CN116462175A - Wide-channel lithium iron phosphate and preparation method thereof - Google Patents
Wide-channel lithium iron phosphate and preparation method thereof Download PDFInfo
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- CN116462175A CN116462175A CN202310479864.5A CN202310479864A CN116462175A CN 116462175 A CN116462175 A CN 116462175A CN 202310479864 A CN202310479864 A CN 202310479864A CN 116462175 A CN116462175 A CN 116462175A
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- iron phosphate
- lithium iron
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 24
- 238000011282 treatment Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000011148 porous material Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 15
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 10
- 239000001488 sodium phosphate Substances 0.000 claims description 10
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical group [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 28
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 28
- 238000009792 diffusion process Methods 0.000 abstract description 20
- 239000010405 anode material Substances 0.000 abstract description 15
- 239000007774 positive electrode material Substances 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 description 18
- 230000008569 process Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910010710 LiFePO Inorganic materials 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 239000002033 PVDF binder Substances 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 5
- 239000006245 Carbon black Super-P Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000006258 conductive agent Substances 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000003837 high-temperature calcination Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000010450 olivine Substances 0.000 description 2
- 229910052609 olivine Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910002589 Fe-O-Fe Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to the technical field of lithium iron phosphate anode materials, and discloses a wide-channel lithium iron phosphate, wherein sodium ions enter a pore canal of the lithium iron phosphate. The preparation method comprises the following steps: and (3) blending the lithium iron phosphate and the sodium ion medium raw material solution, and carrying out pressure treatment and post-treatment on the obtained finished product. According to the invention, the lithium iron phosphate material is put into the sodium salt for post-treatment modification, the characteristic that the size of sodium ions is larger than that of lithium ions is ingeniously utilized, and the sodium ions are doped into the lithium ion diffusion channel to prop open the pore canal, so that the effect of improving the multiplying power performance of the lithium iron phosphate positive electrode material is achieved.
Description
Technical Field
The invention relates to the technical field of lithium iron phosphate anode materials, in particular to a wide-channel lithium iron phosphate and a preparation method thereof.
Background
The lithium iron phosphate anode material has the advantages of stable structure, safety, no pollution, low price and the like, is widely applied, and has relatively excellent discharge capacity and material processability.
In recent years, lithium ion batteries are increasingly used in various fields. The service environment of the battery is complex, and the performance requirement on the battery is higher. The lithium iron phosphate anode material has outstanding safety performance due to the relatively stable olivine structure. In the olivine structured phosphate system, all oxygen ions are bound to P by strong covalent bonds 5+ Form stable (PO 4 ) 3- A group. Oxygen in the crystal lattice is not easily lost because of (PO 4 ) 3- Very strong covalent interactions stabilize Fe 2+ /Fe 3+ The reverse bond structure of the lithium ion battery material is not decomposed to generate oxygen due to deep deintercalation of lithium under the normal overcharge condition, so that the material has better safety.
LiFePO 4 The crystal is made of LiO 6 Octahedron and FeO 6 Octahedral PO 4 Tetrahedra are contained in this spatial structure. On the ab plane, liO 6 Octahedron, feO 6 Octahedral and PO 4 The tetrahedrons are alternately arranged to form a layered scaffold structure. But FeO 6 Octahedral common-vertex quilt PO 4 Tetrahedral separation without continuous FeO 6 The co-prismatic octahedral network can not form an electron conductor, and the conduction of electrons can only be carried out through Fe-O-Fe, so that LiFePO 4 Is about 10 a decrease in electron conductivity -9 S/cm magnitude. Located in LiO 6 Octahedron and FeO 6 PO between octahedrons 4 Tetrahedra to a great extent limit Li + Such that Li + The diffusion rate therein is low, at about 1.8X10 -16 -2.2×10 -14 cm 2 And/s. LiFePO at room temperature 4 The electron conductance of (c) is also much lower than that of other cathode materials. Lithium ions migrate only along the b-axis direction and are transported in LiFePO 4 Lithium ion in [010 ] along]And [001]The activation energy of the directional transport is 0.27eV and 2.5eV, respectively, so the lowest energy channel of the lithium ion transmission energy is [010 ]]In the direction, the diffusion channel is easily blocked or damaged by impurities, so that the actual lithium ion diffusion coefficient of the lithium iron phosphate material is reduced. Thereby causing a slow rate of lithium ion exchange and deterioration of the rate capability of the battery.
Chinese patent publication No. CN104979557a discloses a high-rate lithium iron phosphate positive electrode material and a battery pole piece, and the preparation method comprises: electroless plating metal aluminum simple substance on the surface of the lithium iron phosphate; the doped graphene can greatly improve the conductivity of the lithium iron phosphate material. According to the invention, a layer of aluminum metal is uniformly coated on the surface of lithium iron phosphate, then a composite material is formed by the aluminum metal and graphene, and the graphene is distributed in or on the surface of lithium iron phosphate particles to form a long-range conductive network. Although the preparation method improves the conductivity of the lithium iron phosphate anode material, the preparation method has limited effect on solving the problem of difficult diffusion of lithium ions in the lithium iron phosphate material, and the composite doping step is complicated, and the price of graphene and vapor deposition metal aluminum materials is high.
