CN105226280A - The preparation technology of LiFePO4 - Google Patents
The preparation technology of LiFePO4 Download PDFInfo
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- CN105226280A CN105226280A CN201510678465.7A CN201510678465A CN105226280A CN 105226280 A CN105226280 A CN 105226280A CN 201510678465 A CN201510678465 A CN 201510678465A CN 105226280 A CN105226280 A CN 105226280A
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- solution
- organic
- deionized water
- inorganic solution
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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
-
- 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
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- 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 present invention relates to the preparation technology of LiFePO4, comprise the following steps: configuration inorganic solution I, inorganic solution II, by inorganic solution II slowly to add in inorganic solution I, stir and form inorganic solution; Dispersant, organic carbon source and deionized water are added in beaker, stir to clarify solution and become organic solution, take in ferrous oxalate and agate jar by P:Fe=0.95:0.9, add inorganic solution, organic solution, carry out ball milling, make mixing of materials evenly make the grain diameter nano of slurry simultaneously; Then be atomized, namely once sintered, dry, double sintering obtains product LiFe
0.9p
0.95o
4-x.LiFePO 4 material prepared by the present invention be applied to lithium battery that positive electrode makes can capacity high, stability good, uniform particles.
Description
Technical field
The present invention relates to lithium battery material field, particularly, relate to a kind of preparation technology of LiFePO4.
Background technology
Along with the fast development of traffic, communication and the industrialization of information, the products such as electric automobile, notebook computer and mobile communications tool propose higher and very urgent requirement to Development of Novel chemical power source.Development of new secondary green battery has become and must need.Lithium ion battery is relative to traditional secondary battery, due to its have that energy density is high, power density is high, operating voltage is high, self-discharge rate is low, memory-less effect, have extended cycle life, the unique advantage such as pollution-free, become rapidly a kind of most important and state-of-the-art secondary cell.Having become the ideal source of the electronic installation miniaturization ands such as video camera, mobile phone, notebook computer and portable surveying instrument, is also the first-selected power supply of following light high-energy electrokinetic cell used for electric vehicle.
At present, in commercial Li-ion battery, great majority adopt carbon electrode as negative material.But because the current potential in the current potential of carbon electrode after slotting lithium and metal is very close, and most electrolyte is unstable under this current potential, and electrolyte easily decomposes at electrode surface.So when over-charging of battery, carbon electrodes easily separates out very active lithium metal, form the dendrite of lithium, the danger that barrier film causes short circuit may be pierced through, and the thermal runaway that high temperature is, affect the security performance of battery.Researcher is also to the negative material of other many lithium-ions battery, as lithium alloy, oxide, sulfide and high molecular polymer etc. are explored, at present, these materials are all undesirable, some can not solve the hidden danger in safety, and some is then that cycle performance is too poor etc.Therefore, finding the new negative material substituting carbon electrode is, one of Main way of research at present.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly has that gram volume is high, stability good, the preparation technology of evengranular LiFePO4.
The present invention's adopted technical scheme that solves the problem is: the preparation technology of LiFePO4, comprises the following steps:
1), configuration inorganic solution I: weigh phosphoric acid, deionized water, magnesium acetate in beaker, stir to clarify solution, the mass ratio of phosphoric acid, deionized water, magnesium acetate is 1 ~ 2:10:0.5 ~ 1;
2), inorganic solution II: take lithium carbonate and deionized water in beaker, stir, the mass ratio of lithium carbonate, deionized water is 1 ~ 3:10;
3), inorganic solution: by inorganic solution II slowly to add in inorganic solution I, stir 30min, namely form inorganic solution;
4), organic solution: add in beaker by dispersant, organic carbon source and deionized water, stir to clarify solution and namely form organic solution, dispersant, organic carbon source, deionized mass ratio are 2 ~ 3:0.5 ~ 1:10;
5), by P:Fe=0.95:0.9 take in ferrous oxalate and agate jar, add inorganic solution, organic solution, carry out ball milling, make mixing of materials evenly make the grain diameter nano of slurry simultaneously;
6), be atomized: ball milling disposed slurry in step 5) is carried out atomization drying, and air inlet, air outlet temperature are set to 330 DEG C, 145 DEG C respectively;
7), once sintered: powder after atomization in step 6) is sintered in air atmosphere;
8), broken: mortar by broken for rear material once sintered in step 7), and carry out 200 orders and sieves;
9), dry: the material after fragmentation being sieved is dry under vacuum environment;
10), double sintering: be incubated 5h by dried under 350 DEG C of conditions, then be warming up to 700 DEG C of insulation 10h, obtain product LiFe
0.9p
0.95o
4-x.
Further, described in step 1), the mass ratio of phosphoric acid, deionized water, magnesium acetate is 1.5:10:0.8.
Further, step 2) described lithium carbonate, deionized water mass ratio be 2:10.
Further, dispersant described in step 4) is polyethylene glycol.
Further, organic carbon source described in step 4) is at least one in organic carbonate, Organic Alcohol, organic carbonate.
Further, double sintering described in step 10) carries out under argon shield.
To sum up, the invention has the beneficial effects as follows:
1, of the present invention simple to operate, and environmentally friendly, reduce production cost, be easy to suitability for industrialized production.
2, the LiFePO 4 material that prepared by the present invention be applied to lithium battery that positive electrode makes can capacity high, stability good.
Embodiment
Below in conjunction with embodiment, to the detailed description further of invention do, but embodiments of the present invention are not limited thereto.
Embodiment 1:
The preparation technology of LiFePO4, comprises the following steps:
1), configuration inorganic solution I: weigh phosphoric acid, deionized water, magnesium acetate in beaker, stir to clarify solution, the mass ratio of phosphoric acid, deionized water, magnesium acetate is 1:10:0.5;
2), inorganic solution II: take lithium carbonate and deionized water in beaker, stir, the mass ratio of lithium carbonate, deionized water is 1:10;
3), inorganic solution: by inorganic solution II slowly to add in inorganic solution I, stir 30min, namely form inorganic solution;
4), organic solution: add in beaker by dispersant, organic carbon source and deionized water, stir to clarify solution and namely form organic solution, dispersant, organic carbon source, deionized mass ratio are 2:0.5:10; Described dispersant is polyethylene glycol; Described organic carbon source is organic carbonate;
5), by P:Fe=0.95:0.9 take in ferrous oxalate and agate jar, add inorganic solution, organic solution, carry out ball milling, make mixing of materials evenly make the grain diameter nano of slurry simultaneously;
6), be atomized: ball milling disposed slurry in step 5) is carried out atomization drying, and air inlet, air outlet temperature are set to 330 DEG C, 145 DEG C respectively;
7), once sintered: powder after atomization in step 6) is sintered in air atmosphere;
8), broken: mortar by broken for rear material once sintered in step 7), and carry out 200 orders and sieves;
9), dry: the material after fragmentation being sieved is dry under vacuum environment;
10), double sintering: be incubated 5h by dried under argon shield under 350 DEG C of conditions, then be warming up to 700 DEG C of insulation 10h, obtain product LiFe
0.9p
0.95o
4-x.
Embodiment 2:
The preparation technology of LiFePO4, comprises the following steps:
1), configuration inorganic solution I: weigh phosphoric acid, deionized water, magnesium acetate in beaker, stir to clarify solution, the mass ratio of phosphoric acid, deionized water, magnesium acetate is 1.5:10:0.8;
2), inorganic solution II: take lithium carbonate and deionized water in beaker, stir, the mass ratio of lithium carbonate, deionized water is 2:10;
3), inorganic solution: by inorganic solution II slowly to add in inorganic solution I, stir 30min, namely form inorganic solution;
4), organic solution: add in beaker by dispersant, organic carbon source and deionized water, stir to clarify solution and namely form organic solution, dispersant, organic carbon source, deionized mass ratio are 2.5:0.8:10; Described dispersant is polyethylene glycol; Described organic carbon source is Organic Alcohol;
5), by P:Fe=0.95:0.9 take in ferrous oxalate and agate jar, add inorganic solution, organic solution, carry out ball milling, make mixing of materials evenly make the grain diameter nano of slurry simultaneously;
6), be atomized: ball milling disposed slurry in step 5) is carried out atomization drying, and air inlet, air outlet temperature are set to 330 DEG C, 145 DEG C respectively;
7), once sintered: powder after atomization in step 6) is sintered in air atmosphere;
8), broken: mortar by broken for rear material once sintered in step 7), and carry out 200 orders and sieves;
9), dry: the material after fragmentation being sieved is dry under vacuum environment;
10), double sintering: be incubated 5h by dried under argon shield under 350 DEG C of conditions, then be warming up to 700 DEG C of insulation 10h, obtain product LiFe
0.9p
0.95o
4-x.
Embodiment 3:
The preparation technology of LiFePO4, comprises the following steps:
1), configuration inorganic solution I: weigh phosphoric acid, deionized water, magnesium acetate in beaker, stir to clarify solution, the mass ratio of phosphoric acid, deionized water, magnesium acetate is 2:10:1;
2), inorganic solution II: take lithium carbonate and deionized water in beaker, stir, the mass ratio of lithium carbonate, deionized water is 3:10;
3), inorganic solution: by inorganic solution II slowly to add in inorganic solution I, stir 30min, namely form inorganic solution;
4), organic solution: add in beaker by dispersant, organic carbon source and deionized water, stir to clarify solution and namely form organic solution, dispersant, organic carbon source, deionized mass ratio are 3:1:10; Described dispersant is polyethylene glycol; Described organic carbon source is organic carbonate;
5), by P:Fe=0.95:0.9 take in ferrous oxalate and agate jar, add inorganic solution, organic solution, carry out ball milling, make mixing of materials evenly make the grain diameter nano of slurry simultaneously;
6), be atomized: ball milling disposed slurry in step 5) is carried out atomization drying, and air inlet, air outlet temperature are set to 330 DEG C, 145 DEG C respectively;
7), once sintered: powder after atomization in step 6) is sintered in air atmosphere;
8), broken: mortar by broken for rear material once sintered in step 7), and carry out 200 orders and sieves;
9), dry: the material after fragmentation being sieved is dry under vacuum environment;
10), double sintering: be incubated 5h by dried under argon shield under 350 DEG C of conditions, then be warming up to 700 DEG C of insulation 10h, obtain product LiFe
0.9p
0.95o
4-x.
As mentioned above, the present invention can be realized preferably.
Claims (6)
1. the preparation technology of LiFePO4, is characterized in that, comprises the following steps:
1), configuration inorganic solution I: weigh phosphoric acid, deionized water, magnesium acetate in beaker, stir to clarify solution, the mass ratio of phosphoric acid, deionized water, magnesium acetate is 1 ~ 2:10:0.5 ~ 1;
2), inorganic solution II: take lithium carbonate and deionized water in beaker, stir, the mass ratio of lithium carbonate, deionized water is 1 ~ 3:10;
3), inorganic solution: by inorganic solution II slowly to add in inorganic solution I, stir 30min, namely form inorganic solution;
4), organic solution: add in beaker by dispersant, organic carbon source and deionized water, stir to clarify solution and namely form organic solution, dispersant, organic carbon source, deionized mass ratio are 2 ~ 3:0.5 ~ 1:10;
5), by P:Fe=0.95:0.9 take in ferrous oxalate and agate jar, add inorganic solution, organic solution, carry out ball milling, make mixing of materials evenly make the grain diameter nano of slurry simultaneously;
6), be atomized: ball milling disposed slurry in step 5) is carried out atomization drying, and air inlet, air outlet temperature are set to 330 DEG C, 145 DEG C respectively;
7), once sintered: powder after atomization in step 6) is sintered in air atmosphere;
8), broken: mortar by broken for rear material once sintered in step 7), and carry out 200 orders and sieves;
9), dry: the material after fragmentation being sieved is dry under vacuum environment;
10), double sintering: be incubated 5h by dried under 350 DEG C of conditions, then be warming up to 700 DEG C of insulation 10h, obtain product LiFe
0.9p
0.95o
4-x.
2. the preparation technology of LiFePO4 according to claim 1, is characterized in that, described in step 1), the mass ratio of phosphoric acid, deionized water, magnesium acetate is 1.5:10:0.8.
3. the preparation technology of LiFePO4 according to claim 1, is characterized in that, step 2) described lithium carbonate, deionized water mass ratio be 2:10.
4. the preparation technology of LiFePO4 according to claim 1, is characterized in that, dispersant described in step 4) is polyethylene glycol.
5. the preparation technology of LiFePO4 according to claim 1, is characterized in that, organic carbon source described in step 4) is at least one in organic carbonate, Organic Alcohol, organic carbonate.
6., according to the preparation technology of the arbitrary described LiFePO4 of claim 1 to 5, it is characterized in that, double sintering described in step 10) carries out under argon shield.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510678465.7A CN105226280A (en) | 2015-10-20 | 2015-10-20 | The preparation technology of LiFePO4 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510678465.7A CN105226280A (en) | 2015-10-20 | 2015-10-20 | The preparation technology of LiFePO4 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102651474A (en) * | 2012-05-24 | 2012-08-29 | 四川科能锂电有限公司 | Preparation method of anode active material lithium iron phosphate of lithium battery |
| CN103022495A (en) * | 2012-12-11 | 2013-04-03 | 彩虹集团公司 | Preparation method of high-electrical conductivity lithium iron phosphate |
| CN103066280A (en) * | 2012-12-28 | 2013-04-24 | 珠海泰坦能源电子技术有限公司 | Spherical lithium iron phosphate anode material and preparation method thereof |
| CN104393255A (en) * | 2013-10-07 | 2015-03-04 | 台塑生医科技股份有限公司 | Preparation method and application of composite spherical lithium iron material/carbon cathode material |
-
2015
- 2015-10-20 CN CN201510678465.7A patent/CN105226280A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102651474A (en) * | 2012-05-24 | 2012-08-29 | 四川科能锂电有限公司 | Preparation method of anode active material lithium iron phosphate of lithium battery |
| CN103022495A (en) * | 2012-12-11 | 2013-04-03 | 彩虹集团公司 | Preparation method of high-electrical conductivity lithium iron phosphate |
| CN103066280A (en) * | 2012-12-28 | 2013-04-24 | 珠海泰坦能源电子技术有限公司 | Spherical lithium iron phosphate anode material and preparation method thereof |
| CN104393255A (en) * | 2013-10-07 | 2015-03-04 | 台塑生医科技股份有限公司 | Preparation method and application of composite spherical lithium iron material/carbon cathode material |
Non-Patent Citations (1)
| Title |
|---|
| ZHAO-HUI WANG, ET AL.: ""Electrochemical performance in Na-incorporated nonstoichiometric LiFePO4/C composites with controllable impurity phases"", 《ELECTROCHIMICA ACTA》 * |
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Application publication date: 20160106 |