CN105680043A - Preparation of nano-ferric fluoride and application of nano-ferric fluoride to positive electrode of high-specific-capacity lithium ion battery - Google Patents
Preparation of nano-ferric fluoride and application of nano-ferric fluoride to positive electrode of high-specific-capacity lithium ion battery Download PDFInfo
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- CN105680043A CN105680043A CN201610054845.8A CN201610054845A CN105680043A CN 105680043 A CN105680043 A CN 105680043A CN 201610054845 A CN201610054845 A CN 201610054845A CN 105680043 A CN105680043 A CN 105680043A
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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
- H01M4/582—Halogenides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
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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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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- 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 relates to preparation of nano-ferric fluoride and an application of the nano-ferric fluoride to a positive electrode of a high-specific-capacity lithium ion battery. A preparation method of the nano-ferric fluoride comprises the following steps: preparing a Fe(NO<3>)<3>.9H<2>O ethanol solution, and obtaining a colorless transparent solution under an ultrasonic action; preparing a deionized water solution of NH<4>HF<2>; mixing the solutions to obtain (NH<4>)<3>FeF<6> white precipitate; performing centrifugal separation on the white precipitate, cleaning the centrifugally-separated white precipitate and drying the cleaned white precipitate to obtain (NH<4>)<3>FeF<6> white powder; and calcining the (NH<4>)<3>FeF<6> white powder to obtain a FeF<3> nanometer material. A positive electrode of a high-specific-power lithium ion battery is prepared from the FeF<3> nanometer material. The preparation method has the advantages of easiness in operation, low cost, high yield, simple posttreatment, no need of any special reaction instrument and low preparation cost. FeF3 nanometer materials of different grain sizes can be obtained in a way of easily regulating and controlling a volume ratio of ethanol to deionized water. The electrode has superior electrochemical performance in the lithium ion battery.
Description
Technical field
The present invention is a kind of preparation closing the iron perchloride method for precursor power nanometer ferric flouride and anode material for lithium-ion batteries thereof with hexafluoro. Exactly hexafluoro being closed iron perchloride pyrolytic in an inert atmosphere specifically is ferric flouride, and be applied in lithium primary cell, belong to energy storage material technical field.
Background technology
Lithium ion battery, as a kind of energy accumulating device, has running voltage height, and specific energy is big, has extended cycle life, and safety is good, and self discharge is little, operating temperature range width and the fast feature of discharge and recharge. At present, lithium ion battery has been widely used in electric automobile, the field such as electrical equipment and back-up source. At present, the lithium-ion battery system capacity of the marketization is close to its theoretical capacity, it is difficult to having breakthrough, therefore the battery active material of development of new is significant.
Ferric flouride causes wide sending out and pays close attention to because of its price with high theoretical capacity, high discharge platform and relative moderate and nontoxic, environmental protection. Compared with traditional fluorinated carbon material, except can by the embedding of lithium ion with deviate to store up lithium except, energy can also be stored with lithium metal generation phase chemical conversion, its essence is exactly formation and the decomposition of lithium fluoride, this kind of reaction can make full use of all of valency electron in material, thus obtaining far above traditional capacity embedding deintercalation formula battery. Its theoretical capacity is up to 712mAh/g, and discharge platform is at about 2.7V.
But in ferric flouride, fluorine atom and iron atom are linked together by ionic bond, cause that its electrical conductivity is relatively low, thus limiting the performance of its high rate performance. Reduce ferric flouride granule particle diameter and with other materials compound be solve this problem important means.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that nanometer ferric flouride/carbon composite that novel preparation size is controlled and method prepared by electrode thereof, the method is simple to operate, quick environmental protection. The advantages such as the ferric flouride material of preparation has good electrical conductivity, has the chemical property of excellence with its electrode material prepared, good cyclical stability, it is adaptable to as lithium ion battery electrode material.