Chinese patent publication No. CN105789620a discloses a preparation method of lithium iron phosphate positive electrode material and lithium iron phosphate positive electrode material, the preparation method comprises: the solid phase synthesis method is adopted to prepare lithium iron phosphate, the solid phase synthesis method comprises ball milling mixing and high-temperature calcination, acetylene is introduced into inert atmosphere during calcination, carbon nanotubes are formed inside the generated lithium iron phosphate particles and between the lithium iron phosphate particles, and the high-conductivity lithium iron phosphate anode material is obtained. Although the preparation method improves the conductivity of the anode material, the preparation method of high-temperature calcination and heat preservation consumes more energy, and acetylene gas is required to be introduced in the calcination process.
From the crystal structure of the material, lithium ions are transported mainly through one-dimensional channels. The main bottleneck problem is that the channel transmission severely limits the diffusion rate of lithium ions. Therefore, enlarging the size of the lithium ion diffusion channel becomes an effective solution.
At present, a simple and economical preparation method for improving the lithium ion diffusion channel of the lithium iron phosphate positive electrode material does not exist.
Disclosure of Invention
< technical problem to be solved by the invention >
The method for improving the lithium ion diffusion channel of the lithium iron phosphate positive electrode material is used for solving the problems of complex method and high energy consumption in the prior art.
< technical scheme adopted by the invention >
Aiming at the technical problems, the invention aims to provide wide-channel lithium iron phosphate and a preparation method thereof.
According to the invention, the lithium iron phosphate material is put into the sodium salt for post-treatment modification, the characteristic that the size of sodium ions is larger than that of lithium ions is ingeniously utilized, and the sodium ions are doped into the lithium ion diffusion channel to prop open the pore canal, so that the effect of improving the multiplying power performance of the lithium iron phosphate positive electrode material is achieved.
The specific contents are as follows:
first, the invention provides a wide-channel lithium iron phosphate, sodium ions enter into the pore canal of the lithium iron phosphate.
Second, the present invention provides a method for preparing the aforementioned wide-channel lithium iron phosphate, comprising the steps of:
and (3) blending the lithium iron phosphate and the sodium ion medium raw material solution, and carrying out pressure treatment and post-treatment on the obtained finished product.
< beneficial effects achieved by the invention >
(1) The wide-channel lithium iron phosphate provided by the invention adopts sodium salt as a reaction raw material, and the sodium salt has mature process and low cost.
(2) The preparation method of the wide-channel lithium iron phosphate provided by the invention is a post-treatment technology, can directly process a finished product lithium iron phosphate material, and has simple and effective working procedures.
(3) The preparation method of the wide-channel lithium iron phosphate provided by the invention does not need high-temperature calcination and other processes, and has the advantages of simple process, low pollution and low energy consumption.
(4) According to the wide-channel lithium iron phosphate disclosed by the invention, sodium ions are innovatively fed into the pore canal, so that the effect of expanding a lithium ion diffusion channel is achieved.
Drawings
Fig. 1 is a specific capacity of a wide channel lithium iron phosphate button cell at different discharge rates.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
< technical solution >
First, the present invention provides a wide channel lithium iron phosphate by introducing sodium ions into the pores of the lithium iron phosphate.
Further, sodium ions and lithium iron phosphate are subjected to a pressure heating treatment at least once.
Further, the number of times of pressurization is 3-5, and the container is a pressure reaction kettle. Through multiple treatments, more sodium ions can enter the pore canal and the pore canal is opened at high temperature. The pressure reaction kettle is used as a reaction container, the pressure reaction kettle is convenient to operate in a laboratory or production, and the bottle liner of the pressure reaction kettle is resistant to corrosion of strong acid and strong alkali, so that materials can be put into a solution for quick dissolution.
Further, heating to 180-300 ℃ for 3-10 h. More preferably, the heating is carried out to 180-220 ℃ for 3-5 h.
Further, the medium raw material of sodium ions is soluble sodium salt; the sodium salt is sodium phosphate.
Secondly, the invention provides a preparation method of wide-channel lithium iron phosphate, which comprises the following steps:
and (3) blending the lithium iron phosphate and the sodium ion medium raw material solution, and carrying out pressure treatment and post-treatment on the obtained finished product.
Further, the molar mass ratio of the lithium iron phosphate to the sodium ion medium raw material is 10-20:1; and/or the mass concentration of the sodium ion medium raw material solution is 1-10%.
