CN111170294A - Preparation method of low-cost lithium iron phosphate composite material - Google Patents
Preparation method of low-cost lithium iron phosphate composite material Download PDFInfo
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- CN111170294A CN111170294A CN202010060737.8A CN202010060737A CN111170294A CN 111170294 A CN111170294 A CN 111170294A CN 202010060737 A CN202010060737 A CN 202010060737A CN 111170294 A CN111170294 A CN 111170294A
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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
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
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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
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method of a low-cost lithium iron phosphate composite material, which comprises the steps of adding a lithium source, a phosphorus source, an iron source and a manganese source into an organic carbon source, mixing, carrying out titanium doping and carbon coating, synthesizing a lithium iron phosphate composite material precursor doped with lithium manganate through microwave heating, reducing active points of the composite material by adopting gas surface modification, and improving the first efficiency of the material. According to the lithium iron phosphate composite material prepared by the invention, due to the adoption of microwave heating, the energy consumption is reduced, the efficiency is improved, the carbon source is an asphalt material, the cost is low, the source is wide, and the like, and meanwhile, the lithium manganate with low cost is doped, so that on one hand, the voltage platform of the battery is improved, the energy density is improved, and on the other hand, the lithium manganate with low cost can reduce the cost of the material.
Description
Technical Field
The invention belongs to the field of lithium ion battery material preparation, and particularly relates to a low-cost lithium iron phosphate composite material and a preparation process thereof.
Background
The lithium iron phosphate battery has the advantages of low cost, high safety performance, wide material source, long cycle life and the like, and is widely applied to the fields of passenger cars, energy storage and the like. At present, lithium iron phosphate is prepared by mixing iron phosphate or ferric oxide and a lithium source, the mixture is added into organic carbon sources such as glucose and the like for carbon coating, and high-temperature sintering is carried out in an inert atmosphere, so that the sintering period is long, the power consumption is high, the cost of the carbon source is high, the price of lithium salt in the international market is stable and transparent, the price of the lithium iron phosphate is difficult to obviously reduce, and how to effectively reduce the cost of the lithium iron phosphate becomes a key factor for improving the market competitiveness of the future power battery. The lithium manganate material has the advantages of low price, stable market and high voltage platform, but has deviation of cycle performance, for example, if the lithium manganate material is mixed or synthesized with long-life lithium iron phosphate, the characteristics of long service life of the lithium iron phosphate can be exerted on one hand, the characteristics of low price and high energy density of the lithium manganate are exerted on the other hand, the synergistic effect between the lithium manganate material and the lithium iron phosphate is exerted, the energy density of the lithium manganate is improved, the cost is reduced, the energy density of the battery is also considered, meanwhile, the microwave synthesis method is adopted to improve the synthesis efficiency, the energy consumption is reduced, and the comprehensive cost of the.
Disclosure of Invention
In order to reduce the cost of lithium iron phosphate, the invention dopes lithium manganate with low price in the lithium iron phosphate, adopts a low-cost asphalt carbon source, and utilizes the microwave synthesis technology to improve the efficiency, reduce the energy consumption and reduce the cost of the lithium iron phosphate.
The technical scheme of the invention is realized by the following modes: a preparation method of a low-cost lithium iron phosphate composite material is characterized by comprising the following steps by mass:
1) preparing a precursor material A; adding 2.4-11.1g of lithium source, 11.5-13.2g of phosphorus source, 19.0g of iron source and 1.73-8.65g of manganese source into 500ml of deionized water, uniformly mixing by a ball mill, and spray-drying to obtain a precursor material A;
wherein the lithium source is one of lithium carbonate and lithium hydroxide;
the phosphorus source is one or a mixture of diammonium hydrogen phosphate and ammonium dihydrogen phosphate;
the iron source is ferric acetate; the manganese source is manganese acetate;
molar ratio, lithium source: a phosphorus source: an iron source: manganese source = (1-2): 1:1: (0.1 to 0.6);
2) preparing a precursor material B; adding 100g of precursor material A, 1-5g of dispersing agent and 1-5g of additive into 200-300ml of coating agent solution with the concentration of 0.5-2%, uniformly mixing, ball-milling, and heating under the microwave condition: the power is 2000W, and the time is 30min, so that a precursor material B is obtained;
wherein the coating agent is a modified asphalt material;
the dispersant is one of calcium alkyl benzene sulfonate and polyvinylpyrrolidone;
the additive is one of tetrabutyl titanate, diisopropoxy titanium dichloride and 2-ethylhexyl titanium oxide;
3) and transferring the precursor material B into a tubular furnace, and introducing mixed gas to carry out surface modification on the precursor material B to obtain the lithium iron phosphate composite material.
The mixed gas is a mixed gas of inert gas and hydrogen, and the volume ratio (1-10): 1;
the modified asphalt material comprises: crushing the low-temperature asphalt, adding a sodium carbonate pore-forming agent, a terephthalaldehyde crosslinking agent and a ferric trichloride oxidizing agent, uniformly mixing, heating to 200-350 ℃, introducing ammonia gas for nitriding, and finally obtaining the nitrogen-containing crosslinked asphalt.
The mass ratio is as follows: sodium carbonate: terephthalaldehyde: ferric trichloride =100 (0.5-2), (2-6), (1-5).
The invention has the beneficial effects that: 1. the modified asphalt has the characteristics of high molecular weight, high conductivity, high porosity and the like, and is coated on the surface of lithium iron phosphate or lithium manganate to have the characteristics of strong binding force, strong liquid absorption capacity and the like, so that the defects of poor cycle performance and the like of the lithium manganate are overcome, and meanwhile, the modified asphalt can form a network structure, a network frame is formed between materials, and the cycle performance of the modified asphalt is improved. Meanwhile, compared with carbon materials such as glucose and the like, the asphalt material has the advantages of wide sources, lower cost and the like. 2. By adopting the microwave heating synthesis technology, the manufacturing cost of the material can be reduced by utilizing the advantages of high microwave heating speed, low energy consumption and the like, and the consistency of the material is ensured by combining the continuous stirring in the heating process in the preparation process. 3. Titanium-containing additives such as tetrabutyl titanate and the like are doped in the modified asphalt, the multiplying power charge and discharge and the low-temperature performance of the material can be improved by utilizing the advantages of stable structure, large interlayer spacing and the like of a titanide, the liquid absorption and retention capacity of the material is improved by utilizing a porous structure left after sodium carbonate carbonization, and the cycle performance of the material is improved.
Drawings
Fig. 1 is an SEM image of the lithium iron phosphate composite prepared in example 1.
Detailed Description
Preparing modified asphalt: after 100g of low-temperature asphalt (the softening point is 100 ℃), 1g of sodium carbonate, 4g of terephthalaldehyde crosslinking agent and 3g of ferric trichloride oxidant are added and uniformly mixed, the temperature is raised to 300 ℃ in the argon atmosphere, the temperature is kept for 2 hours, then the argon introduction is stopped, the ammonia introduction is changed, and finally the nitrogen-containing crosslinked asphalt is obtained.
Example 1:
1. preparing a precursor material A; adding 11.1g of lithium carbonate (0.15 mol), 13.2g of diammonium phosphate (0.1 mol), 19.0g of iron acetate (0.1 mol) and 8.65g of manganese acetate (0.05 mol) into 500ml of deionized water, uniformly mixing by a ball mill, and performing spray drying to obtain a precursor material A;
2. adding 100g of precursor material A, 3g of calcium alkyl benzene sulfonate and 3g of tetrabutyl titanate into 300ml of 1% pitch carbon tetrachloride solution, uniformly mixing, ball-milling, and heating under the microwave condition (power 2000W, time 30 min) to obtain precursor material B;
3. and transferring the precursor material B into a tube furnace, introducing mixed gas (argon gas: hydrogen =5:1, flow rate is 10 mL/min), and carrying out surface modification for 120min to finally obtain the lithium iron phosphate composite material.
Example 2:
1. preparing a precursor material A;
adding 2.4g of lithium hydroxide (0.10 mol), 11.5g of ammonium dihydrogen phosphate (0.1 mol), 19.0g of iron acetate (0.1 mol) and 1.73g of manganese acetate (0.01 mol) into 500ml of deionized water, uniformly mixing by a ball mill, and carrying out spray drying to obtain a precursor material A;
2. adding 100g of precursor material A, 1g of polyvinylpyrrolidone and 1g of diisopropoxy titanium dichloride into 200ml of 0.5% pitch carbon tetrachloride solution, uniformly mixing, carrying out ball milling, and heating under the microwave condition (power 2000W, time 30 min) to obtain precursor material B;
3. and transferring the precursor material B into a tube furnace, introducing mixed gas (argon gas: hydrogen =10:1, flow rate is 10 mL/min), and carrying out surface modification for 120min to finally obtain the lithium iron phosphate composite material.
Example 3:
1. preparing a precursor material A;
adding 7.4g of lithium carbonate (0.15 mol), 11.5g of ammonium dihydrogen phosphate (0.1 mol), 19.0g of iron acetate (0.1 mol) and 10.38g of manganese acetate (0.06 mol) into 500ml of deionized water, uniformly mixing by a ball mill, and performing spray drying to obtain a precursor material A;
2. adding 100g of precursor material A, 5g of polyvinylpyrrolidone and 5g of calcium alkyl benzene sulfonate into 250ml of asphalt carbon tetrachloride solution with the concentration of 2%, uniformly mixing, carrying out ball milling, and heating under the microwave condition (the power is 2000W, the time is 30 min) to obtain precursor material B;
3. and transferring the precursor material B into a tube furnace, introducing mixed gas (argon gas: hydrogen =1:1, flow rate is 10 mL/min), and carrying out surface modification for 120min to finally obtain the lithium iron phosphate composite material.
Comparative example:
a commercially mature lithium iron phosphate composite material (model N2, model No. of Jiangsu Leneng battery material Co., Ltd.) coated with carbonized glucose was used.
1) SEM electron microscope test
As can be seen from FIG. 1, the lithium iron phosphate composite material prepared by the example is spherical-like, has uniform size distribution, and has a particle size of (2-8) μm.
2) Physical and chemical properties and button cell testing thereof
2.0000g of the lithium iron phosphate composite powder of the positive electrode active material prepared in the examples 1 to 3 and the comparative example, 0.1111g of conductive carbon black, and 0.1111g of conductive carbon black were weighed in a mass ratio of 0.9: 0.05, respectively1111g of PVDF were mixed, and then 2.5g of NMP (N-methylpyrrolidone) as an organic solvent was added thereto and mixed well. Coating a film with the thickness of 140 micrometers on an aluminum foil, drying the film for 2 hours at 120 ℃ in vacuum, beating the film into a wafer with the thickness of 5mm by using a puncher, tabletting the wafer by using a tabletting machine under the pressure of 10MPa, keeping the temperature for 12 hours at 120 ℃ in vacuum, and weighing the weight of the positive plate. The button cell is assembled in a glove box protected by argon, a metal lithium sheet is taken as a negative electrode, an electrolyte is EC (ethylene carbonate), DMC ((1, 2-dimethyl carbonate) solvent and electrolyte LiPF (lithium ion plasma) with the volume ratio of 1:16And the diaphragm is a Celgard2400 microporous polyethylene film. The assembled cell was tested for electrical performance on a blue tester. And (3) charging/discharging at a constant current of 0.2C within a voltage range of 2.5V-4.2V, testing the specific capacity and the liquid absorption and retention capacity of the pole piece, and preparing button cells A1, A2, A3 and B1 as shown in Table 1.
TABLE 1 comparison of test results of test for test of test and comparative test
As can be seen from table 1, the discharge capacity of the lithium iron phosphate material prepared in the example is substantially equivalent to that of the comparative sample, and the first efficiency is significantly higher than that of the comparative sample, because the asphalt material modified on the surface of the lithium iron phosphate has high electronic conductivity, the gram capacity and the first efficiency of the material are improved, and meanwhile, the titanium-doped material has a stable structure, and the defect degree is reduced through gas surface modification, so that the first efficiency of the material is improved.
TABLE 2 comparison of the liquid absorption capacities of the different materials
| Imbibition speed (mL/min) | Liquid retention rate: (24h electrolyte volume/0 h electrolyte volume) | |
| Example 1 | 7.2 | 92.3% |
| Example 2 | 6.4 | 91.2% |
| Example 3 | 6.2 | 90.1% |
| Comparative example | 3.5 | 84.7% |
As can be seen from table 2, the liquid absorption and retention capacities of the electrode sheets of the materials prepared in examples 1 to 3 are significantly higher than those of the comparative examples, because the carbonized carbon material of the asphalt coated on the surface of the lithium iron phosphate has the characteristics of high porosity and large specific surface area, thereby improving the liquid absorption and retention capacities of the electrode sheets.
3) Testing the soft package battery:
respectively taking the lithium iron phosphate prepared in the embodiment 1, the embodiment 2, the embodiment 3 and the comparative example as a positive electrode material, preparing a positive electrode piece, taking artificial graphite as a negative electrode material, and adopting LiPF6And preparing 5Ah soft package batteries C1, C2, C3 and D1 by using/EC + DEC (volume ratio of 1: 1) as an electrolyte and Celgard2400 membrane as a diaphragm, and testing the rate capability and the cycle performance of the materials.
Cycle performance test parameters: charge-discharge multiplying power: 1.0C/1.0C; voltage range: 2.5V-4.2V; temperature: 25 +/-3 ℃;
the method for testing the rate capability comprises the following steps: 0.5C charged, 0.5C, 5C, 10C discharged; voltage range: 2.5V-4.2V; temperature: 25 +/-3 ℃;
TABLE 3 comparison of cycling/rate Performance of examples and comparative examples
As can be seen from table 3, the carbon material coated on the surface of the lithium iron phosphate is formed by carbonizing the pitch, and is doped with the characteristics of high conductivity, stable structure and the like of titanium dioxide, so that the multiplying power and the cycle performance of the material are improved.