Technical scheme is as follows:
A kind of preparation method of nanometer of ferric flouride material, step is as follows:
(1) preparation Fe (NO3)3·9H2O alcoholic solution, obtains colourless clear solution under ultrasonication;
(2) preparation is by NH4HF2Deionized water solution;
(3) aqueous solution that (2) obtain is poured in the alcoholic solution obtained in (1), obtain (NH4)3FeF6White precipitate;
(4) the white precipitate centrifugation in (3), cleaning, drying are obtained (NH4)3FeF6White powder;
(5) by (NH4)3FeF6White powder calcining obtains FeF3Nano material.
Described preparation Fe (NO3)3·9H2O ethanol solution concentration is 1-5mol/L.
Described NH4HF2With Fe (NO3)3·9H2The mass ratio of the material of O is 1:2-20.
Described the aqueous solution that (2) obtain is poured in the alcoholic solution obtained in (1), and stir 1-5min.
Described step (4) ethanol purge, at 60-80 DEG C, vacuum drying 12-24h, obtains (NH4)3FeF6White powder.
Described calcination condition is at 400 DEG C-700 DEG C, heats 2-5 hour, obtain FeF under inert atmosphere3Nano material.
Utilize FeF3Nano material prepares the method for electrode; Its step is as follows:
(1)FeF3Nano material and acetylene black, Kynoar is blended in arriving in the N-Methyl pyrrolidone of 10ml-20ml according to the mass ratio of 7:2:1 and mixes homogenate;
(2) mix homogenate in planetary ball mill with the rotating speed ball milling 2-5h of 500-700rmp by what obtain, obtain containing FeF3The thickness homogenate of/C composite;
(3) the thickness homogenate obtained is coated on aluminium foil, vacuum drying 6h-12h at 120-150 DEG C, after be cut to the disk that diameter is similar to button cell.
The present invention is simple to operate, and cost is low, and yield is high, and post processing is simple, it is not necessary to special reaction kit, preparation cost is cheap. The FeF of different-grain diameter can be obtained by simply regulating and controlling the volume ratio of ethanol and deionized water3Nano material; It addition, prepared electrode has the chemical property of excellence in lithium ion battery.
Accompanying drawing explanation
Fig. 1: the XRD spectra of nano material;
Fig. 2: nano material has the highest X-ray diffraction intensity;
Fig. 3: the charging and discharging curve of electrode prepared by nano material.
Detailed description of the invention
Below by way of specific embodiment, technical solution of the present invention is illustrated.
Example 1
(1) by the Fe (NO of 0.1mol3)3·9H2O is dissolved in 1L ethanol, and concentration is 1mol, obtains colourless clear solution under ultrasonication.
(2) by the NH of 0.3mol4HF2It is dissolved in 1L deionized water, (NH4)HF2With Fe (NO3)3·9H2The amount of substance of O is than for 20:1.
(3) aqueous solution that (2) obtain is poured in the alcoholic solution obtained in (1), and acutely stir 1min, obtain (NH4)3FeF6White precipitate.
(4) being obtained with centrifugal method by the white precipitate in (3), with ethanol purge three times, at 60 DEG C, vacuum drying 12h, obtains (NH4)3FeF6White powder.
(5) (the NH that will obtain in (4)4)3FeF6White powder at 400 DEG C, heat treated under argon two hours, obtain FeF3Nano material.
It is above FeF3The preparation of nano material.
(6) FeF that will obtain in (5)3Nano material and acetylene black, Kynoar is blended in arriving in the N-Methyl pyrrolidone of 10ml according to the mass ratio of 7:2:1 and mixes homogenate.
(7) mix homogenate in planetary ball mill with the rotating speed ball milling 2h of 500rmp by what (6) obtained, obtain containing FeF3The thickness homogenate of/C composite.
It is above FeF3The preparation process of/C.
(8) the thickness homogenate obtained in (7) is coated on aluminium foil, vacuum drying 6h at 120 DEG C, after will be just the disk of 1cm for diameter.