Further, the post-treatment comprises washing and filtering; the mass ratio of the finished product to the washing water is controlled to be 1:10-50 in the washing process. Part of sodium ions remained in the deep part of the pore canal can keep the wide channel state of the lattice pore canal, thereby facilitating the entry and exit of lithium ions and effectively improving the multiplying power performance of lithium iron phosphate.
< example >
Example 1
The embodiment provides a LiFePO with wide channel 4 The following operations are performed:
according to the molar mass ratio of the lithium iron phosphate to the sodium phosphate being 10:1, 157.76g of lithium iron phosphate powder and 800ml of 2% sodium phosphate solution are weighed and added into a pressure reaction kettle, the reaction kettle is heated to 180 ℃ after being well sealed, the container is cooled to room temperature after continuous reaction for 3 hours, and the operation is repeated for 3 times. 1577.6g of purified water was added thereto for washing for 1 hour.
According to measurement, the lithium ion diffusion channel of the lithium iron phosphate positive electrode material prepared in the embodiment is expanded, and the diffusion rate of lithium ions is improved. The lithium iron phosphate anode material prepared in the embodiment is used as an anode, super-P is used as a conductive agent, polyvinylidene fluoride (PVDF) is used as a binder to prepare an electrode slice, and metallic lithium is used as a cathode to assemble a button cell for electrochemical performance test.
The test result shows that the first gram capacity of the positive electrode material is 160.2mAh/g, the theoretical gram capacity is 170mAh/g, the 1C discharge gram capacity is 156.1mAh/g, and the 2C discharge gram capacity is 148.6mAh/g. Therefore, the lithium iron phosphate anode material prepared by the embodiment has improved rate discharge performance.
Example 2
The embodiment provides a LiFePO with wide channel 4 The following operations are performed:
according to the molar mass ratio of the lithium iron phosphate to the sodium phosphate being 15:1, 236.64g of lithium iron phosphate powder and 390mL of 4% sodium phosphate solution are weighed and added into a pressure reaction kettle, the reaction kettle is heated to 220 ℃ after being well sealed, the reaction is continued for 5 hours, the container is cooled to room temperature, and the operation is repeated for 3 times. 1577.6g of purified water was added thereto for washing for 3 hours.
According to measurement, the lithium ion diffusion channel of the lithium iron phosphate positive electrode material prepared in the embodiment is expanded, and the diffusion rate of lithium ions is improved. The lithium iron phosphate anode material prepared in the embodiment is used as an anode, super-P is used as a conductive agent, PVDF is used as a binder to prepare an electrode slice, and metal lithium is used as a cathode to assemble a button cell for electrochemical performance test. The test result shows that the first gram capacity of the positive electrode material is 162.2mAh/g, the theoretical gram capacity is 170mAh/g, the 1C discharge gram capacity is 159.3mAh/g, and the 2C discharge gram capacity is 154.0mAh/g. Therefore, the lithium iron phosphate anode material prepared by the embodiment has improved rate discharge performance.
Example 3
The embodiment provides a LiFePO with wide channel 4 The following operations are performed:
according to the molar mass ratio of the lithium iron phosphate to the sodium phosphate being 10:1, 157.76g of lithium iron phosphate powder and 220mL of 7% sodium phosphate solution are weighed and added into a pressure reaction kettle, the reaction kettle is heated to 260 ℃ after being well sealed, the container is cooled to room temperature after continuous reaction for 8 hours, and the operation is repeated for 4 times. 6310.4g of purified water was added thereto for washing for 4 hours.
According to measurement, the lithium ion diffusion channel of the lithium iron phosphate positive electrode material prepared in the embodiment is expanded, and the diffusion rate of lithium ions is improved. The lithium iron phosphate anode material prepared in the embodiment is used as an anode, super-P is used as a conductive agent, PVDF is used as a binder to prepare an electrode slice, and metal lithium is used as a cathode to assemble a button cell for electrochemical performance test. The test result shows that the first gram capacity of the positive electrode material is 160.5mAh/g, the theoretical gram capacity is 170mAh/g, the 1C discharge gram capacity is 154.6mAh/g, and the 2C discharge gram capacity is 142.7mAh/g. Therefore, the lithium iron phosphate anode material prepared by the embodiment has improved rate discharge performance.
Example 4
The embodiment provides a LiFePO with wide channel 4 The following operations are performed:
according to the molar mass ratio of the lithium iron phosphate to the sodium phosphate being 20:1, 157.76g of lithium iron phosphate powder and 73.8mL of 10% sodium phosphate solution are weighed and added into a pressure reaction kettle, the reaction kettle is heated to 300 ℃ after being well sealed, the reaction is continued for 10 hours, the container is cooled to room temperature, and the operation is repeated for 5 times. 7888g of purified water was added thereto for washing for 5 hours.
