CN110429277A - A kind of preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability - Google Patents
A kind of preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability Download PDFInfo
- Publication number
- CN110429277A CN110429277A CN201910573857.5A CN201910573857A CN110429277A CN 110429277 A CN110429277 A CN 110429277A CN 201910573857 A CN201910573857 A CN 201910573857A CN 110429277 A CN110429277 A CN 110429277A
- Authority
- CN
- China
- Prior art keywords
- dispersion liquid
- iron phosphate
- lithium iron
- lithium
- positive material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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
-
- 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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
-
- 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
- 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
-
- 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
- H01M4/366—Composites as layered products
-
- 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
-
- 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
- H01M4/625—Carbon or graphite
-
- 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 a kind of preparation methods of the lithium iron phosphate positive material of high-pressure solid high rate capability, be related to anode material for lithium-ion batteries technical field, comprising the following steps: according to 100: 4.5: the mass ratio of (0.5~4) takes layered mesoporous graphite phase carbon nitride powder g-C3N4, PVP and glucide, be add to deionized water, disperse, obtain dispersion liquid A；According to FePO4∶g‑C3N4=50: the mass ratio of (0.8~1.5) weighs FePO4, it is added in dispersion liquid A, disperses, obtain dispersion liquid B；According to stoichiometric ratio Fe: Li=1: 1, lithium source is weighed, is added in dispersion liquid B, disperses, obtains dispersion liquid C；Dispersion liquid C is subjected to extra-fine grinding, it is spray-dried, then under protective atmosphere, after pre-burning, sintering, natural cooling to get.The present invention is with g-C3N4Morphological control and modification are carried out in LiFePO4 processing procedure, can increase substantially the compacting and charge-discharge magnification performance of lithium iron phosphate positive material using the dispersion performance that PVP is excellent for stratiform template and primary carbon source.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field more particularly to a kind of phosphorus of high-pressure solid high rate capability
The preparation method of sour iron lithium anode material.
Background technique
In recent years, the influence with fossil energy to earth environment increasingly sharpens, and clean energy resource has been pushed away as substitute
It is wide to use.As the representative of clean energy resource, new energy battery is increasingly becoming the first choice of passenger car, bus and energy storage cause.Phosphorus
Sour lithium iron battery is because its is cheap, and theoretical capacity is higher (about 170mAh/g), stable operating voltage, asepsis environment-protecting, and structure is steady
It is fixed, it has a safety feature, thermal stability is good and the cycle life of overlength and becomes the hot spot that current new energy battery is studied.Just at present
From the point of view of the LiFePO4 product developed, that there is also ionic conductivities is low for the material, electric conductivity is poor, compacted density is low and low
Warm nature can difference the disadvantages of, it is low, processing performance is bad so as to cause energy density the problems such as, it is wide on power battery to limit it
General application.
In view of the above problems, correlative study person is improved by carrying out nanosizing processing and carbon coating to LiFePO 4 material
The high rate performance of material or compacting, still, the overwhelming majority can only all meet single high magnification or high-pressure solid performance, it is difficult to simultaneously
It takes into account and accomplishes high-pressure solid high magnification, and the problems such as there are material carbon coating is uneven, and machining property is poor.How phosphorus is optimized
Sour iron lithium making technology improves compacted density, is current primary study target while making material have both high rate capability.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of LiFePO4s of high-pressure solid high rate capability
The preparation method of positive electrode is with g-C3N4For stratiform template, the uniform stratiform phosphoric acid of carbon coating is obtained by stratiform template
Iron lithium finished product can increase substantially the compacting and charge-discharge magnification performance of material.
