CN102392311A - Method for synthesizing lithium iron phosphate material by adopting electrostatic spinning - Google Patents
Method for synthesizing lithium iron phosphate material by adopting electrostatic spinning Download PDFInfo
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- CN102392311A CN102392311A CN2010105345452A CN201010534545A CN102392311A CN 102392311 A CN102392311 A CN 102392311A CN 2010105345452 A CN2010105345452 A CN 2010105345452A CN 201010534545 A CN201010534545 A CN 201010534545A CN 102392311 A CN102392311 A CN 102392311A
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Abstract
The invention belongs to a method for synthesizing a lithium iron phosphate material by adopting electrostatic spinning. The selected compounds comprise an iron source compound which is selected from one or a mixture of two of FeC2O4, Fe2O3 and FePO4, a lithium source compound which is selected from one or a mixture of two of LiH2PO4, Li2CO3, Li2HPO4 and LiOH, a phosphate radical containing compound which is selected from one or a mixture of two of LiH2PO4, (NH4)2HPO4, NH4H2PO4 and H3PO4, a polymer which is selected from one or two of polyvinyl alcohol, polyacrylonitrile and polyvinylpyrrolidone, and a solvent used by polymer solution which is selected from one or a mixture of more than two of water, ethanol, glycol, acetic acid and isopropanol. The lithium iron phosphate in a nano structure is prepared by preparing spinning solution, preparing a lithium iron phosphate precursor and drying and calcining the lithium iron phosphate precursor. The method has the following beneficial effects: the high-rate charge/discharge performance of the lithium iron phosphate and the specific capacity of charge/discharge under low temperature are improved; and the new method is provided for synthesizing lithium iron phosphate.
Description
Technical field
The invention belongs to a kind of method of electrostatic spinning synthesizing lithium iron phosphate materials.
Technical background
Lithium ion battery is a kind of desirable energy storage device.Advantages such as it is pollution-free, long service life, memory-less effect.Be widely used in the various electronic equipments.In recent years, along with the minimizing gradually of the fossil level energy such as coal, oil, people are to the enhancing of the consciousness of environmental protection, and lithium ion battery has also obtained huge development in electric automobiles.
Lithium ion battery is made up of following several parts usually: positive pole, negative pole, barrier film, electrolyte, collector, shell.Wherein positive pole occupies an important position in battery.The positive pole of Traditional business battery is generally cobalt acid lithium, and its advantage is a good cycle, and preparation technology is simple.But it also has self fatal shortcoming.Because the scarcity of cobalt resource causes its cost high.And the security performance of cobalt acid lithium is very poor, and this has just restricted its application in the battery of big reactor.LiFePO 4 is with respect to the sour lithium of cobalt, and its cost is low, aboundresources, good cycle, most critical be that it is that security performance is best in the at present known positive electrode, be desirable lithium ion anode material.
Though LiFePO 4 has many good qualities, following shortcoming has restricted its application: the diffusion difficulty of (1) lithium ion in LiFePO 4 causes the utilization rate of active material low; (2) electrical conductivity of LiFePO 4 is low, causes its high rate performance relatively poor.At present, the researcher through synthesis nano LiFePO 4 and carry out carbon at LiFePO 4 and coat the diffusion rate of the lithium ion that improves material and the problem of electrical conductivity.The method of synthesis nano LiFePO 4 mainly contains sol-gal process, hydro-thermal method, coprecipitation at present.
Sol-gal process is that reactant is dissolved in the solvent jointly, concentrates the amorphous gel that is converted into transparent homogeneous behind ion hydrolysis in the solution formation colloidal solid, again gel drying, roasting is obtained powder body material, and wherein the preparation of gel and drying are crucial.The precursor solution chemical uniformity of sol-gal process is good, can reach the molecular level level, and each component ratio is easy to control, and sintering temperature is lower, the less and narrowly distributing of product particle diameter.Choi etc. are at Journal of Power Sources, 2007,163 (2): in 1064 with CH
3COOLi2H
2O, FeCl
24H
2O and P
2O
5Be dissolved in ethanol and process the solution of 1mol/L; To contain Fe and P solution again and mix stirring 3h by stoichiometric proportion earlier, and add the solution that contains Li, the laurate that stirring back adding waits the amount of substance ratio is as surfactant; Put into the volatilization of high-purity Ar stream and concentrate 4h, containing 10%H at last
2Ar atmosphere in obtain product in 500 ℃ of heat treatment 5h.The particle diameter of product is 100～300nm, and specific area reaches 36m
2/ g.The sample that does not add surfactant among the contrast experiment, its specific area are 8m
2/ g.The 1C discharge-rate is 133mAh/g down.Though sol-gal process has synthesized nano level LiFePO
4But grain diameter is still bigger, and the high rate performance of material does not still well improve.