Claims (5)
1. A preparation method of a low-cost lithium iron phosphate composite material is characterized by comprising the following steps by mass:
1) preparing a precursor material A; adding 2.4-11.1g of lithium source, 11.5-13.2g of phosphorus source, 19.0g of iron source and 1.73-8.65g of manganese source into 500ml of deionized water, uniformly mixing by a ball mill, and spray-drying to obtain a precursor material A;
2) preparing a precursor material B; adding 100g of precursor material A, 1-5g of dispersing agent and 1-5g of additive into 200-300ml of coating agent solution with the concentration of 0.5-2%, uniformly mixing, ball-milling, and heating under the microwave condition: the power is 2000W, and the time is 30min, so that a precursor material B is obtained;
and transferring the precursor material B into a tubular furnace, and introducing mixed gas to carry out surface modification on the precursor material B to obtain the lithium iron phosphate composite material.
2. The method of claim 1, wherein the method comprises the steps of: the lithium source in the step 1) is one of lithium carbonate and lithium hydroxide;
the phosphorus source is one or a mixture of diammonium hydrogen phosphate and ammonium dihydrogen phosphate;
the iron source is ferric acetate; the manganese source is manganese acetate;
molar ratio, lithium source: a phosphorus source: an iron source: the manganese source = 1-2: 1:1: 0.1 to 0.6.
3. The method of claim 1, wherein the method comprises the steps of: the coating agent in the step 2) is a modified asphalt material;
the dispersant is one of calcium alkyl benzene sulfonate and polyvinylpyrrolidone;
the additive is one of tetrabutyl titanate, diisopropoxy titanium dichloride and 2-ethylhexyl titanium oxide.
4. The method of claim 1, wherein the method comprises the steps of: the modified asphalt material in the step 3) is as follows: crushing low-temperature asphalt, adding a sodium carbonate pore-forming agent, a terephthalaldehyde crosslinking agent and a ferric trichloride oxidant, uniformly mixing, heating to 200-350 ℃, introducing ammonia gas for nitriding, and finally obtaining the nitrogen-containing crosslinked asphalt: mass ratio, low-temperature asphalt: sodium carbonate: terephthalaldehyde: ferric trichloride =100: 0.5-2: 2-6: 1-5.
5. The method of claim 1, wherein the method comprises the steps of: the mixed gas in the step 3) is a mixed gas of inert gas and hydrogen, and the volume ratio is 1-10: 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113054195A (en) * | 2021-03-16 | 2021-06-29 | 河北九丛科技有限公司 | Post-treatment method of phosphate anode material |
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| CN102074689A (en) * | 2010-12-23 | 2011-05-25 | 天津巴莫科技股份有限公司 | Method for preparing lithium iron phosphate composite material |
| CN105489864A (en) * | 2016-01-13 | 2016-04-13 | 李震祺 | Titanium sub-oxide coated and modified lithium iron phosphate composite material and preparation method thereof |
| CN107845791A (en) * | 2017-10-17 | 2018-03-27 | 合肥国轩高科动力能源有限公司 | Preparation method of double-layer asphalt carbon-coated lithium iron phosphate cathode material |
| CN108899511A (en) * | 2018-07-03 | 2018-11-27 | 江苏乐能电池股份有限公司 | A kind of LiFePO4/lithium metaaluminate composite positive pole and preparation method thereof |
| CN109103433A (en) * | 2018-08-22 | 2018-12-28 | 江苏元景锂粉工业有限公司 | A kind of nitrogen mixes carbon-coated lithium iron phosphate composite and preparation method thereof |
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- 2020-01-19 CN CN202010060737.8A patent/CN111170294A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102074689A (en) * | 2010-12-23 | 2011-05-25 | 天津巴莫科技股份有限公司 | Method for preparing lithium iron phosphate composite material |
| CN105489864A (en) * | 2016-01-13 | 2016-04-13 | 李震祺 | Titanium sub-oxide coated and modified lithium iron phosphate composite material and preparation method thereof |
| CN107845791A (en) * | 2017-10-17 | 2018-03-27 | 合肥国轩高科动力能源有限公司 | Preparation method of double-layer asphalt carbon-coated lithium iron phosphate cathode material |
| CN108899511A (en) * | 2018-07-03 | 2018-11-27 | 江苏乐能电池股份有限公司 | A kind of LiFePO4/lithium metaaluminate composite positive pole and preparation method thereof |
| CN109103433A (en) * | 2018-08-22 | 2018-12-28 | 江苏元景锂粉工业有限公司 | A kind of nitrogen mixes carbon-coated lithium iron phosphate composite and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113054195A (en) * | 2021-03-16 | 2021-06-29 | 河北九丛科技有限公司 | Post-treatment method of phosphate anode material |
| CN113054195B (en) * | 2021-03-16 | 2022-05-03 | 河北九丛科技有限公司 | Post-treatment method of phosphate anode material |
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