CN103094564A - Method for preparing composite nano material filled with lithium iron phosphate between graphene layers - Google Patents
Method for preparing composite nano material filled with lithium iron phosphate between graphene layers Download PDFInfo
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- CN103094564A CN103094564A CN2013100155440A CN201310015544A CN103094564A CN 103094564 A CN103094564 A CN 103094564A CN 2013100155440 A CN2013100155440 A CN 2013100155440A CN 201310015544 A CN201310015544 A CN 201310015544A CN 103094564 A CN103094564 A CN 103094564A
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Abstract
The invention relates to a method for preparing a composite nano material filled with lithium iron phosphate between graphene layers and belongs to the technical field of anode materials for lithium ion batteries. The method comprises the following steps of: dispersing graphene and a surfactant in ethylene glycol to prepare a suspension, sequentially adding lithium salt, iron salt and phosphate into the suspension according to a molar ratio, and ultrasonically stirring, thereby obtaining a precursor solution; performing a thermal reaction on the precursor solution at the temperature of 150-200 DEG C, washing, filtering, grinding and calcining the precipitate, thereby obtaining the composite nano material filled with lithium iron phosphate between graphene layers. The method has the advantages that the process is simple, the nano lithium iron phosphate particle layer on graphene in the obtained composite material is uniform in distribution, the composite nano material has a sandwich overlapped structure, and according to the composite material, the charging and discharging performance of the lithium ion battery are improved.
Description
Technical field
The present invention relates to fill between a kind of graphene layer the composite nano materials preparation method of LiFePO4, belong to the positive electrode technical field of lithium ion battery.
Background technology
LiFePO 4 material (LiFePO
4) be mainly used in the positive electrode of various lithium ion batteries.1996 and 1997, Japan and the research group of the U.S. find and have reported the characteristic that the LiFePO 4 material of olivine structural is moved into and deviate from lithium ion with having invertibity, make this material be subject to great attention, and cause research widely and development rapidly.With traditional lithium ion secondary battery anode material, to compare as the cobalt acid lithium of layer structure and the LiMn2O4 of spinel structure, LiFePO4 has following characteristics: (1) energy density is high, and its theoretical specific capacity is 170 mAh/g; (2) life-span long, can discharge and recharge more than 2000 times; (3) operating voltage is moderate, and its smooth working voltage is 3.4V; (4) safety non-toxic is pollution-free, and LiFePO 4 material is present safest anode material for lithium-ion batteries, does not contain any harmful heavy metal element; (5) high-temperature behavior and Heat stability is good, memory-less effect; (6) the raw material wide material sources, cheap.
LiFePO 4 material has attracted people to pay close attention to widely as the desirable positive electrode of lithium ion battery of new generation, but in lithium iron phosphate positive material development process, still have some key issues to be still waiting further to be solved and perfect, mainly comprise: (1) traditional LiFePO 4 material preparation technology adopts solid phase method high temperature sintering technology, energy consumption is high and granular size is uneven, easily produces capacity attenuation in using in the later stage; (2) LiFePO4 of preparation is that semi-conducting material and particle are larger, causes between granule interior and particle diffusion rate and the transmission rate of electronics and lithium ion low, has limited the high-rate charge-discharge capability of material.
For improving the conductance of lithium iron phosphate positive material, in traditional preparation process, the carbon black of the high structure of many employings is conductive agent, and (5 ~ 20wt%) are unfavorable for the raising of battery specific energy but the carbon black consumption is relatively large.Therefore, use the higher novel low dimensional structures material with carbon element (graphite, carbon nano-tube, fullerene etc.) of conductance can effectively improve electronics and lithium ion diffusion transport speed between LiFePO4 inside and material granule as conductive agent, improve energy density and the power density of material.Graphene as a kind of novel Two-dimensional Carbon nano material, is the ultra-thin materials of monatomic thickness.Graphene itself has good electron conduction, can be used for improving the electric conductivity of positive electrode.The high theoretical specific area of grapheme material can make itself and electrode active material better compound, is easy to form the multidimensional conductive structure.Outstanding mechanical property and the heat conductivility of grapheme material, carry out the compound popular method that improves the LiFePO4 performance that becomes with Graphene and lithium iron phosphate positive material in addition.