Hydro-thermal is synthetic to be meant in sealing system such as autoclave, is solvent with water, under the self-generated pressure of uniform temperature and water, and a kind of synthetic method that original stock reacts.The hydrothermal condition of HTHP provides the special physicochemical environment that can't obtain under a kind of normal pressure, makes predecessor fully dissolving and reach certain saturation degree in reaction system, is carried out to crystalline nucleation again and generates powder or nanocrystal.Hydro-thermal method can directly obtain good powder, need not to carry out high-temperature roasting and handles, and has avoided the powder reuniting that possibly form in the roasting process.First hydro-thermal method is applied to LiFePO among Electrochem Commun (2001) 3:505 such as Yang
4Synthetic, promptly be 1: 1: 3 FeSO with stoichiometric proportion
4, H
3PO
4With LiOH be raw material, earlier with FeSO
4And H
3PO
4Solution mixes, and splashes into LiOH solution again and stirs 1min, thereby can prevent to form Fe
2(OH)
2, be oxidized to Fe (III) then.The pH value of mixed solution is 7.56 o'clock, at 120 ℃ of hydro-thermal reaction 5h.The particle diameter of product is about 3 μ m, and less than the particle diameter of solid phase method synthetic product, but the capacity of product under the low discharge multiplying power is still lower.
Coprecipitation generally is dissolved in logical N with solubility lithium salts, divalent iron salt and phosphoric acid (or phosphate)
2Water in, regulate pH value and also stir, obtain precipitating, after the filtration washing drying presoma is carried out high temperature sintering under inert environments, obtain the product of crystallization.In solution, feed N
2Not only can reduce contacting of solution and air, prevent Fe
2+Oxidation, and N
2Bubble also help the even mixing of raw material.Arnold is waiting Journal of Power Sources, and 2003, synthesize chemical property product preferably with the method among the 119:247, but occurred the Li of rhombic form in the product easily
3PO
4Deng impurity, influence the energy density of material.
In a word, in existing synthetic method, though synthesized the LiFePO 4 of nano-scale to a certain extent.But the size of particle is still bigger.We use the method for electrostatic spinning here, have synthesized the truly LiFePO 4 of nano-scale, have improved the high rate performance of LiFePO 4 greatly, for nanometer ferrous phosphate lithium material synthetic provides a kind of new method.
Summary of the invention
The method that the purpose of this invention is to provide a kind of electrostatic spinning synthesizing lithium iron phosphate materials.
The present invention is directed to above-mentioned weak point, adopted the method for electrostatic spinning to synthesize the LiFePO 4 electrode material of nano-grade size, improved the electrical conductivity of LiFePO 4 and the diffusion rate of lithium ion, improved the chemical property of material.For LiFePO 4 synthetic provides a kind of new method.
Concrete technical scheme of the present invention is:
The compound that the present invention selects is that Fe source compound is FeC
2O
4, Fe
2O
3, FePO
4In a kind of or two kinds mixture, Li source compound is LiH
2PO
4, Li
2CO
3, Li
2HPO
4, a kind of among the LiOH or two kinds mixture; The phosphoric acid radical compound is LiH
2PO
4, (NH
4)
2HPO
4, NH
4H
2PO
4, H
3PO
4A kind of or two kinds mixture;
Polymer is a kind of in polyvinyl alcohol, polyacrylonitrile, the polyvinylpyrrolidone or two kinds, and the used solvent of polymer solution is: the one or more kinds of mixtures in water, ethanol, ethylene glycol, acetate, the isopropyl alcohol.
Inert gas is N
2, Ar, H
2One or more kinds of mists wherein.
Preparation process is following:
1) spinning solution preparation: it is in the polymer solution of 4%-50% than concentration that Fe source compound, Li source compound, phosphate compounds are joined quality, mixes 1～24 hour down at 25 ℃～100 ℃; Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 0.9～1.1: 1: 1; Fe source compound, Li source compound, phosphate compounds gross mass are m1, and the quality of polymer solution is m2, and m1: m2=0.0025～10 make electrostatic spinning stoste after stirring;
2) LiFePO 4 precursor preparation: the spinning solution for preparing is joined in the syringe, set spinning parameter, wherein spinning voltage is 5KV～30KV; Solidifying distance is 3cm～25cm; Control solution delivery rate is 0.01mL/h～10mL/h;
3) with the LiFePO 4 precursor after 50 ℃ of-80 ℃ of following dryings, place the atmosphere protection stove, 550 ℃～850 ℃ down calcinings 1 hour～24 hours, naturally cool to room temperature, the LiFePO 4 of preparation nanostructured.
The present invention has adopted the method for electrostatic spinning to synthesize nanometer ferrous phosphate lithium first; Improved the performance of LiFePO 4 high power charging-discharging; Improved the specific discharge capacity that discharges and recharges under the cryogenic conditions, for LiFePO 4 synthetic provides a kind of new method.
Description of drawings
Fig. 1. the discharge curve of one-dimensional nano structure ferrousphosphate lithium material under the different multiplying
As can be seen from the figure, under 0.5C, 3C, 5C multiplying power, the specific discharge capacity of synthetic LiFePO 4 is respectively 158mAH/g, 143mAH/g, 135mAH/g.Along with the increase of multiplying power, it is very little that the specific discharge capacity of LiFePO 4 reduces amplitude.
The specific embodiment
Embodiment one:
With FeC
2O
4, LiH
2PO
4Join in the polyvinyl alcohol water solution of quality than concentration 4%, mixed 1 hour down at 25 ℃.Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 0.9: 1: 1; FeC
2O
4, LiH
2PO
4Gross mass is 0.1g, and the quality of polyvinyl alcohol water solution is 40g.Make spinning solution after stirring.The electrostatic spinning stoste that makes is added in the syringe, set spinning voltage 5KV; Solidifying distance is 3cm; Control solution delivery rate is 10mL/h.So prepare LiFePO 4 one-dimensional nano line precursor.The LiFePO 4 precursor for preparing after 50 ℃ of following dryings, is placed N
2In the atmosphere protection stove, calcined 24 hours down, naturally cool to room temperature, the ferrousphosphate lithium material of preparation one-dimensional nano structure at 550 ℃.
Embodiment two:
With FeC
2O
4, Li
2CO
3, NH
4H
2PO
4Join quality and be in 50% the polyvinyl alcohol ethanolic solution, mixed 24 hours down at 50 ℃ than concentration.Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 1: 1: 1; FeC
2O
4, Li
2CO
3, NH
4H
2PO
4Gross mass is 10g, and the quality of polyvinyl alcohol ethanolic solution is 1g.Make spinning solution after stirring.The electrostatic spinning stoste that makes is added in the syringe, set spinning voltage 30KV; Solidifying distance is 25cm; Control solution delivery rate is 0.01mL/h.So prepare the LiFePO 4 precursor.The LiFePO 4 precursor for preparing after 80 ℃ of following dryings, is placed Ar atmosphere protection stove, calcined 1 hour down, naturally cool to room temperature, prepare the ferrousphosphate lithium material of one-dimensional nano structure at 850 ℃.
Synthetic LiFePO 4 is assembled into button cell; Measure the discharge capacity of LiFePO 4 under the different multiplying with cell tester; As shown in Figure 1 under 0.5C, 3C, 5C multiplying power discharge curve, the specific discharge capacity of synthetic LiFePO 4 is respectively 158mAH/g, 143mAH/g, 135mAH/g.
Embodiment three:
With Fe
2O
3, Li
2HPO
4Join in the ethylene glycol solution that mass fraction is 15% polyvinylpyrrolidone, mixed 12 hours down at 80 ℃.Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 1.1: 1: 1; Fe
2O
3, Li
2HPO
4Gross mass is 5g, and the quality of polyvinyl alcohol water solution is 50g.Make electrostatic spinning stoste after stirring.The electrostatic spinning stoste that makes is added in the syringe, set spinning voltage 10KV; Solidifying distance is 6cm; Control solution delivery rate is 5mL/h.So prepare the LiFePO 4 precursor.The LiFePO 4 precursor for preparing after 75 ℃ of following dryings, is placed H
2In the atmosphere protection stove, calcined 23 hours down, naturally cool to room temperature, the LiFePO 4 of preparation nanostructured at 600 ℃.
Embodiment four:
With FePO
4, LiOH joins in the aqueous isopropanol that quality is 20% polyvinyl alcohol than concentration, mixed 2 hours down at 30 ℃.Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 1: 1: 1; FePO
4, the LiOH gross mass is 5g, the quality of polyvinyl alcohol water solution is 60g.Make electrostatic spinning stoste after stirring.The electrostatic spinning stoste that makes is added in the syringe, set spinning voltage 20KV; Solidifying distance is 10cm; Control solution delivery rate is 4mL/h.So prepare the LiFePO 4 precursor.The LiFePO 4 precursor for preparing after 65 ℃ of following dryings, is placed N
2In Ar atmosphere protection stove, calcined 22 hours down at 650 ℃, naturally cool to room temperature, the ferrousphosphate lithium material of preparation one-dimensional nano structure.
Embodiment five:
With FePO
4, Li
2CO
3Join quality and be in 30% the polyvinyl alcohol water solution, mixed 6 hours down at 40 ℃ than concentration.Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 1: 1: 1; FePO
4, Li
2CO
3Gross mass is 5g, and the quality of polyvinyl alcohol water solution is 80g.Make electrostatic spinning stoste after stirring.The electrostatic spinning stoste that makes is added in the syringe, set spinning voltage 20KV; Solidifying distance is 18cm; Control solution delivery rate is 3mL/h.So prepare the LiFePO 4 precursor.The LiFePO 4 precursor for preparing after 80 ℃ of following dryings, is placed N
2In the atmosphere protection stove, calcined 21 hours down, naturally cool to room temperature, the ferrousphosphate lithium material of preparation one-dimensional nano structure at 750 ℃.
Embodiment six:
With Fe
2O
3, Li
2HPO
4Join in the acetic acid solution that mass fraction is 20% polyvinylpyrrolidone, mixed 12 hours down at 80 ℃.Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 1.05: 1: 1; Fe
2O
3, Li
2HPO
4Gross mass is 5g, and the quality of polyvinyl alcohol water solution is 45g.Make electrostatic spinning stoste after stirring.The electrostatic spinning stoste that makes is added in the syringe, set spinning voltage 10KV; Solidifying distance is 7cm; Control solution delivery rate is 4mL/h.So prepare the LiFePO 4 precursor.The LiFePO 4 precursor for preparing after 75 ℃ of following dryings, is placed H
2In Ar mixed atmosphere protection stove, calcined 24 hours down at 600 ℃, naturally cool to room temperature, the LiFePO 4 of preparation nanostructured.