A kind of preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability proposed by the present invention, including it is following
Step:
S1, according to 100: 4.5: the mass ratio of (0.5~4) takes layered mesoporous graphite phase carbon nitride powder g-C3N4, polyethylene
Base pyrrolidones PVP and glucide, are add to deionized water, and dispersion obtains dispersion liquid A；
S2, according to FePO4∶g-C3N4=50: the mass ratio of (0.8~1.5) weighs FePO4, it is added in dispersion liquid A,
Dispersion, obtains dispersion liquid B；
S3, according to stoichiometric ratio Fe: Li=1: 1, weigh lithium source, be added in dispersion liquid B, disperse, obtain dispersion liquid C；
S4, dispersion liquid C is subjected to extra-fine grinding, it is spray-dried, ferric lithium phosphate precursor is obtained, presoma is being protected
Under atmosphere, then after pre-burning, sintering, natural cooling obtains high-pressure solid high rate lithium iron phosphate anode material.
Preferably, in S1, layered mesoporous graphite phase carbon nitride powder g-C3N4With a thickness of 90-120nm；Preferably, g-
C3N4Prepare it is as follows: take urea and ammonium sulfate according to the mass ratio of 11.5:1, be dissolved in ultrapure water, prepare solid content be 55%
Solution, the dry 19-24h at 65-80 DEG C, then obtain powder sample through 450-600 DEG C of tube furnace sintering 5-8h, by powder-like
Product carry out ultrasound removing 12h in ultrapure water, obtain layered mesoporous graphite phase carbon nitride powder g-C3N4。
Preferably, in S1, the molecular weight of polyvinylpyrrolidone PVP is 8000-16000；Preferably, glucide is
Glucose, fructose, galactolipin, sucrose, maltose, starch it is any one or more than one.
Preferably, in S1, disperse 30-50min.
Preferably, in S2, disperse 0.5-2h.
Preferably, in S3, lithium source be lithium carbonate, in lithium hydroxide any one or both mixture.
Preferably, in S3, disperse 2-3.5h.
Preferably, in S4, the granularity D50 after dispersion liquid C extra-fine grinding is 300-400nm.
Preferably, in S4, protective atmosphere is high pure nitrogen, high-purity helium, the one or more of high-purity argon gas.
Preferably, in S4, in 330-460 DEG C of pre-burning 3-5h, 680-790 DEG C of sintering 8-14h.
The utility model has the advantages that the invention proposes a kind of preparation sides of the lithium iron phosphate positive material of high-pressure solid high rate capability
Method is with layered mesoporous graphite phase carbon nitride powder g-C3N4For stratiform template, using the dispersion performance that PVP is excellent, by g-C3N4
It is evenly dispersed with glucide and be coated on iron phosphate grains surface, by the control of extra-fine grinding granularity, make close between particle
It being combined together, forms the spherical presoma of intercalation formula in later period drying-granulating, particle compactness is higher, under low-temperature sintering,
LiFePO4 can be grown on the basis of stratiform template forms layer structure, as temperature elapses, g-C3N4Template decomposition and with carbon source
Form is uniformly wrapped in LiFePO4 layer structure, the lithium iron phosphate positive material obtained by the stratiform template, can be with
Increase substantially the compacting and charge-discharge magnification performance of material.
Detailed description of the invention
Fig. 1 is the SEM figure of LiFePO 4 material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of the LiFePO 4 material of comparative example of the present invention preparation.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
(1) urea, ammonium sulfate in mass ratio 11.5: 1 is dissolved in ultrapure water, is configured to 55% solution of solid content, in
Dry 20h obtains dried feed at 70 DEG C, then dried feed is obtained powder sample through 570 DEG C of tube furnace sintering 7h, by powder sample
Ultrasound removing 12h is carried out in ultrapure water, obtains the layered mesoporous graphite phase carbon nitride powder (g-C of 100nm thickness3N4)；
(2) g-C in step (1) is weighed according to mass ratio 100: 4.5: 13N4, relative molecular weight be 10000 PVP and Portugal
Grape sugar is add to deionized water dispersion 40min, obtains dispersion liquid A；
(3) according to FePO4∶g-C3N4=50: 1 mass ratio, weighs FePO4, it is added in the dispersion liquid A in step (2)
Disperse 1h, obtain dispersion liquid B, then stoichiometrically Fe: Li=1: 1, weigh lithium source, is added in dispersion liquid B and disperses 2.5h, score
Dispersion liquid C；
(4) the dispersion liquid C in step (3) is subjected to extra-fine grinding 2h, the granularity D50=380nm after grinding is done by spraying
It is dry, ferric lithium phosphate precursor is obtained, by presoma under protective atmosphere, 420 DEG C of pre-burning 4h, 710 DEG C of sintering 12h, natural cooling
Afterwards, high-pressure solid high rate lithium iron phosphate anode material is obtained.