According to measurement, the lithium ion diffusion channel of the lithium iron phosphate positive electrode material prepared in the embodiment is expanded, and the diffusion rate of lithium ions is improved. The lithium iron phosphate anode material prepared in the embodiment is used as an anode, super-P is used as a conductive agent, PVDF is used as a binder to prepare an electrode slice, and metal lithium is used as a cathode to assemble a button cell for electrochemical performance test. The test result shows that the first gram capacity of the positive electrode material is 160.9mAh/g, the theoretical gram capacity is 170mAh/g, the 1C discharge gram capacity is 155.0mAh/g, and the 2C discharge gram capacity is 144.5mAh/g. Therefore, the lithium iron phosphate anode material prepared by the embodiment has improved rate discharge performance.
< test example >
The cell parameters of the XRD test of the lithium iron phosphate prepared in example 1 are shown in table 1 below.
TABLE 1 comparison of lithium iron phosphate unit cell parameters before and after the treatment of the process
From the results of table 1, it can be seen that the unit cell parameters are significantly increased, indicating that sodium ions have entered the lattice and enlarged the lithium ion diffusion channel.
The discharge performance of the lithium iron phosphate material prepared in example 1 was measured, and the results are shown in fig. 1 and table 2.
Specific capacities of different discharge rates of wide-channel lithium iron phosphate button cells prepared in Table 2
Compared with the prior art, the wide-channel olivine-structured lithium iron phosphate has more excellent discharge rate performance.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The wide-channel lithium iron phosphate is characterized in that sodium ions enter the pore canal of the lithium iron phosphate.
2. The wide-channel lithium iron phosphate of claim 1, wherein the sodium ions and lithium iron phosphate are heat treated at least once.
3. The wide-channel lithium iron phosphate according to claim 2, wherein the number of heating is 3-5, and the container is a pressure reactor.
4. A wide channel lithium iron phosphate according to claim 2 or 3, wherein the heating is to 180-300 ℃ for 3-10 hours.
5. The wide-channel lithium iron phosphate of claim 4, wherein the heating is to 180-220 ℃ for 3-5 hours.
6. The wide channel lithium iron phosphate of claim 1 or 2, wherein the medium material for sodium ions is a soluble sodium salt.
7. The wide-channel lithium iron phosphate of claim 6, wherein the sodium salt is sodium phosphate.
8. A method for preparing the wide-channel lithium iron phosphate according to any one of claims 1 to 7, comprising the steps of:
and (3) blending the lithium iron phosphate and the sodium ion medium raw material solution, and carrying out pressure treatment and post-treatment on the obtained finished product.
9. The method for preparing wide-channel lithium iron phosphate according to claim 8, wherein the molar mass ratio of the lithium iron phosphate to the sodium ion medium raw material is 10-20:1; and/or the mass concentration of the sodium ion medium raw material solution is 1-10%.
10. The method for preparing wide-channel lithium iron phosphate according to claim 8 or 9, wherein the post-treatment comprises washing and filtering; the mass ratio of the finished product to the washing water is controlled to be 1:10-50 in the washing process.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120058039A1 (en) * | 2010-03-02 | 2012-03-08 | Guiqing Huang | HIGH PERFORMANCE CATHODE MATERIAL LiFePO4, ITS PRECURSORS AND METHODS OF MAKING THEREOF |
| US20120328947A1 (en) * | 2011-06-22 | 2012-12-27 | Lih-Hsin Chou | LiFePO4 FLAKES FOR Li-ION BATTERY AND METHOD FOR MANUFACTURING THE SAME |
| CN104009228A (en) * | 2014-05-21 | 2014-08-27 | 成都新柯力化工科技有限公司 | Method for preparing special diamond structure lithium iron phosphate for secondary lithium battery |
| CN106450332A (en) * | 2016-10-28 | 2017-02-22 | 广东电网有限责任公司电力科学研究院 | Method for preparing lithium ion battery material |
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- 2023-04-28 CN CN202310479864.5A patent/CN116462175B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120058039A1 (en) * | 2010-03-02 | 2012-03-08 | Guiqing Huang | HIGH PERFORMANCE CATHODE MATERIAL LiFePO4, ITS PRECURSORS AND METHODS OF MAKING THEREOF |
| US20120328947A1 (en) * | 2011-06-22 | 2012-12-27 | Lih-Hsin Chou | LiFePO4 FLAKES FOR Li-ION BATTERY AND METHOD FOR MANUFACTURING THE SAME |
| CN104009228A (en) * | 2014-05-21 | 2014-08-27 | 成都新柯力化工科技有限公司 | Method for preparing special diamond structure lithium iron phosphate for secondary lithium battery |
| CN106450332A (en) * | 2016-10-28 | 2017-02-22 | 广东电网有限责任公司电力科学研究院 | Method for preparing lithium ion battery material |
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