CN103367722A - Preparation method of carbon-coated lithium iron phosphate nanometer composite material - Google Patents
Preparation method of carbon-coated lithium iron phosphate nanometer composite material Download PDFInfo
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- CN103367722A CN103367722A CN2013102993851A CN201310299385A CN103367722A CN 103367722 A CN103367722 A CN 103367722A CN 2013102993851 A CN2013102993851 A CN 2013102993851A CN 201310299385 A CN201310299385 A CN 201310299385A CN 103367722 A CN103367722 A CN 103367722A
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Abstract
The invention discloses a preparation method of a carbon-coated lithium iron phosphate nanometer composite material. The method comprises the following steps: preparing an amphiphilic carbon material and ethylene glycol to suspension, adding a lithium source including lithium hydroxide, a phosphorus source including phosphoric acid and a ferrum source including ferrous sulfate into the suspension, stirring to react the ingredients, putting the ingredients in a high temperature reaction kettle to perform a solvent thermal reaction, and putting the ingredients in a carbonization furnace to perform heat treatment to obtain the carbon-coated lithium iron phosphate nanometer composite material with granule size of 30-100 nm. The preparation method disclosed by the invention has the advantages that the synthesis process is simple, the process conditions are easy to control and are free of environmental pollution; the prepared carbon-coated lithium iron phosphate nanometer composite material is good in orientation, few in defects and high in crystallinity and has good large-current charge and discharge performance and stable circulation performance when being used as anode materials of lithium ion batteries.
Description
Technical field
The present invention relates to a kind of preparation method of charcoal coated LiFePO 4 for lithium ion batteries nanocomposite, belong to the anode material for lithium-ion batteries technical field.
Background technology
Anode material for lithium ion battery mainly is the intercalation compounds that lithium and transition metal form, and research and comparison is many LiCoO
2, LiNiO
2, LiMn
2O
4, LiFePO
4Deng.But Co is resource-constrained, and is expensive and toxicity is larger, and environmental pollution is serious; Ni is that synthesis condition is harsh; Mn system is because the Jahn-Teller effect causes cycle performance of lithium ion battery poor.1997, Padhi etc. were with LiFePO
4Introduce lithium ion battery.Because LiFePO
4Theoretical capacity with 170 mAh/g, 3.2～3.5 V (vs. Li
+/ Li) plateau potential, good cyclical stability and fail safe, environmental friendliness, raw material sources are extensive, become the good anode material for lithium-ion batteries of application prospect.But LiFePO
4Electronic conductivity low by (10
-10～10
-9S/cm) and lithium ion diffusion rate slow (1.8 * 10
-14Cm
2/ s), limited LiFePO
4The chemical property of material.The researcher is mainly from nanometer and pattern control at present, and conductive phase is surperficial to be coated, and LiFePO is improved in the aspects such as non-equivalence ion doping
4Chemical property.Wherein nanometer can shorten Li
+The time required from bulk diffusion to electrolyte with electronics, improve Li
+Diffusion rate; The surperficial coating of conductive phase (such as carbon) can improve the transmission of electronics between material interface.
At present more about the research of nano-grade lithium iron phosphate, its Patent CN101944601A prepares the method for even charcoal coated nano-grade lithium iron phosphate, adopt the homogeneous phase crystallisation to make the ferric lithium phosphate precursor that particle diameter is 20～100 nm, carry out fully mixing in the solution with the nanoscale charcoal again, sintering obtains the nano-grade lithium iron phosphate that even charcoal coats.Charcoal coats the coating that belongs to after synthesizing, and has increased preparation section.Patent CN102623701A prepares the method for low form nano lithium iron phosphate material, and first with wet-mixed such as lithium source, source of iron, phosphorus sources, the high energy Ultrafine Grinding is processed, and spray drying is sieved; The processing of secondary high energy Ultrafine Grinding is carried out in presintering again, and spray drying is sieved; Finally by crossing air-flow crushing, twice high-temperature heat treatment obtains the LiFePO 4 material that crystallite dimension is 60～70 nm.Technological process is complicated.
The relative low temperature of solvent heat, equipressure, solution condition are conducive to few defective, are orientated, the perfectly growth of crystal, and product degree of crystallinity is high, and is easy to control the granularity of product crystal, are widely applied in inorganic micro Nano material synthetic.The original position charcoal coats by the obvious refinement particle of steric effect, not only can effectively control pattern and the crystallite dimension of product, avoids LiFePO
4Reuniting generates large particle diameter, thereby shortens Li
+Diffusion length increases Li
+Diffusion rate; Can also improve the electron conduction between the particle, the charge transfer between the variable grain can in time be finished, can realize the even coating to synthetic product.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of charcoal coated LiFePO 4 for lithium ion batteries nanocomposite, this charcoal coated LiFePO 4 for lithium ion batteries nanocomposite has good chemical property, and its method preparation process is simple, environmental friendliness, energy consumption is low.