Fig. 1 is the SEM figure that LiFePO4 is prepared in the present embodiment, it is clear from the figure that with g-C3N4For template system
The LiFePO 4 material obtained is the lamellar structure of distribution uniform in size, and carbon coating is uniform, and material surface does not have agraphitic carbon.
Embodiment 2
(1) urea, ammonium sulfate in mass ratio 11.5: 1 is dissolved in ultrapure water, is configured to 55% solution of solid content, in
Dry 20h obtains dried feed at 70 DEG C, then dried feed is obtained powder sample through 570 DEG C of tube furnace sintering 7h, by powder sample
Ultrasound removing 12h is carried out in ultrapure water, obtains the layered mesoporous graphite phase carbon nitride powder (g-C of 100nm thickness3N4)；
(2) g-C in step (1) is weighed according to mass ratio 100: 4.5: 0.53N4, relative molecular weight be 10000 PVP and
Glucose is add to deionized water dispersion 40min, obtains dispersion liquid A；
(3) according to FePO4∶g-C3N4=50: 1 mass ratio, weighs FePO4, it is added in the dispersion liquid A in step (2)
Disperse 1h, obtain dispersion liquid B, then stoichiometrically Fe: Li=1: 1, weigh lithium source, is added in dispersion liquid B and disperses 2.5h, score
Dispersion liquid C；
(4) the dispersion liquid C in step (3) is subjected to extra-fine grinding 2h, the granularity D50=380nm after grinding is done by spraying
It is dry, ferric lithium phosphate precursor is obtained, by presoma under protective atmosphere, 420 DEG C of pre-burning 4h, 710 DEG C of sintering 12h, natural cooling
Afterwards, high-pressure solid high rate lithium iron phosphate anode material is obtained.
Embodiment 3
(1) urea, ammonium sulfate in mass ratio 11.5: 1 is dissolved in ultrapure water, is configured to 55% solution of solid content, in
Dry 20h obtains dried feed at 70 DEG C, then dried feed is obtained powder sample through 570 DEG C of tube furnace sintering 7h, by powder sample
Ultrasound removing 12h is carried out in ultrapure water, obtains the layered mesoporous graphite phase carbon nitride powder (g-C of 100nm thickness3N4)；
(2) g-C in step (1) is weighed according to mass ratio 100: 4.5: 43N4, relative molecular weight be 10000 PVP and Portugal
Grape sugar is add to deionized water dispersion 40min, obtains dispersion liquid A；
(3) according to FePO4∶g-C3N4=50: 1 mass ratio, weighs FePO4, it is added in the dispersion liquid A in step (2)
Disperse 1h, obtain dispersion liquid B, then stoichiometrically Fe: Li=1: 1, weigh lithium source, is added in dispersion liquid B and disperses 2.5h, score
Dispersion liquid C；
(4) the dispersion liquid C in step (3) is subjected to extra-fine grinding 2h, the granularity D50=380nm after grinding is done by spraying
It is dry, ferric lithium phosphate precursor is obtained, by presoma under protective atmosphere, 420 DEG C of pre-burning 4h, 710 DEG C of sintering 12h, natural cooling
Afterwards, high-pressure solid high rate lithium iron phosphate anode material is obtained.