Chinese patent application CN201110222958.1A discloses a kind of lithium iron phosphate/carbon composite material and application thereof of the Graphene modification that obtains by the compound mode of solvent heat original position; Chinese patent application CN201210011527.5A discloses method for making of a kind of LiFePO4/graphene composite material that the interlayer flake structure arranged and uses thereof, its main method is at first to adopt the solution chemistry route to synthesize with " precursor conversion method " to have the alternate layer structure precursor of inorganic-organic, then is the alternate LiFePO4 of lamella/Graphene interlayer composite material by the processing of high temperature inert atmosphere with precursor conversion.But the method weak point is: 1. step is slightly many, complex process, the homogeneity of bad control product; 2. the organic amine that adds or affect the chemical property of composite material.
Sum up Patents in recent years, find that this area not yet reports by the solvent-thermal method preparation and have the Graphene of sandwich/LiFePO4 composite nano materials.
Summary of the invention
The object of the invention is to provide the composite nano materials preparation method who fills LiFePO4 between a kind of graphene layer, and the method advantage is the technique simple and stable, and cost is relatively low, and the nano composite material that makes has good performance.
The present invention is realized by the following technical programs, fills the composite nano materials preparation method of LiFePO4 between a kind of graphene layer, it is characterized in that comprising following process:
1) presoma preparation
Wherein a kind of of Graphene and surfactant neopelex, lauryl sodium sulfate and three-sulfopropyl myristyl diformazan betaine is dispersed in ethylene glycol for 1:1 in mass ratio, be mixed with the suspension of graphene-containing 0.29 ~ 2.29g/L, mass ratio by LiFePO4 and Graphene is 1: 0.5 ~ 5%, and presses Li: Fe: PO
4Mol ratio be 2.7: 1: 1, at first add wherein a kind of of lithium hydroxide, lithium acetate, lithium carbonate and lithium nitrate to suspension, then add wherein a kind of of frerrous chloride, ferrous sulfate, ferrous phosphate and ferrous citrate, add at last wherein a kind of of phosphoric acid, ammonium di-hydrogen phosphate and DAP, ultrasonic 5 ~ 10min at room temperature, stir 2 ~ 6h in 30 ~ 80 ℃ of lower magnetic forces of temperature again, obtain precursor solution;
2) thermal synthesis and calcining
The precursor solution of step 1) system is added at 150 ~ 200 ℃ of inherent temperature of reactor react 4 ~ 12h, then remove the supernatant of reactant, with deionized water to sediment wash to cleaning solution pH be 7, through suction filtration, pulverize after, powder is at 60 ~ 100 ℃ of oven dry 8-12h of temperature; Again powder is spread out and put in quartz boat, quartz boat is placed in the tube furnace flat-temperature zone, passes into argon gas 5-30min to tube furnace with flow 100-300mL/min, and in argon shield, heating rate with 7.5 ~ 10 ℃/min is warming up to 400 ~ 600 ℃, calcining at constant temperature 0.5 ~ 3h; Be down to room temperature with the rate of temperature fall of 5 ~ 10 ℃/min afterwards under the protection of argon gas, obtain filling between graphene layer the composite nano materials of LiFePO4.
The present invention has the following advantages: preparation technology is simple, and in preparation process, Graphene has good dispersiveness in organic solvent; In resulting composite material, homodisperse graphene film forms multidimensional conductive network structure, nano-grade lithium iron phosphate stratum granulosum on Graphene is evenly distributed, Graphene/LiFePO4 composite nano materials presents the sandwich-like overlay structure, the Graphene surface is complete and utilance is high, and this composite material can improve the charge-discharge performance of lithium ion battery.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the Graphene that uses of the embodiment of the present invention 1 to embodiment 7.
Fig. 2 is that the embodiment of the present invention 1 makes the stereoscan photograph of filling the composite nano materials of LiFePO4 between graphene layer.
Fig. 3 is that the embodiment of the present invention 1 makes the transmission electron microscope photo of filling the composite nano materials of LiFePO4 between graphene layer.
Fig. 4 is that the embodiment of the present invention 1 makes the X ray collection of illustrative plates of filling the composite nano materials of LiFePO4 between graphene layer.
Fig. 5 is that the embodiment of the present invention 1 makes the charge/discharge capacity of composite nano materials under the 0.1C discharge-rate of filling LiFePO4 between graphene layer.
Embodiment
Further the present invention will be described below in conjunction with embodiment, and these embodiment only are used for explanation the present invention, do not limit the present invention.