The XRD spectra of the nano material of example 1 preparation demonstrates and is similar to FeF3The diffraction maximum of crystal structure, it is corresponding to the crystal structure of fluorite class. (as shown in Figure 1).
The XRD spectra of the nano material of the example 1 preparation relatively low diffraction maximum of intensity at 35 ° of places is corresponding to tiltedly side-Fe2O3Impurity, this is due to FeF in thermal decomposition process3Reacting with the water and air of residual and cause, battery performance is disadvantageous by this. (as shown in Figure 1).
The nano material of example 1 preparation has the highest X-ray diffraction intensity, and this illustrates that it has minimum physical dimension, and illustrates that the ratio of change ethanol and water can control the particle diameter of final ferric flouride. (as shown in Figure 2).
The charging and discharging curve of electrode prepared by the nano material of example 1 preparation demonstrates it and has higher capacity, and its first lap capacity is 220mAh/g, and this index is better than existing ferric fluoride anode material. (as shown in Figure 3).
The discharge voltage of the electrode of example 1 preparation is at about 3.0V. (as shown in Figure 3).
The capacity of the electrode of example 1 preparation tends towards stability gradually. (as shown in Figure 3).
Example 2
(1) by the Fe (NO of 0.1mol3)3·9H2O is dissolved in 1L ethanol, and concentration is 2mol, obtains colourless clear solution under ultrasonication.
(2) by the NH of 0.3mol4HF2It is dissolved in 1L deionized water, NH4HF2With Fe (NO3)3·9H2The amount of substance of O is than for 10:1.
(3) aqueous solution that (2) obtain is poured in the alcoholic solution obtained in (1), and acutely stir 1min, obtain (NH4)3FeF6White precipitate.
(4) being obtained with centrifugal method by the white precipitate in (3), with ethanol purge three times, at 60 DEG C, vacuum drying 12h, obtains (NH4)3FeF6White powder.
(5) (the NH that will obtain in (4)4)3FeF6White powder at 400 DEG C, heat treated under argon two hours, obtain FeF3Nano material.
It is above FeF3The preparation of nano material.
(6) FeF that will obtain in (5)3Nano material and acetylene black, Kynoar is blended in arriving in the N-Methyl pyrrolidone of 10ml according to the mass ratio of 7:2:1 and mixes homogenate.
(7) mix homogenate in planetary ball mill with the rotating speed ball milling 2h of 500rmp by what (6) obtained, obtain containing FeF3The thickness homogenate of/C composite.
It is above FeF3The preparation process of/C.
(8) the thickness homogenate obtained in (7) is coated on aluminium foil, vacuum drying 6h at 120 DEG C, after will be just the disk of 1cm for diameter.
Electrode first circle specific capacity prepared by the method is 160mAh/g.
Example 3
(1) by the Fe (NO of 0.1mol3)3·9H2O is dissolved in 1L ethanol, and concentration is 3mol, obtains colourless clear solution under ultrasonication.
(2) by the NH of 0.3mol4HF2It is dissolved in 1L deionized water, NH4HF2With Fe (NO3)3·9H2The amount of substance of O is than for 5:1.
(3) aqueous solution that (2) obtain is poured in the alcoholic solution obtained in (1), and acutely stir 1min, obtain (NH4)3FeF6White precipitate.
(4) being obtained with centrifugal method by the white precipitate in (3), with ethanol purge three times, at 60 DEG C, vacuum drying 12h, obtains (NH4)3FeF6White powder.
(5) (the NH that will obtain in (4)4)3FeF6White powder at 400 DEG C, heat treated under argon two hours, obtain FeF3Nano material.
It is above FeF3The preparation of nano material.
(6) FeF that will obtain in (5)3Nano material and acetylene black, Kynoar is blended in arriving in the N-Methyl pyrrolidone of 10ml according to the mass ratio of 7:2:1 and mixes homogenate.
(7) mix homogenate in planetary ball mill with the rotating speed ball milling 2h of 500rmp by what (6) obtained, obtain containing FeF3The thickness homogenate of/C composite.
It is above FeF3The preparation process of/C.
(8) the thickness homogenate obtained in (7) is coated on aluminium foil, vacuum drying 6h at 120 DEG C, after will be just the disk of 1cm for diameter.
Electrode first circle specific capacity prepared by the method is 185mAh/g.
Example 4
(1) by the Fe (NO of 0.1mol3)3·9H2O is dissolved in 1L ethanol, and concentration is 5mol, obtains colourless clear solution under ultrasonication.
(2) by the NH of 0.3mol4HF2It is dissolved in 1L deionized water, NH4HF2With Fe (NO3)3·9H2The amount of substance of O is than for 2:1.
(3) aqueous solution that (2) obtain is poured in the alcoholic solution obtained in (1), and acutely stir 1min, obtain (NH4)3FeF6White precipitate.
(4) being obtained with centrifugal method by the white precipitate in (3), with ethanol purge three times, at 60 DEG C, vacuum drying 12h, obtains (NH4)3FeF6White powder.
(5) (the NH that will obtain in (4)4)3FeF6White powder at 400 DEG C, heat treated under argon two hours, obtain FeF3Nano material.
It is above FeF3The preparation of nano material.
(6) FeF that will obtain in (5)3Nano material and acetylene black, Kynoar is blended in arriving in the N-Methyl pyrrolidone of 10ml according to the mass ratio of 7:2:1 and mixes homogenate.
(7) mix homogenate in planetary ball mill with the rotating speed ball milling 2h of 500rmp by what (6) obtained, obtain containing FeF3The thickness homogenate of/C composite.
It is above FeF3The preparation process of/C.
(8) the thickness homogenate obtained in (7) is coated on aluminium foil, vacuum drying 6h at 120 DEG C, after will be just the disk of 1cm for diameter.
Electrode first circle specific capacity prepared by the method is 200mAh/g.
The preparation of disclosure and proposition controllable nanon size ferric flouride and the application in height ratio capacity lithium ion cell positive thereof, those skilled in the art can pass through to use for reference present disclosure, suitably change the links such as condition route to realize, although the method for the present invention and technology of preparing have passed through preferred embodiment and are described, methods and techniques described herein route substantially can be modified or reconfigure in without departing from present invention, spirit and scope by person skilled, realizes final technology of preparing. Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are considered as including in present invention spirit, scope and content.
Claims (7)
1. a preparation method for nanometer ferric flouride material, is characterized in that step is as follows:
(1) preparation Fe (NO3)3·9H2O alcoholic solution, obtains colourless clear solution under ultrasonication;
(2) preparation is by NH4HF2Deionized water solution;
(3) aqueous solution that (2) obtain is poured in the alcoholic solution obtained in (1), obtain (NH4)3FeF6White precipitate;
(4) the white precipitate centrifugation in (3), cleaning, drying are obtained (NH4)3FeF6White powder;
(5) by (NH4)3FeF6White powder calcining obtains FeF3Nano material.
2. the method for claim 1, is characterized in that described preparation Fe (NO3)3·9H2O ethanol solution concentration is 1-5mol/L.
3. the method for claim 1, is characterized in that NH4HF2With Fe (NO3)3·9H2The mass ratio of the material of O is 1:2-20.
4. the method for claim 1, is characterized in that described being poured in the alcoholic solution obtained in (1) by the aqueous solution that (2) obtain, and stirs 1-5min.
5. the method for claim 1, is characterized in that described step (4) ethanol purge, and at 60-80 DEG C, vacuum drying 12-24h, obtains (NH4)3FeF6White powder.
6. the method for claim 1, is characterized in that described calcination condition is for, at 400 DEG C-700 DEG C, heating 2-5 hour under inert atmosphere, obtain FeF3Nano material.