Embodiment 4
(1) urea, ammonium sulfate in mass ratio 11.5: 1 is dissolved in ultrapure water, is configured to 55% solution of solid content, in
Dry 19h obtains dried feed at 65 DEG C, then dried feed is obtained powder sample through 450 DEG C of tube furnace sintering 5h, by powder sample
Ultrasound removing 12h is carried out in ultrapure water, obtains the layered mesoporous graphite phase carbon nitride powder g-C of 90nm thickness3N4；
(2) g-C in step (1) is weighed according to mass ratio 100: 4.5: 23N4, relative molecular weight be 8000 PVP and Portugal
Grape sugar is add to deionized water dispersion 30min, obtains dispersion liquid A；
(3) according to FePO4∶g-C3N4=50: 0.8 mass ratio, weighs FePO4, the dispersion liquid A that is added in step (2)
Middle dispersion 0.5h, obtains dispersion liquid B, then stoichiometrically Fe: Li=1: 1, weighs lithium source, is added in dispersion liquid B and disperses 2h, obtains
Dispersion liquid C；
(4) the dispersion liquid C in step (3) is subjected to extra-fine grinding 1.5h, the granularity D50=400nm after grinding, through spraying
It is dry, ferric lithium phosphate precursor is obtained, by presoma under protective atmosphere, 330 DEG C of pre-burning 3h, 680 DEG C of sintering 8h, natural cooling
Afterwards, high-pressure solid high rate lithium iron phosphate anode material is obtained.
Embodiment 5
(1) urea, ammonium sulfate in mass ratio 11.5: 1 is dissolved in ultrapure water, is configured to 55% solution of solid content, in
It is dry at 80 DEG C to obtain dried feed for 24 hours, then dried feed is obtained into powder sample through 600 DEG C of tube furnace sintering 8h, by powder sample
Ultrasound removing 12h is carried out in ultrapure water, obtains the layered mesoporous graphite phase carbon nitride powder g-C of 120nm thickness3N4；
(2) g-C in step (1) is weighed according to mass ratio 100: 4.5: 3.53N4, relative molecular weight be 16000 PVP and
Glucose is add to deionized water dispersion 50min, obtains dispersion liquid A；
(3) according to FePO4∶g-C3N4=50: 1.5 mass ratio, weighs FePO4, the dispersion liquid A that is added in step (2)
Middle dispersion 2h, obtains dispersion liquid B, then stoichiometrically Fe: Li=1: 1, weighs lithium source, is added in dispersion liquid B and disperses 3.5h, obtains
Dispersion liquid C；
(4) the dispersion liquid C in step (3) is subjected to extra-fine grinding 3h, the granularity D50=300nm after grinding is done by spraying
It is dry, ferric lithium phosphate precursor is obtained, by presoma under protective atmosphere, 460 DEG C of pre-burning 5h, 790 DEG C of sintering 14h, natural cooling
Afterwards, lithium iron phosphate positive material is obtained.
Comparative example
(1) PVP that glucose and relative molecular weight are 10000 is weighed according to mass ratio 100: 4.5, is added to deionized water
Middle dispersion 40min, obtains dispersion liquid A；
(2) according to FePO4: glucose=50: 1 mass ratio weighs FePO4, it is added in the dispersion liquid A in step (1)
Disperse 1h, obtain dispersion liquid B, then stoichiometrically Fe: Li=1: 1, weigh lithium source, is added in dispersion liquid B and disperses 2.5h, score
Dispersion liquid C；
(3) the dispersion liquid C in step (2) is subjected to extra-fine grinding 2h, the granularity D50=380nm after grinding is done by spraying
It is dry, ferric lithium phosphate precursor is obtained, by presoma under protective atmosphere, 420 DEG C of pre-burning 4h, 710 DEG C of sintering 12h, natural cooling
Afterwards, lithium iron phosphate positive material is obtained.
Fig. 2 show this comparative example prepare LiFePO 4 material correspond to SEM figure, it can be seen from the figure that phosphoric acid obtained
Iron lithium finished product is the hardened irregular structure of size particles, and there are increased number of stomata for particle surface, this is low with its compacted density
There is certain relationship.
To the performances such as the button electricity of the LiFePO 4 material prepared in 1-3 of the embodiment of the present invention and comparative example, compacted density into
Row test, test result are shown in Table 1.