Embodiment 1
The Graphene of 0.02g is added in 20mL ethylene glycol, add simultaneously three-sulfopropyl myristyl diformazan betaine of 0.02g, at room temperature ultrasonic 1h.The ammonium dihydrogen phosphate of weighing 0.34855g and the green vitriol of 0.8425g add in mentioned solution, at room temperature continue afterwards magnetic agitation 10min.Take the hydronium(ion) oxidation lithium of 0.37764g, be dissolved in 15mL ethylene glycol, in the mentioned solution that dropwise adds with the speed of 15/min with dropper after dissolving, dropwise rear continuation magnetic agitation 3h and obtain precursor mixed solution.With precursor mixed solution magnetic agitation 30min at room temperature after ultrasonic 30min at room temperature, be placed in rapidly the gained mixed liquor in autoclave subsequently, react 10h under 200 ℃, room temperature cooled and filtered, washing are dried 10h in the vacuum drying chamber of 80 ℃.After being ground, powder after oven dry spreads out and puts in quartz boat; quartz boat is placed in the tube furnace flat-temperature zone; flow with 200mL/min passes into the 10min argon gas to drain air; heating rate with 10 ℃/min is warming up to 500 ℃ under argon shield afterwards; at this temperature calcining at constant temperature 1h; with the speed of 5 ℃/min, the tube furnace temperature is down to room temperature afterwards, obtains Graphene/LiFePO4 composite nano materials.
The Graphene of 0.01g is added in 20mL ethylene glycol, add simultaneously three-sulfopropyl myristyl diformazan betaine of 0.01g, at room temperature ultrasonic 1h.The ammonium dihydrogen phosphate of weighing 0.34855g and the green vitriol of 0.8425g add in mentioned solution, at room temperature continue afterwards to stir.Take the hydronium(ion) oxidation lithium of 0.37764g, be dissolved in 15mL ethylene glycol, in the mentioned solution that dropwise adds with the speed of 15/min with dropper after dissolving, dropwise rear continuation stirring 3h and obtain precursor mixed solution.Precursor mixed solution is at room temperature at room temperature being stirred 30min after ultrasonic 30min, subsequently the gained mixed liquor is being placed in rapidly in autoclave, react 10h under 200 ℃, room temperature cooled and filtered, washing are dried 10h in the vacuum drying chamber of 80 ℃.After being ground, powder after oven dry spreads out and puts in quartz boat; quartz boat is placed in the tube furnace flat-temperature zone; flow with 200mL/min passes into the 10min argon gas to drain air; heating rate with 10 ℃/min is warming up to 500 ℃ under argon shield afterwards; at this temperature calcining at constant temperature 1h; with the speed of 5 ℃/min, the tube furnace temperature is down to room temperature afterwards, obtains Graphene/LiFePO4 composite nano materials.
Embodiment 3
The Graphene of 0.08g is added in 20mL ethylene glycol, add simultaneously three-sulfopropyl myristyl diformazan betaine of 0.08g, at room temperature ultrasonic 1h.The ammonium dihydrogen phosphate of weighing 0.34855g and the green vitriol of 0.8425g add in mentioned solution, at room temperature continue afterwards to stir.Take the hydronium(ion) oxidation lithium of 0.37764g, be dissolved in 15mL ethylene glycol, in the mentioned solution that dropwise adds with the speed of 15/min with dropper after dissolving, dropwise rear continuation stirring 3h and obtain precursor mixed solution.Precursor mixed solution is at room temperature at room temperature being stirred 30min after ultrasonic 30min, subsequently the gained mixed liquor is being placed in rapidly in autoclave, react 10h under 200 ℃, room temperature cooled and filtered, washing are dried 10h in the vacuum drying chamber of 80 ℃.After being ground, powder after oven dry spreads out and puts in quartz boat; quartz boat is placed in the tube furnace flat-temperature zone; flow with 200mL/min passes into the 10min argon gas to drain air; heating rate with 10 ℃/min is warming up to 500 ℃ under argon shield afterwards; at this temperature calcining at constant temperature 1h; with the speed of 5 ℃/min, the tube furnace temperature is down to room temperature afterwards, obtains Graphene/LiFePO4 composite nano materials.
