li2CO3、NH4H2PO4、Cr2O3With metal Dy powder as raw material, according to
Li1-xFe0.9Cr0.1DyxPO4（0.01≤X≤0.1）Atomic ratio dispensing；
(2) the raw material prepared is poured into together in acetone soln and cleaned and filtered；
(3) the raw mixture being collected by filtration is poured into ball grinder together again, and add suitable sucrose and steel ball, in acetone
Protection under, carry out ball milling with planetary ball mill；
Ball milling for a period of time after, alloy powder is taken out and is dried；
(5) the powder dried is fitted into quartz glass tube, carries out vacuum sealing；
(6) glass tube is put into water, if bubble-free, its leakproofness can be examined good；
(7) glass tube is taken out again, be put into high temperature furnace, calcined after drying moisture；
(8) treated glass tube is taken out, glass tube is smashed after cooling, collect powder up to product.
2. a kind of preparation process of the li-ion electrode materials of addition dysprosium element as shown in claim 1, which is characterized in that
Step (1) in, according to Li1-xFe0.9Cr0.1DyxPO4（0.03≤X≤0.05）Atomic ratio dispensing.
3. a kind of preparation process of the li-ion electrode materials of addition dysprosium element as shown in claim 1, which is characterized in that
Step (3) in, ratio of grinding media to material 15-20, planetary ball mill speed control 250-350 r/min operation.
4. a kind of preparation process of the li-ion electrode materials of addition dysprosium element as shown in claim 1, which is characterized in that
Step (4) in, the time that ball milling is carried out with planetary ball mill is 20-40h.
5. a kind of preparation process of the li-ion electrode materials of addition dysprosium element as shown in claim 1, which is characterized in that
Step (7) in, high-temperature calcination temperature be 600-800 DEG C, time control is in 10-15h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611133989.9A CN108615856A (en) | 2016-12-10 | 2016-12-10 | A kind of li-ion electrode materials and its preparation process of addition dysprosium element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611133989.9A CN108615856A (en) | 2016-12-10 | 2016-12-10 | A kind of li-ion electrode materials and its preparation process of addition dysprosium element |
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| Publication Number | Publication Date |
|---|---|
| CN108615856A true CN108615856A (en) | 2018-10-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611133989.9A Withdrawn CN108615856A (en) | 2016-12-10 | 2016-12-10 | A kind of li-ion electrode materials and its preparation process of addition dysprosium element |
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| CN (1) | CN108615856A (en) |
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2016
- 2016-12-10 CN CN201611133989.9A patent/CN108615856A/en not_active Withdrawn
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Application publication date: 20181002 |