The LiFePO 4 material prepared in 1 embodiment 1-3 of table and comparative example buckles electricity, compacted density data
From table 1 it follows that 0.2C head puts gram volume and is up to 164.9mAh/g, head effect 99%, 1C, 2C in embodiment 1
And corresponding electric discharge gram volume is respectively 152.3mAh/g, 149.1mAh/g and 141.9mAh/g, corresponding pole piece compacting under 3C multiplying power
Density 2.42g/cc.Compared to embodiment 1, glucose dosage is reduced in embodiment 2, material is integrally detained electrical property and is slightly decreased,
Pole piece compaction density is 2.4g/cc, and compacted density is compared with Example 1, in a slight decrease.Increase the use of glucose in embodiment 3
After amount, it is in a slight decrease that material integrally detains electrical property, but first effect still reaches 98.9%, and compacted density is also reduced to 2.37g/cc.It says
Bright excessive carry out carbon coating not necessarily has good castering action to the compaction capacity and button electricity of material.Compared to embodiment 1-
3, the whole button electrical property of the LiFePO 4 material prepared in comparative example is poor, is compacted lower, illustrates good carbon coating method
And material morphology has most important effect to high-pressure solid high rate capability.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability, which is characterized in that including following step
It is rapid:
S1, according to 100: 4.5: the mass ratio of (0.5~4) takes layered mesoporous graphite phase carbon nitride powder g-C3N4, polyvinyl pyrrole
Pyrrolidone PVP and glucide, are add to deionized water, and dispersion obtains dispersion liquid A；
S2, according to FePO4∶g-C3N4=50: the mass ratio of (0.8~1.5) weighs FePO4, it is added in dispersion liquid A, disperses,
Obtain dispersion liquid B；
S3, according to stoichiometric ratio Fe: Li=1: 1, weigh lithium source, be added in dispersion liquid B, disperse, obtain dispersion liquid C；
S4, dispersion liquid C is subjected to extra-fine grinding, it is spray-dried, ferric lithium phosphate precursor is obtained, by presoma in protective atmosphere
Under, then after pre-burning, sintering, natural cooling obtains high-pressure solid high rate lithium iron phosphate anode material.
2. the preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1, feature
It is, in S1, layered mesoporous graphite phase carbon nitride powder g-C3N4With a thickness of 90-120nm；Preferably, g-C3N4Preparation such as
Under: urea and ammonium sulfate are taken according to the mass ratio of 11.5:1, is dissolved in ultrapure water, the solution that solid content is 55% is prepared, in 65-
Dry 19-24h at 80 DEG C, then powder sample is obtained through 450-600 DEG C of tube furnace sintering 5-8h, by powder sample in ultrapure water
Ultrasound removing 12h is carried out, layered mesoporous graphite phase carbon nitride powder g-C is obtained3N4。
3. the preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1 or 2, special
Sign is, in S1, the molecular weight of polyvinylpyrrolidone PVP is 8000-16000；Preferably, glucide be glucose,
Fructose, galactolipin, sucrose, maltose, starch it is any one or more than one.
4. the preparation side of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1-3
Method, which is characterized in that in S1, disperse 30-50min.
5. the preparation side of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1-4
Method, which is characterized in that in S2, disperse 0.5-2h.
6. the preparation side of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1-5
Method, which is characterized in that in S3, lithium source be lithium carbonate, in lithium hydroxide any one or both mixture.
7. the preparation side of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1-6
Method, which is characterized in that in S3, disperse 2-3.5h.
8. the preparation side of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1-7
Method, which is characterized in that in S4, the granularity D50 after dispersion liquid C extra-fine grinding is 300-400nm.
9. the preparation side of the lithium iron phosphate positive material of high-pressure solid high rate capability according to claim 1-8
Method, which is characterized in that in S4, protective atmosphere is high pure nitrogen, high-purity helium, the one or more of high-purity argon gas.