Embodiment 4
The Graphene of 0.02g is added in 20mL ethylene glycol, add simultaneously three-sulfopropyl myristyl diformazan betaine of 0.02g, at room temperature ultrasonic 1h.The ammonium dihydrogen phosphate of weighing 0.34855g and the green vitriol of 0.8425g add in mentioned solution, at room temperature continue afterwards to stir.Take the hydronium(ion) oxidation lithium of 0.37764g, be dissolved in 15mL ethylene glycol, in the mentioned solution that dropwise adds with the speed of 15/min with dropper after dissolving, dropwise rear continuation stirring 3h and obtain precursor mixed solution.Precursor mixed solution is at room temperature at room temperature being stirred 30min after ultrasonic 30min, subsequently the gained mixed liquor is being placed in rapidly in autoclave, react 4h under 200 ℃, room temperature cooled and filtered, washing are dried 10h in the vacuum drying chamber of 80 ℃.After being ground, powder after oven dry spreads out and puts in quartz boat; quartz boat is placed in the tube furnace flat-temperature zone; flow with 200mL/min passes into the 10min argon gas to drain air; heating rate with 10 ℃/min is warming up to 500 ℃ under argon shield afterwards; at this temperature calcining at constant temperature 1h; with the speed of 5 ℃/min, the tube furnace temperature is down to room temperature afterwards, obtains Graphene/LiFePO4 composite nano materials.
Embodiment 5
The Graphene of 0.02g is added in 20mL ethylene glycol, add simultaneously three-sulfopropyl myristyl diformazan betaine of 0.02g, at room temperature ultrasonic 1h.The ammonium dihydrogen phosphate of weighing 0.34855g and the green vitriol of 0.8425g add in mentioned solution, at room temperature continue afterwards to stir.Take the hydronium(ion) oxidation lithium of 0.37764g, be dissolved in 15mL ethylene glycol, in the mentioned solution that dropwise adds with the speed of 15/min with dropper after dissolving, dropwise rear continuation stirring 3h and obtain precursor mixed solution.Precursor mixed solution is at room temperature at room temperature being stirred 30min after ultrasonic 30min, subsequently the gained mixed liquor is being placed in rapidly in autoclave, react 12h under 150 ℃, room temperature cooled and filtered, washing are dried 10h in the vacuum drying chamber of 80 ℃.After being ground, powder after oven dry spreads out and puts in quartz boat; quartz boat is placed in the tube furnace flat-temperature zone; flow with 200mL/min passes into the 10min argon gas to drain air; heating rate with 10 ℃/min is warming up to 500 ℃ under argon shield afterwards; at this temperature calcining at constant temperature 1h; with the speed of 5 ℃/min, the tube furnace temperature is down to room temperature afterwards, obtains Graphene/LiFePO4 composite nano materials.
Embodiment 6
The Graphene of 0.02g is added in 20mL ethylene glycol, add simultaneously three-sulfopropyl myristyl diformazan betaine of 0.02g, at room temperature ultrasonic 1h.The ammonium dihydrogen phosphate of weighing 0.11618g and the green vitriol of 0.28083g add in mentioned solution, at room temperature continue afterwards to stir.Take the hydronium(ion) oxidation lithium of 0.12588g, be dissolved in 15mL ethylene glycol, in the mentioned solution that dropwise adds with the speed of 15/min with dropper after dissolving, dropwise rear continuation stirring 3h and obtain precursor mixed solution.Precursor mixed solution is at room temperature at room temperature being stirred 30min after ultrasonic 30min, subsequently the gained mixed liquor is being placed in rapidly in autoclave, react 10h under 200 ℃, room temperature cooled and filtered, washing are dried 10h in the vacuum drying chamber of 80 ℃.After being ground, powder after oven dry spreads out and puts in quartz boat; quartz boat is placed in the tube furnace flat-temperature zone; flow with 200mL/min passes into the 10min argon gas to drain air; heating rate with 10 ℃/min is warming up to 500 ℃ under argon shield afterwards; at this temperature calcining at constant temperature 1h; with the speed of 5 ℃/min, the tube furnace temperature is down to room temperature afterwards, obtains Graphene/LiFePO4 composite nano materials.
Embodiment 7
The Graphene of 0.02g is added in 20mL ethylene glycol, add simultaneously three-sulfopropyl myristyl diformazan betaine of 0.02g, at room temperature ultrasonic 1h.The ammonium dihydrogen phosphate of weighing 0.6971g and the green vitriol of 1.685g add in mentioned solution, at room temperature continue afterwards to stir.Take the hydronium(ion) oxidation lithium of 0.75528g, be dissolved in 15mL ethylene glycol, in the mentioned solution that dropwise adds with the speed of 15/min with dropper after dissolving, dropwise rear continuation stirring 3h and obtain precursor mixed solution.Precursor mixed solution is at room temperature at room temperature being stirred 30min after ultrasonic 30min, subsequently the gained mixed liquor is being placed in rapidly in autoclave, react 10h under 200 ℃, room temperature cooled and filtered, washing are dried 10h in the vacuum drying chamber of 80 ℃.After being ground, powder after oven dry spreads out and puts in quartz boat; quartz boat is placed in the tube furnace flat-temperature zone; flow with 200mL/min passes into the 10min argon gas to drain air; heating rate with 10 ℃/min is warming up to 500 ℃ under argon shield afterwards; at this temperature calcining at constant temperature 1h; with the speed of 5 ℃/min, the tube furnace temperature is down to room temperature afterwards, obtains Graphene/LiFePO4 composite nano materials.