Claims (2)
1. the method for an electrostatic spinning synthesizing lithium iron phosphate materials, the compound of selection is that Fe source compound is FeC
2O
4, Fe
2O
3, FePO
4In a kind of or two kinds mixture, Li source compound is LiH
2PO
4, Li
2CO
3, Li
2HPO
4, a kind of among the LiOH or two kinds mixture; The phosphoric acid radical compound is LiH
2PO
4, (NH
4)
2HPO
4, NH
4H
2PO
4, H
3PO
4A kind of or two kinds mixture;
Polymer is a kind of in polyvinyl alcohol, polyacrylonitrile, the polyvinylpyrrolidone or two kinds, and the used solvent of polymer solution is: the one or more kinds of mixtures in water, ethanol, ethylene glycol, acetate, the isopropyl alcohol;
Preparation process is following:
1) spinning solution preparation: it is in the polymer solution of 4%-50% than concentration that Fe source compound, Li source compound, phosphate compounds are joined quality, mixes 1～24 hour down at 25 ℃～100 ℃; Li wherein
+: Fe
2+: PO
4 3-Mol ratio be 0.9～1.1: 1: 1; Fe source compound, Li source compound, phosphate compounds gross mass are m1, and the quality of polymer solution is m2, and m1: m2=0.0025～10 make electrostatic spinning stoste after stirring;
2) LiFePO 4 precursor preparation: the spinning solution for preparing is joined in the syringe, set spinning parameter, wherein spinning voltage is 5KV～30KV; Solidifying distance is 3cm～25cm; Control solution delivery rate is 0.01mL/h～10mL/h;
3) with the LiFePO 4 precursor after 50 ℃ of-80 ℃ of following dryings, place inert atmosphere furnace, 550 ℃～850 ℃ down calcinings 1 hour～24 hours, naturally cool to room temperature, the LiFePO 4 of preparation nanostructured.
2. as claimed in claim a kind of method of electrostatic spinning synthesizing lithium iron phosphate materials is characterized in that described inert gas is N
2, Ar, H
2One or more kinds of mists wherein.
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Cited By (5)
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|---|---|---|---|---|
| CN103094565A (en) * | 2013-01-23 | 2013-05-08 | 哈尔滨工业大学深圳研究生院 | Lithium iron phosphate/iron phosphide/carbon composite nanofiber as well as preparation and applications of composite nanofiber |
| CN106328942A (en) * | 2016-11-11 | 2017-01-11 | 宁德新能源科技有限公司 | Lithium ferric manganese phosphate anode material, preparation method and application thereof |
| CN107093714A (en) * | 2017-04-12 | 2017-08-25 | 浙江大学 | A kind of electrostatic spinning preparation method of the LiFePO 4 electrode material of Surface coating nano-metal particle |
| CN108598474A (en) * | 2018-04-24 | 2018-09-28 | 湖北工程学院 | A kind of high-energy density lithium battery lithium iron phosphate positive material and preparation method thereof |
| CN109280993A (en) * | 2018-09-03 | 2019-01-29 | 济南大学 | A kind of method of electrostatic spinning technique synthetic silicic acid iron lithium nanofiber |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103094565A (en) * | 2013-01-23 | 2013-05-08 | 哈尔滨工业大学深圳研究生院 | Lithium iron phosphate/iron phosphide/carbon composite nanofiber as well as preparation and applications of composite nanofiber |
| CN103094565B (en) * | 2013-01-23 | 2016-06-08 | 哈尔滨工业大学深圳研究生院 | LiFePO 4/iron phosphide/carbon composite nano-fiber and its preparation method and application |
| CN106328942A (en) * | 2016-11-11 | 2017-01-11 | 宁德新能源科技有限公司 | Lithium ferric manganese phosphate anode material, preparation method and application thereof |
| CN106328942B (en) * | 2016-11-11 | 2019-07-09 | 宁德新能源科技有限公司 | A kind of lithium ferric manganese phosphate positive electrode, preparation method and application |
| CN107093714A (en) * | 2017-04-12 | 2017-08-25 | 浙江大学 | A kind of electrostatic spinning preparation method of the LiFePO 4 electrode material of Surface coating nano-metal particle |
| CN108598474A (en) * | 2018-04-24 | 2018-09-28 | 湖北工程学院 | A kind of high-energy density lithium battery lithium iron phosphate positive material and preparation method thereof |
| CN108598474B (en) * | 2018-04-24 | 2019-07-05 | 湖北工程学院 | A kind of high-energy density lithium battery lithium iron phosphate positive material and preparation method thereof |
| CN109280993A (en) * | 2018-09-03 | 2019-01-29 | 济南大学 | A kind of method of electrostatic spinning technique synthetic silicic acid iron lithium nanofiber |
| CN109280993B (en) * | 2018-09-03 | 2021-03-30 | 济南大学 | Method for synthesizing lithium iron silicate nanofiber by electrostatic spinning technology |
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Application publication date: 20120328 |