10. the preparation side of the lithium iron phosphate positive material of -9 described in any item high-pressure solid high rate capabilities according to claim 1
Method, which is characterized in that in S4, in 330-460 DEG C of pre-burning 3-5h, 680-790 DEG C of sintering 8-14h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910573857.5A CN110429277B (en) | 2019-06-28 | 2019-06-28 | Preparation method of high-compaction high-rate lithium iron phosphate cathode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910573857.5A CN110429277B (en) | 2019-06-28 | 2019-06-28 | Preparation method of high-compaction high-rate lithium iron phosphate cathode material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110429277A true CN110429277A (en) | 2019-11-08 |
| CN110429277B CN110429277B (en) | 2021-01-29 |
Family
ID=68409886
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910573857.5A Active CN110429277B (en) | 2019-06-28 | 2019-06-28 | Preparation method of high-compaction high-rate lithium iron phosphate cathode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110429277B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114229818A (en) * | 2021-12-23 | 2022-03-25 | 沈阳国科金能科技有限公司 | Preparation method of in-situ doped graphene low-temperature lithium iron phosphate cathode material |
| CN114628637A (en) * | 2021-12-15 | 2022-06-14 | 杭州华宏通信设备有限公司 | Preparation method of high-conductivity lithium iron phosphate positive plate |
| WO2023102584A1 (en) * | 2021-12-10 | 2023-06-15 | Hydrosolid Gmbh | Process for producing nanoflakes from g-c3n4/metal composite material |
| CN114551973B (en) * | 2021-12-24 | 2023-08-15 | 杭州华宏通信设备有限公司 | Low-temperature type long-circulation lithium iron phosphate battery |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130112915A1 (en) * | 2011-11-08 | 2013-05-09 | Gue-Sung Kim | Composite cathode active material, cathode and lithium battery that include the composite cathode active material, and method of preparing the composite cathode active material |
| CN104134801A (en) * | 2014-07-28 | 2014-11-05 | 北京万源工业有限公司 | Carbon nitride and graphene cladded lithium iron phosphate composite anode material and preparation method thereof |
| CN105206809A (en) * | 2015-09-11 | 2015-12-30 | 合肥国轩高科动力能源有限公司 | C3N4-carbon-coated lithium iron phosphate composite anode material and preparation method thereof |
| CN105226274A (en) * | 2015-07-01 | 2016-01-06 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of LiFePO4/graphene composite material of graphene uniform dispersion |
| CN107394152A (en) * | 2017-07-17 | 2017-11-24 | 深圳市贝特瑞纳米科技有限公司 | The spherical composite of the high graphene-based LiFePO4 of conductance, its preparation method and include its lithium ion battery |
| CN109244395A (en) * | 2018-08-28 | 2019-01-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of situ Nitrogen Doping packet carbon lithium iron phosphate positive material |
-
2019
- 2019-06-28 CN CN201910573857.5A patent/CN110429277B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130112915A1 (en) * | 2011-11-08 | 2013-05-09 | Gue-Sung Kim | Composite cathode active material, cathode and lithium battery that include the composite cathode active material, and method of preparing the composite cathode active material |
| CN104134801A (en) * | 2014-07-28 | 2014-11-05 | 北京万源工业有限公司 | Carbon nitride and graphene cladded lithium iron phosphate composite anode material and preparation method thereof |
| CN105226274A (en) * | 2015-07-01 | 2016-01-06 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of LiFePO4/graphene composite material of graphene uniform dispersion |
| CN105206809A (en) * | 2015-09-11 | 2015-12-30 | 合肥国轩高科动力能源有限公司 | C3N4-carbon-coated lithium iron phosphate composite anode material and preparation method thereof |
| CN107394152A (en) * | 2017-07-17 | 2017-11-24 | 深圳市贝特瑞纳米科技有限公司 | The spherical composite of the high graphene-based LiFePO4 of conductance, its preparation method and include its lithium ion battery |
| CN109244395A (en) * | 2018-08-28 | 2019-01-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of situ Nitrogen Doping packet carbon lithium iron phosphate positive material |
Non-Patent Citations (2)
| Title |
|---|
