CN106410140A - High-capacity LiFePO4/C positive plate and preparation method thereof - Google Patents
High-capacity LiFePO4/C positive plate and preparation method thereof Download PDFInfo
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- CN106410140A CN106410140A CN201610911811.6A CN201610911811A CN106410140A CN 106410140 A CN106410140 A CN 106410140A CN 201610911811 A CN201610911811 A CN 201610911811A CN 106410140 A CN106410140 A CN 106410140A
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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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- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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 high-capacity LiFePO4/C positive plate and a preparation method thereof. The preparation method comprises the following steps: (1) preparing a mixture from a lithium source, an iron source, a phosphate radical source, an organic carbon source and a super conductive carbon black; (2) under the existence of protective gas, performing ball grinding, drying and tabletting on the mixture in isopropyl alcohol, and then performing thermal treatment under a microwave condition at the temperature of 600 to 900 DEG C to prepare the high-capacity LiFePO4/C positive plate, wherein based on 1 mol of lithium elements in the lithium source, the content of iron elements in the iron source is 0.95 to 1.05 mol, the content of phosphate radicals in the phosphate radical source is 0.95 to 1.05 mol, and the thickness of a sheet formed by tabletting is 0.45 to 0.55 cm. The high-capacity LiFePO4/C positive plate prepared by the method is excellent in conductivity, diffusion speed of lithium ions, multiplying power, gram volume and charge-discharge cycle performance; meanwhile, the method is simple in procedure and convenient to operate.
Description
Technical field
The present invention relates to positive plate, in particular it relates to high power capacity LiFePO4/ C positive plate and preparation method thereof.
Background technology
Iron phosphate lithium positive pole piece has higher theoretical specific capacity, good cycle life, relatively high and stable discharge and recharge
Platform, have the advantages that simultaneously raw material sources enrich, advantage of lower cost, have a safety feature, nontoxic, thus LiFePO4?
Through becoming the focus of new forms of energy research field.
But LiFePO4Electronic conductivity (10-9-10-10) and lithium ion diffusion rate (10 S/cm-14-10-16m2/s)
Relatively low, high rate performance is also to be further improved；And the industrialized production of current LiFePO4 mainly adopts high temperature solid
Xiang Fa, this method long the production cycle, energy consumption are big, thus leading to the production cost of LiFePO4 to remain high.Above reason is led
Its large-scale application is caused to receive certain restriction.
Content of the invention
It is an object of the invention to provide a kind of high power capacity LiFePO4/ C positive plate and preparation method thereof, by party's legal system
The high power capacity LiFePO obtaining4/ C positive plate has excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and fills
Discharge cycles performance, the method operation is simple simultaneously, be easy to operation.
To achieve these goals, the invention provides a kind of the invention provides high power capacity LiFePO4/ C positive plate
Preparation method, including：
1) by lithium source, source of iron, phosphoric acid root, organic carbon source and superconductive carbon black so that mixture is obtained；
2) in the presence of shielding gas, mixture is carried out ball milling, drying, tabletting in isopropanol, then in microwave
Under the conditions of carry out at 600-900 DEG C heat treatment be obtained high power capacity LiFePO4/ C positive plate；
Wherein, on the basis of the elemental lithium of 1mol in lithium source, in source of iron, the content of ferrum element is 0.95-1.05mol, phosphoric acid
The content of the phosphate radical in root is 0.95-1.05mol, and the thickness of the sheet material being formed after tabletting is 0.45-0.55cm.
Present invention also offers a kind of high power capacity LiFePO4The preparation method of/C positive plate, this high power capacity LiFePO4/ C is just
Pole piece is prepared by above-mentioned preparation method.
By technique scheme, the present invention prepares high power capacity LiFePO by microwave method4/ C positive pole platelet
Body structural integrity, thing are mutually uniform (grain shape is close to spherical, smooth surface), double carbon source (superconductive carbon black and organic carbons
Source) surface modification not only increase the electric conductivity of material, be also beneficial to strengthen the microwave absorption capacity of starting material, make reaction
System thermally equivalent, thus compared with can get under low energy consumption, crystal structure is complete, thing mutually uniform high power capacity LiFePO4/ C is just
Pole piece.The high power capacity LiFePO of the method preparation4/ C positive plate has higher electrical conductivity and the diffusion rate of lithium ion, thus
So that the multiplying power of material and charge-discharge performance is improved, improve gram volume simultaneously.Meanwhile, this preparation method not only has
Have the advantages that heat time heating time is short, material is heated evenly, efficient energy-saving, reached reduces cost and improved product chemical property
Purpose.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of description, with following tool
Body embodiment is used for explaining the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is high power capacity LiFePO in embodiment 1 in detection example 14The SEM figure of/C positive plate；
Fig. 2 is high power capacity LiFePO in embodiment 2 in detection example 14The SEM figure of/C positive plate；
Fig. 3 is high power capacity LiFePO in embodiment 3 in detection example 14The SEM figure of/C positive plate；
Fig. 4 is conventional LiFePO in detection example 14The SEM figure of positive plate.
Specific embodiment
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that it is described herein concrete
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of high power capacity LiFePO4The preparation method of/C positive plate, including：
1) by lithium source, source of iron, phosphoric acid root, organic carbon source and superconductive carbon black so that mixture is obtained；
2) in the presence of shielding gas, mixture is carried out ball milling, drying, tabletting in isopropanol, then in microwave
Under the conditions of carry out at 600-900 DEG C heat treatment be obtained high power capacity LiFePO4/ C positive plate；
Wherein, on the basis of the elemental lithium of 1mol in lithium source, in source of iron, the content of ferrum element is 0.95-1.05mol, phosphoric acid
The content of the phosphate radical in root is 0.95-1.05mol, and the thickness of the sheet material being formed after tabletting is 0.45-0.55cm.
In the present invention, the consumption of organic carbon source and superconductive carbon black can select in wide scope, but in order to
Make prepared high power capacity LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume
And charge-discharge performance is it is preferable that on the basis of the gross weight of mixture, the content of organic carbon source is 5-10 weight %,
The content of superconductive carbon black is 0.5-2 weight %.
Meanwhile, in the present invention, the time of heat treatment can select in wide scope, but in order that the Gao Rong being obtained
Amount LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and discharge and recharge and follows
Ring performance is it is preferable that the time of heat treatment is 30-90min.
In the present invention, the concrete species of lithium source can select in wide scope, but in order that the high power capacity being obtained
LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and charge and discharge cycles
Performance is it is preferable that lithium source is selected from one or more of Lithium hydrate, lithium carbonate, Quilonorm (SKB).
In the present invention, the concrete species of source of iron can select in wide scope, but in order that the high power capacity being obtained
LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and charge and discharge cycles
Performance is it is preferable that source of iron is ferrous sulfate and/or Ferrox..
In the present invention, the concrete species of phosphoric acid root can select in wide scope, but in order that the height being obtained
Capacity LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and discharge and recharge
Cycle performance is it is preferable that phosphoric acid root is diammonium phosphate and/or ammonium phosphate.
In the present invention, the concrete species of organic carbon source can select in wide scope, but in order that the height being obtained
Capacity LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and discharge and recharge
Cycle performance is it is preferable that organic carbon source refers to one or more of citric acid, glucose, sucrose.
In addition, in the present invention, the actual conditions of ball milling can select in wide scope, but in order that the height being obtained
Capacity LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and discharge and recharge
Cycle performance is it is preferable that ball milling meets following condition：Rotating speed is 250-350r/min, and Ball-milling Time is 2-4h.
Finally, in the present invention, the concrete species of shielding gas can select in wide scope, but in order that be obtained
High power capacity LiFePO4/ C positive plate has more excellent conductivity, the diffusion rate of lithium ion, multiplying power, gram volume and charge and discharge
Electric cycle performance is it is preferable that shielding gas is selected from one or more of argon, helium and nitrogen.
Present invention also offers a kind of high power capacity LiFePO4The preparation method of/C positive plate, this high power capacity LiFePO4/ C is just
Pole piece is prepared by above-mentioned preparation method.
Hereinafter will be described the present invention by embodiment.
Preparation example 1
Conventional LiFePO4The preparation of positive plate：
1) by LiOH, FeSO4And NH4H2PO4With 1:1:1 mixed in molar ratio is uniform；
2) by mixed material with isopropanol for medium in argon atmospher with 300r/min ball milling 3h；
3) it is pressed into the disk of 0.5cm after being dried, be then placed in the corundum crucible in microwave oven, under an argon quickly
It is warming up to 600 DEG C, and sustained response 60min is to be obtained LiFePO4Positive plate.
Embodiment 1
High power capacity LiFePO4The preparation of/C positive plate：
1) by LiOH, FeSO4And NH4H2PO4With 1:1:1 mixed in molar ratio uniformly, and add 10% citric acid and
1% superconductive carbon black is as double carbon sources；
2) mixed material is done medium in argon atmospher with 300r/min ball milling 3h with isopropanol；
3) be pressed into the disk of 0.5cm after being dried, be then placed in the corundum crucible in microwave oven, under an argon in fast
Speed is warming up to 600 DEG C, and sustained response 60min is to be obtained high power capacity LiFePO4/ C positive plate.
Test shows, circulates 100 weeks, result shows under 0.5C discharge-rate：With respect to the LiFePO in preparation example 14
Positive plate, the high power capacity LiFePO in the present embodiment4/ C positive plate capability retention improves more than 15%, and gram volume improves
More than 20mAh.
Embodiment 2：
High power capacity LiFePO4The preparation of/C positive plate：
1) by LiOH, FeSO4And NH4H2PO4With 1:1:1 mixed in molar ratio uniformly, and add 10% citric acid and
1% superconductive carbon black is as double carbon sources；
2) mixed material is done medium in argon atmospher with 200r/min ball milling 4h with isopropanol；
3) it is pressed into the disk of 0.5cm after being dried, be then placed in the corundum crucible in microwave oven, under an argon quickly
It is warming up to 650 DEG C, and sustained response 50min is to be obtained high power capacity LiFePO4/ C positive plate.
Test shows, circulates 100 weeks, result shows under 0.5C discharge-rate：With respect to the LiFePO in preparation example 14
Positive plate, the high power capacity LiFePO in the present embodiment4/ C positive plate capability retention improves more than 15%, and gram volume improves
More than 20mAh.
Embodiment 3：
High power capacity LiFePO4The preparation of/C positive plate：
1) by LiOH, FeSO4And NH4H2PO4With 1:1:1 mixed in molar ratio uniformly, and add 10% citric acid and
1% superconductive carbon black is as double carbon sources；
2) mixed material is done medium in argon atmospher with 200r/min ball milling 5h with isopropanol；
3) it is pressed into the disk of 0.5cm after being dried, be then placed in the corundum crucible in microwave oven, under an argon quickly
It is warming up to 700 DEG C, and sustained response 40min is to be obtained high power capacity LiFePO4/ C positive plate.
Test shows, circulates 100 weeks, result shows under 0.5C discharge-rate：With respect to the LiFePO in preparation example 14
Positive plate, the high power capacity LiFePO in the present embodiment4/ C positive plate capability retention improves more than 15%, and gram volume improves
More than 20mAh.
Embodiment 4：
High power capacity LiFePO4The preparation of/C positive plate：
1) by Li2CO3、FeC2O4·2H2O and NH4H2PO4With 1:2:2 mixed in molar ratio uniformly, and adds 10% Portugal
Grape sugar and 1% superconductive carbon black as double carbon sources；
2) mixed material is done medium in argon atmospher with 200r/min ball milling 4h with isopropanol；
3) it is pressed into the disk of 0.5cm after being dried, be then placed in the corundum crucible in microwave oven, under an argon quickly
It is warming up to 650 DEG C, and sustained response 50min is to be obtained high power capacity LiFePO4/ C positive plate.
Test shows, circulates 100 weeks, result shows under 0.5C discharge-rate：With respect to the LiFePO in preparation example 14
Positive plate, the high power capacity LiFePO in the present embodiment4/ C positive plate capability retention improves more than 15%, and gram volume improves
More than 20mAh.
Embodiment 5：
High power capacity LiFePO4The preparation of/C positive plate：
1) by Li2CO3、FeC2O4·2H2O and NH4H2PO4With 1:2:2 mixed in molar ratio uniformly, and adds 10% Portugal
Grape sugar and 1% superconductive carbon black as double carbon sources；
2) mixed material is done medium in argon atmospher with 200r/min ball milling 5h with isopropanol；
3) it is pressed into the disk of 0.5cm after being dried, be then placed in the corundum crucible in microwave oven, under an argon quickly
It is warming up to 700 DEG C, and sustained response 40min is to be obtained high power capacity LiFePO4/ C positive plate.
Test shows, circulates 100 weeks, result shows under 0.5C discharge-rate：With respect to the LiFePO in preparation example 14
Positive plate, the high power capacity LiFePO in the present embodiment4/ C positive plate capability retention improves more than 15%, and gram volume improves
More than 20mAh.