The present invention is achieved by the following technical solutions, a kind of preparation method of charcoal coated LiFePO 4 for lithium ion batteries nanocomposite, described charcoal coated lithium iron phosphate composite, the particle diameter of this charcoal coated lithium iron phosphate composite is 30～100 nm, wherein, the charcoal coating thickness is 2～3 nm, and the mass ratio of charcoal coating layer and LiFePO4 nuclear is (0.1 ~ 0.01): (0.9 ~ 0.99) is characterized in that may further comprise the steps:
(1) amphipathic Carbon Materials is mixed with ethylene glycol, ultrasonic dispersion 0.3～2 h is mixed with the suspension that mass concentration is 1.5～6 mg/ml; Wherein, the precursor material of amphipathic Carbon Materials comprises: coal tar pitch, petroleum coke, needle coke;
(2) take lithium hydroxide, lithium acetate as the lithium source, take phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate as the phosphorus source, stir lower in lithium source adding step (1) suspension, the content that makes Li in the reaction system is 0.03～3 mol/L, is 3:1 by the mol ratio of Li and P, slowly adds the phosphorus source in reaction system, carry out stirring reaction 0.5～2 h, make the lithium phosphate suspension-turbid liquid, the ferrous salt of adding and lithium phosphate Isoequivalent weight carries out stirring reaction 0.5～2 h in the suspension-turbid liquid that makes.Described ferrous salt is ferrous sulfate, frerrous chloride;
(3) the equal phase dispersant liquid of step (2) preparation is transferred in the polytetrafluoroethylene reactor, sealing, reactor placed 110～220 ℃ constant temperature oven, carry out solvent thermal reaction 5～24 h, after naturally cooling to room temperature product is washed to existing without heteroion with deionized water and absolute ethyl alcohol, then at 60～120 ℃ of lower vacuumize 3～24 h, obtain the composite ferric lithium phosphate material that amphipathic Carbon Materials coats;
(4) composite ferric lithium phosphate material that the amphipathic Carbon Materials that step (3) is made coats places retort; under the protection of nitrogen or argon gas; heating rate with 1～10 ℃/min rises to 500～800 ℃; constant temp. heating is processed 1～15 h; then naturally cool to room temperature, obtain charcoal coated LiFePO 4 for lithium ion batteries nanocomposite.
The present invention has following advantage: the present invention adopts solvent-thermal method, so that can evenly mix, is conducive to few defective between the solution environmental intermediate ion, is orientated, the perfectly growth of crystal, and product degree of crystallinity is high; Synthesis technique of the present invention is simple, and process conditions are easy to control and advantages of nontoxic raw materials, pollution-free, cheap and easy to get; The method that adopts original position to coat coats with precursor synthesis charcoal and finishes in the lump, and the charcoal coating layer can improve the electron conduction ability of material greatly; This method controlledly synthesis particle size is the LiFePO4 of 30～100 nm; When using as anode material for lithium-ion batteries, have good high rate during charging-discharging and stable cycle performance.
Description of drawings
Fig. 1 is the XRD collection of illustrative plates of the charcoal coated LiFePO 4 for lithium ion batteries nanocomposite of the embodiment of the invention 1 preparation.
Fig. 2 is the SEM photo of the charcoal coated LiFePO 4 for lithium ion batteries nanocomposite of the embodiment of the invention 1 preparation.
Fig. 3 is the HRTEM photo of the charcoal coated LiFePO 4 for lithium ion batteries nanocomposite of the embodiment of the invention 1 preparation.
Fig. 4 is that the charcoal coated LiFePO 4 for lithium ion batteries nanocomposite of the embodiment of the invention 1 preparation is as the rate charge-discharge curve chart of anode material for lithium-ion batteries.
Fig. 5 is that the charcoal coated LiFePO 4 for lithium ion batteries nanocomposite of the embodiment of the invention 1 preparation is as the cycle performance curve chart of anode material for lithium-ion batteries.
Embodiment
Embodiment 1
1. take medium temperature coal tar pitch as raw material, adopt acid oxidation to prepare amphipathic Carbon Materials, concrete preparation process is as follows: pitch is used the ball mill crushing screening, get particle diameter less than the pitch particle of 150 μ m as raw material.With 50 ml nitration mixture (take mass concentration as 65% red fuming nitric acid (RFNA) and the concentrated sulfuric acid volume ratio of mass concentration as 98% as the 3:7 preparation) be heated to 80 ℃, stir speed (S.S.) with 300 r/min stirs, add 10 g medium temperature coal pitch, react 3 h, pour reactant in 500 mL deionized waters cessation reaction, the employing pressure-reducing filter filters, and the gained filter cake is extremely neutral with the deionized water washing; The solid matter that obtains is joined in the NaOH solution of 500 mL concentration, 1 mol/L, the rotating speed with 300 r/min under 80 ℃ stirs 1 h, and filtration under diminished pressure keeps the pH value of solution all the time greater than 12 in this process; Collect filtrate, in the filtrate that obtains, drip the HCl of 1 mol/L, regulate its pH value to 2, have this moment precipitation to generate; Centrifugation, with the sediment that obtains with deionized water wash to the pH value be 3,100 ℃ of oven dry 10 h namely get the amphipathic Carbon Materials of asphaltic base in baking oven.
2. the amphipathic Carbon Materials of asphaltic base that 0.1896 g step 1 is made joins in the 60 ml ethylene glycol, ultrasonic dispersion 30 min.Add 1.5120 g lithium hydroxide powder,, drip mass concentration under the magnetic agitation condition and be 85% phosphatase 11 .3835 g to suspension, continue to stir 30 min, obtain the lithium phosphate suspension-turbid liquid.In above-mentioned suspension-turbid liquid, add 3.336 g ferrous sulfate, continue to stir 30 min, join in the 75 ml reactors final suspension-turbid liquid and sealing, put into baking oven and be heated to 180 ℃, be incubated 10 h, naturally centrifugal after the cooling, and with deionized water and absolute ethanol washing extremely without SO
4 2-Heteroion exists, 80 ℃ of vacuumize 12 h.The product of getting after the oven dry places the high temperature carbonization stove, and the heating rate with 2 ℃/min under nitrogen protection is warming up to 650 ℃, naturally cools to room temperature behind constant temperature 3 h, namely obtains product.
The XRD collection of illustrative plates of the charcoal coated lithium iron phosphate composite that embodiment 1 makes as shown in Figure 1, the peak position of the peak position of this material and standard card (PDF 81-1173) is in full accord, provable material is the LiFePO4 pure phase.Get approximately 30 nm of prepared product particle size, even size distribution from the SEM photo of Fig. 2.And from the HRTEM photo of Fig. 3, can find out the thick charcoal layer of product particle coated with uniform one deck 2～3 nm.Being assembled into battery records material capacity under discharge current density 1C, 10C, 30C and reaches respectively 138.8 mAh/g, 106.7 mAh/g, 77.9 mAh/g.
Embodiment 2
The preparation method is substantially the same manner as Example 1, and difference is to add in the step 2 the amphipathic Carbon Materials of 0.0948 g asphaltic base.The products obtained therefrom particle mean size is 100 nm approximately.
Embodiment 3
The preparation method is substantially the same manner as Example 1, and difference is that initial feed is needle coke in the step 1, and the nitration mixture consumption is 100 ml, the amphipathic Carbon Materials of preparation needle coke base.Replace the amphipathic Carbon Materials of asphaltic base with the amphipathic Carbon Materials of needle coke base in the step 2.The products obtained therefrom particle mean size is 100 nm approximately.
Embodiment 4
1. the step 1 with embodiment 1 is identical.
2. the amphipathic Carbon Materials of asphaltic base that 0.2844 g step 1 is made joins in the 60 ml ethylene glycol, ultrasonic dispersion 1 h.Add 5.5080 g lithium acetate powder, add 2.0700 g ammonium dihydrogen phosphates under the magnetic agitation condition, continue to stir 1 h, obtain the lithium phosphate suspension-turbid liquid.In above-mentioned suspension-turbid liquid, add 5.0040 g ferrous sulfate, continue to stir 30 min, join in the 75 ml reactors final suspension-turbid liquid and sealing, put into baking oven and be heated to 170 ℃, be incubated 6 h, naturally centrifugal after the cooling, and with deionized water and absolute ethanol washing extremely without SO
4 2-Heteroion exists, 90 ℃ of vacuumize 12 h.The product of getting after the oven dry places the high temperature carbonization stove, and the heating rate with 5 ℃/min under nitrogen protection is warming up to 700 ℃, naturally cools to room temperature behind constant temperature 3 h, namely obtains product.The products obtained therefrom particle size is 50 nm approximately, even size distribution.
Embodiment 5
1. the step 1 with embodiment 1 is identical.
2. the amphipathic Carbon Materials of asphaltic base that 0.1517 g step 1 is made joins in the 60 ml ethylene glycol, ultrasonic dispersion 30 min.Add 3.6720 g lithium acetate powder, add 1.5720 g diammonium hydrogen phosphates under the magnetic agitation condition, continue to stir 1 h, obtain the lithium phosphate suspension-turbid liquid.In above-mentioned suspension-turbid liquid, add 2.3880 g frerrous chlorides, continue to stir 30 min, join in the 75 ml reactors final suspension-turbid liquid and sealing, put into baking oven and be heated to 200 ℃, be incubated 8 h, naturally centrifugal after the cooling, and with deionized water and absolute ethanol washing extremely without Cl
-Heteroion exists, 80 ℃ of vacuumize 12 h.The product of getting after the oven dry places the high temperature carbonization stove, and the heating rate with 1 ℃/min under nitrogen protection is warming up to 650 ℃, naturally cools to room temperature behind constant temperature 6 h, namely obtains product.The products obtained therefrom particle size is 45 nm approximately, even size distribution.
Claims (1)
1. the preparation method of a charcoal coated LiFePO 4 for lithium ion batteries nanocomposite, described charcoal coated lithium iron phosphate composite, the particle diameter of this charcoal coated lithium iron phosphate composite is 30～100 nm, wherein, the charcoal coating thickness is 2～3 nm, the mass ratio of charcoal coating layer and LiFePO4 nuclear is (0.1 ~ 0.01): (0.9 ~ 0.99) is characterized in that may further comprise the steps:
(1) amphipathic Carbon Materials is mixed with ethylene glycol, ultrasonic dispersion 0.3～2 h is mixed with the suspension that mass concentration is 1.5～6 mg/ml; Wherein, the precursor material of amphipathic Carbon Materials comprises: coal tar pitch, petroleum coke, needle coke;
(2) take lithium hydroxide, lithium acetate as the lithium source, take phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate as the phosphorus source, stir lower in lithium source adding step (1) suspension, the content that makes Li in the reaction system is 0.03～3 mol/L, mol ratio by Li and P is 3:1, in reaction system, slowly add the phosphorus source, carry out stirring reaction 0.5～2 h, make the lithium phosphate suspension-turbid liquid, in the suspension-turbid liquid that makes, add the ferrous salt with the lithium phosphate Isoequivalent weight, carry out stirring reaction 0.5～2 h, described ferrous salt is ferrous sulfate, frerrous chloride;
(3) the equal phase dispersant liquid of step (2) preparation is transferred in the polytetrafluoroethylene reactor, sealing, reactor placed 110～220 ℃ constant temperature oven, carry out solvent thermal reaction 5～24 h, after naturally cooling to room temperature product is washed to existing without heteroion with deionized water and absolute ethyl alcohol, then at 60～120 ℃ of lower vacuumize 3～24 h, obtain the composite ferric lithium phosphate material that amphipathic Carbon Materials coats;
(4) composite ferric lithium phosphate material that the amphipathic Carbon Materials that step (3) is made coats places retort; under the protection of nitrogen or argon gas; heating rate with 1～10 ℃/min rises to 500～800 ℃; constant temp. heating is processed 1～15 h; then naturally cool to room temperature, obtain charcoal coated LiFePO 4 for lithium ion batteries nanocomposite.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103904325A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | High-multiplying-power type lithium iron phosphate/carbon composite material and preparation method thereof |
| CN105633369A (en) * | 2016-01-04 | 2016-06-01 | 兰州理工大学 | Preparation method of carbon-coated lithium iron phosphate material |
| CN107507975A (en) * | 2017-08-24 | 2017-12-22 | 扬州大学 | A kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nano-hollow ball |
| CN114171740A (en) * | 2021-11-04 | 2022-03-11 | 江苏涛立电子新材料有限公司 | Preparation method of nano lithium iron phosphate cathode material and lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103904325A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | High-multiplying-power type lithium iron phosphate/carbon composite material and preparation method thereof |
| CN105633369A (en) * | 2016-01-04 | 2016-06-01 | 兰州理工大学 | Preparation method of carbon-coated lithium iron phosphate material |
| CN105633369B (en) * | 2016-01-04 | 2017-11-07 | 兰州理工大学 | A kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries material |
| CN107507975A (en) * | 2017-08-24 | 2017-12-22 | 扬州大学 | A kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nano-hollow ball |
| CN114171740A (en) * | 2021-11-04 | 2022-03-11 | 江苏涛立电子新材料有限公司 | Preparation method of nano lithium iron phosphate cathode material and lithium ion battery |
| CN114171740B (en) * | 2021-11-04 | 2024-01-30 | 江苏涛立电子新材料有限公司 | Preparation method of nano lithium iron phosphate positive electrode material and lithium ion battery |
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