Claims (1)
1. fill the composite nano materials preparation method of LiFePO4 between a graphene layer, it is characterized in that comprising following process:
1) presoma preparation
Wherein a kind of of Graphene and surfactant neopelex, lauryl sodium sulfate and three-sulfopropyl myristyl diformazan betaine is dispersed in ethylene glycol for 1:1 in mass ratio, be mixed with the suspension of graphene-containing 0.29 ~ 2.29g/L, mass ratio by LiFePO4 and Graphene is 1: 0.5 ~ 5%, and presses Li: Fe: PO
4Mol ratio be 2.7: 1: 1, at first add wherein a kind of of lithium hydroxide, lithium acetate, lithium carbonate and lithium nitrate to suspension, then add wherein a kind of of frerrous chloride, ferrous sulfate, ferrous phosphate and ferrous citrate, add at last wherein a kind of of phosphoric acid, ammonium di-hydrogen phosphate and DAP, ultrasonic 5 ~ 10min at room temperature, stir 2 ~ 6h in 30 ~ 80 ℃ of lower magnetic forces of temperature again, obtain precursor solution;
2) thermal synthesis and calcining
The precursor solution of step 1) system is added at 150 ~ 200 ℃ of inherent temperature of reactor react 4 ~ 12h, then remove the supernatant of reactant, with deionized water to sediment wash to cleaning solution pH be 7, through suction filtration, pulverize after, powder is at 60 ~ 100 ℃ of oven dry 8-12h of temperature; Again powder is spread out and put in quartz boat, quartz boat is placed in the tube furnace flat-temperature zone, passes into argon gas 5-30min to tube furnace with flow 100-300mL/min, and in argon shield, heating rate with 7.5 ~ 10 ℃/min is warming up to 400 ~ 600 ℃, calcining at constant temperature 0.5 ~ 3h; Be down to room temperature with the rate of temperature fall of 5 ~ 10 ℃/min afterwards under the protection of argon gas, obtain filling between graphene layer the composite nano materials of LiFePO4.
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Cited By (8)
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| CN103943864A (en) * | 2014-04-15 | 2014-07-23 | 中南大学 | Lithium iron phosphate-based composite positive electrode material as well as preparation method and application thereof |
| CN104835939A (en) * | 2015-05-05 | 2015-08-12 | 南京理工大学 | Preparation method of high-performance lithium iron phosphate composite material |
| CN105789591A (en) * | 2016-04-13 | 2016-07-20 | 同济大学 | Method for synthesizing graphene/FeSn-nanorod array/graphene composite material of tent type frame structure |
| CN106450214A (en) * | 2016-11-08 | 2017-02-22 | 成都新柯力化工科技有限公司 | Layered lithium iron phosphate composite material and preparation method thereof |
| CN107941880A (en) * | 2017-11-16 | 2018-04-20 | 江苏鱼跃医疗设备股份有限公司 | For improving the reaction reagent and glucose sensor comprising betanin derivative of glucose sensor storage stability |
| CN108199019A (en) * | 2017-12-25 | 2018-06-22 | 深圳市山木新能源科技股份有限公司 | Multi-layer graphene/LiFePO4 intercalation composite material preparation method and application |
| CN109037658A (en) * | 2018-08-31 | 2018-12-18 | 重庆工商大学 | A kind of lithium iron phosphate positive material preparation method of polymer overmold |
| CN109301177A (en) * | 2018-08-15 | 2019-02-01 | 湖南鸿跃电池材料有限公司 | A kind of stratiform composite ferric lithium phosphate material and preparation method thereof |
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| CN108199019A (en) * | 2017-12-25 | 2018-06-22 | 深圳市山木新能源科技股份有限公司 | Multi-layer graphene/LiFePO4 intercalation composite material preparation method and application |
| CN109301177A (en) * | 2018-08-15 | 2019-02-01 | 湖南鸿跃电池材料有限公司 | A kind of stratiform composite ferric lithium phosphate material and preparation method thereof |
| CN109037658A (en) * | 2018-08-31 | 2018-12-18 | 重庆工商大学 | A kind of lithium iron phosphate positive material preparation method of polymer overmold |
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