Detection example 1
Conventional LiFePO is detected by scanning electron microscope4High power capacity LiFePO in positive plate, embodiment 1-34/ C positive plate, knot
As Figure 1-4, wherein, Fig. 1 is high power capacity LiFePO in embodiment 1 to fruit4/ C positive plate, Fig. 2 is high power capacity in embodiment 2
LiFePO4/ C positive plate, Fig. 3 is high power capacity LiFePO in embodiment 34/ C positive plate, Fig. 4 is conventional LiFePO4Positive plate
SEM schemes, the high power capacity LiFePO being provided from Fig. 1-4, the present invention4/ C positive plate grain shape is close to spherical, surface light
Sliding, crystal structure is complete, and thing is mutually uniform.
High power capacity LiFePO in detection embodiment 4-5 in the same manner4In/C positive plate, result and embodiment 1-3
High power capacity LiFePO4The testing result of/C positive plate is consistent.
Detection example 2
High power capacity LiFePO in detection embodiment 1-34The tap density of/C positive plate, conductivity, grain size and carbon
Mass percent (being represented with C (%)) in positive active material, concrete outcome is shown in Table 1；Detect real in the same manner
Apply high power capacity LiFePO in a 4-54/ C positive plate, result and high power capacity LiFePO in embodiment 1-34The detection knot of/C positive plate
Fruit is consistent.
Table 1
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, multiple simple variant can be carried out to technical scheme, this
A little simple variant belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy no longer separately illustrates.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it equally should be considered as content disclosed in this invention.
Claims (10)
1. a kind of high power capacity LiFePO4The preparation method of/C positive plate is it is characterised in that include：
1) by lithium source, source of iron, phosphoric acid root, organic carbon source and superconductive carbon black so that mixture is obtained；
2) in the presence of shielding gas, described mixture is carried out ball milling, drying, tabletting in isopropanol, then in microwave
Under the conditions of carry out at 600-900 DEG C heat treatment be obtained described high power capacity LiFePO4/ C positive plate；
Wherein, on the basis of the elemental lithium of 1mol in lithium source, in described source of iron, the content of ferrum element is 0.95-1.05mol, described
The content of the phosphate radical in phosphoric acid root is 0.95-1.05mol, and the thickness of the sheet material being formed after tabletting is 0.45-0.55cm.
2. preparation method according to claim 1, wherein, on the basis of the gross weight of described mixture, described organic carbon
The content in source is 5-10 weight %, and the content of described superconductive carbon black is 0.5-2 weight %.
3. preparation method according to claim 1 and 2, wherein, the time of described heat treatment is 30-90min.
4. preparation method according to claim 3, wherein, described lithium source is in Lithium hydrate, lithium carbonate, Quilonorm (SKB)
One or more.
5. preparation method according to claim 3, wherein, described source of iron is ferrous sulfate and/or Ferrox..
6. preparation method according to claim 3, wherein, described phosphoric acid root is diammonium phosphate and/or ammonium phosphate.
7. preparation method according to claim 3, wherein, described organic carbon source refer to citric acid, glucose, in sucrose one
Plant or multiple.
8. the preparation method according to any one in claim 4-7, wherein, described ball milling meets following condition：Rotating speed
For 250-350r/min, Ball-milling Time is 2-4h.
9. preparation method according to claim 8, wherein, described shielding gas is selected from one of argon, helium and nitrogen
Or it is multiple.
10. a kind of high power capacity LiFePO4The preparation method of/C positive plate is it is characterised in that described high power capacity LiFePO4/ C positive pole
Piece is prepared by the preparation method described in any one in claim 1-9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108336306A (en) * | 2017-12-28 | 2018-07-27 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of composite ceramics electrode |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821064A (en) * | 2006-03-20 | 2006-08-23 | 清华大学 | Method for preparing high density lithium ferric phosphate by microwave heating |
| CN1911792A (en) * | 2006-08-22 | 2007-02-14 | 南京大学 | Microwave synthesis method for carbon coated iron phosphate of ion battery composite anode material |
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2016
- 2016-10-19 CN CN201610911811.6A patent/CN106410140A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821064A (en) * | 2006-03-20 | 2006-08-23 | 清华大学 | Method for preparing high density lithium ferric phosphate by microwave heating |
| CN1911792A (en) * | 2006-08-22 | 2007-02-14 | 南京大学 | Microwave synthesis method for carbon coated iron phosphate of ion battery composite anode material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108336306A (en) * | 2017-12-28 | 2018-07-27 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of composite ceramics electrode |
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Application publication date: 20170215 |
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