7. utilize FeF3Nano material prepares the method for electrode; It is characterized in that step is as follows:
(1)FeF3Nano material and acetylene black, Kynoar is blended in arriving in the N-Methyl pyrrolidone of 10ml-20ml according to the mass ratio of 7:2:1 and mixes homogenate;
(2) mix homogenate in planetary ball mill with the rotating speed ball milling 2-5h of 500-700rmp by what obtain, obtain containing FeF3The thickness homogenate of/C composite;
(3) the thickness homogenate obtained is coated on aluminium foil, vacuum drying 6h-12h at 120-150 DEG C, after be cut to the disk that diameter is similar to button cell.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107634219A (en) * | 2017-07-26 | 2018-01-26 | 昆明理工大学 | A kind of liquid-phase precipitation method synthesis nanometer Fe F3The method of/Ag positive electrodes |
| CN108270003A (en) * | 2018-01-05 | 2018-07-10 | 昆明理工大学 | A kind of liquid phase method synthesizes FeF3The method of/CNTs positive electrodes |
| CN111606358A (en) * | 2020-05-15 | 2020-09-01 | 南京工业大学 | Preparation method of nano ferric fluoride |
| CN112777640A (en) * | 2020-12-30 | 2021-05-11 | 钦州南海化工有限公司 | Method for deeply defluorinating high-purity manganese sulfate |
| CN113224311A (en) * | 2020-12-28 | 2021-08-06 | 中国科学院过程工程研究所 | Multi-fluoride positive electrode material, preparation method thereof and lithium ion battery |
| CN114639827A (en) * | 2022-03-29 | 2022-06-17 | 多氟多新材料股份有限公司 | Preparation method of iron-based fluoride composite positive electrode material |
Citations (1)
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| CN103022483A (en) * | 2012-12-07 | 2013-04-03 | 南京工业大学 | Preparation method for positive electrode material of power lithium ion battery |
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| CN103022483A (en) * | 2012-12-07 | 2013-04-03 | 南京工业大学 | Preparation method for positive electrode material of power lithium ion battery |
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| TING LI ET AL.: "Reversible Three-Electron Redox Behaviors of FeF3 Nanocrystals as High-Capacity Cathode-Active Materials for Li-Ion Batteries", 《J.PHYS.CHEM.C》 * |
| XIN ZHAO ET AL.: "Photothermal-assisted fabrication of iron fluoride–graphene composite paper cathodes for high-energy lithium-ion batteries", 《CHEM.COMMUM.》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107634219A (en) * | 2017-07-26 | 2018-01-26 | 昆明理工大学 | A kind of liquid-phase precipitation method synthesis nanometer Fe F3The method of/Ag positive electrodes |
| CN108270003A (en) * | 2018-01-05 | 2018-07-10 | 昆明理工大学 | A kind of liquid phase method synthesizes FeF3The method of/CNTs positive electrodes |
| CN111606358A (en) * | 2020-05-15 | 2020-09-01 | 南京工业大学 | Preparation method of nano ferric fluoride |
| CN111606358B (en) * | 2020-05-15 | 2022-08-30 | 南京工业大学 | Preparation method of nano ferric fluoride |
| CN113224311A (en) * | 2020-12-28 | 2021-08-06 | 中国科学院过程工程研究所 | Multi-fluoride positive electrode material, preparation method thereof and lithium ion battery |
| CN113224311B (en) * | 2020-12-28 | 2022-10-04 | 中国科学院过程工程研究所 | Multi-fluoride positive electrode material, preparation method thereof and lithium ion battery |
| CN112777640A (en) * | 2020-12-30 | 2021-05-11 | 钦州南海化工有限公司 | Method for deeply defluorinating high-purity manganese sulfate |
| CN114639827A (en) * | 2022-03-29 | 2022-06-17 | 多氟多新材料股份有限公司 | Preparation method of iron-based fluoride composite positive electrode material |
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