| PEIDONG LI，ET AL.: "(NH4)2SO4-assisted polycondensation of dicyandiamide for porous g-C3N4 with enhanced photocatalytic NO removal", 《RSC ADVANCES》 * |
| 刘嘉星，等: "氮化碳介孔材料的合成、改性及研究进展", 《中国陶瓷》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023102584A1 (en) * | 2021-12-10 | 2023-06-15 | Hydrosolid Gmbh | Process for producing nanoflakes from g-c3n4/metal composite material |
| CN114628637A (en) * | 2021-12-15 | 2022-06-14 | 杭州华宏通信设备有限公司 | Preparation method of high-conductivity lithium iron phosphate positive plate |
| CN114628637B (en) * | 2021-12-15 | 2023-08-04 | 杭州华宏通信设备有限公司 | Preparation method of high-conductivity lithium iron phosphate positive plate |
| CN114229818A (en) * | 2021-12-23 | 2022-03-25 | 沈阳国科金能科技有限公司 | Preparation method of in-situ doped graphene low-temperature lithium iron phosphate cathode material |
| CN114551973B (en) * | 2021-12-24 | 2023-08-15 | 杭州华宏通信设备有限公司 | Low-temperature type long-circulation lithium iron phosphate battery |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110429277B (en) | 2021-01-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110429277A (en) | A kind of preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability | |
| CN101955175B (en) | Industrial preparation method for lithium iron phosphate | |
| CN102034971B (en) | Lithium-ion battery lithium iron phosphate/polypyrrole pyridine composite anode material and preparation method thereof | |
| CN101420034A (en) | Carbon coated granularity controllable spherical lithium ferric phosphate composite positive pole material and preparation method thereof | |
| CN109860572A (en) | The preparation method of the compound carbon-coated nano-scale lithium iron phosphate of three-dimensional net structure | |
| CN102255078A (en) | Coordinated method for preparing nanometer spherical iron phosphate and then using carbon fusion method to prepare nanometer spherical lithium iron phosphate | |
| CN110350198B (en) | Preparation method of sodium phosphate surface modified sodium ion battery positive electrode material | |
| CN111162256A (en) | Mixed polyanion type sodium ion battery positive electrode material and preparation thereof | |
| CN108199011B (en) | Preparation method of lithium titanate negative electrode material | |
| Cheng et al. | Hydrothermal synthesis of LiNi0. 5Mn1. 5O4 sphere and its performance as high-voltage cathode material for lithium ion batteries | |
| CN102583300A (en) | Fluorine and vanadium ion-doped lithium iron phosphate material and preparation method thereof | |
| CN102867957A (en) | Preparation method for spherical mesoporous lithium iron phosphate anode material | |
| CN106935830B (en) | lithium ion battery composite positive electrode material and preparation method and application thereof | |
| CN114665058A (en) | Preparation method of lithium ion battery anode material lithium iron manganese phosphate | |
| CN109616651B (en) | Heteroatom-doped graphene-based vanadium sodium phosphate composite nano material for sodium ion anode material | |
| CN103326010A (en) | Process for preparing nano-silicon-doped composite-lithium-titanate anode materials | |
| KR20230137807A (en) | Method for preparing carbon-coated lithium iron phosphate material from ferrous phosphate | |
| CN102800858A (en) | Preparation method and purpose for iron oxide-based anode material for lithium ion battery | |
| CN104681814B (en) | A kind of anode material for lithium-ion batteries LiFePO with porous star pattern4And preparation method thereof | |
| CN114229818A (en) | Preparation method of in-situ doped graphene low-temperature lithium iron phosphate cathode material | |
| CN100391830C (en) | Method for preparing lithium vanadium phosphoric acid of anode material of lithium ion battery under high pressure | |
| CN102299334A (en) | Carbon coated LiFePO4 porous anode and preparation method thereof | |
| CN101267034A (en) | LiFePO4/CRF nano compound anode material and its meso-pore compound method | |
| CN107681131B (en) | Preparation method of low-cost nano silicon powder and silicon carbon material | |
| CN111099569B (en) | Preparation method of reduced graphene oxide/carbon material coated lithium iron phosphate material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |