CN104600295A - Micron-scale spheroidal ferric fluoride positive electrode material and preparation method thereof - Google Patents
Micron-scale spheroidal ferric fluoride positive electrode material and preparation method thereof Download PDFInfo
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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
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- 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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- 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
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Abstract
The invention specifically relates to a micron-scale spheroidal ferric fluoride positive electrode material and a preparation method thereof. The micron-scale spheroidal ferric fluoride positive electrode material is prepared from a water/alcohol mixed solution of a ferric salt and a fluorine-containing aqueous solution. The preparation method is performed at a normal temperature and under a normal pressure, the preparation process is simple, the consuming time is short, the energy consumption is low, the cost is low, the environment-friendly effect is achieved, and the industrial production can be realized easily; the prepared FeF3(H2O)0.33 particles are spheroidal at the micron scale; the tap density of the material is improved; the material has excellent mobility, dispersibility and machinability, and is applicable to producing a positive electrode material slurry and coating an electrode plate; meanwhile, the material has a one-dimensional tunnel structure and is beneficial to the migration of lithium ions, so that the electrical conductivity of the material can be improved; in addition, the stability of the FeF3 structure is maintained in the charging/discharging process by use of little crystal water, and therefore, good electrochemical properties can be realized.
Description
(1) technical field
The present invention relates to lithium ion secondary battery anode material, be specifically related to a kind of micron level spherical ferric fluoride anode material and preparation method thereof.
(2) background technology
Society, to the demand of the energy, facilitates the development of energy storage technology greatly.Lithium ion battery has developed very swift and violent Novel energy storage apparatus since 1990, there is the advantages such as high-energy-density, high open circuit voltage, long circulation life, memory-less effect and non-environmental-pollution, establish unrivaled dominant advantage in portable type electronic product fields such as mobile phone, notebook computer, digital cameras, and actively develop to electric tool, electric automobile, UPS equipment and national defence.
Lithium ion battery is primarily of compositions such as positive and negative pole material, electrolyte, barrier films, and wherein positive electrode is in occupation of most important status, directly affects the important performances such as the capacity of battery, life-span, cost, fail safe.Because the electronegativity of fluorine is large, the operating voltage of metal fluoride positive electrode is far above other positive electrodes such as metal oxide, metal sulfide.This reversible chemical conversioning reaction can make full use of the various oxidation state of material in oxidation-reduction process, electronics all in exchange material, and its capacity of releasing is far away higher than the Lithium-ion embeding on traditional outline/deintercalation reaction.Equal within 1997, to propose transition metal fluorides as after the positive electrode of lithium rechargeable battery from Kyoto Univ Japan Arai, on U.S. MRS autumn sessions in 2002 and first international energy Conversion Project meeting in 2003, professor Amatucci again proposes metal fluoride and is used as lithium ion secondary battery anode material, has again caused the upsurge of metal fluoride positive electrode research.FeF
3because it has high, with low cost, the eco-friendly advantage of specific capacity, be considered to the anode material for lithium-ion batteries of new generation having researching value and application prospect.
FeF prepared by domestic and international research
3material is mostly R-3C space group, belongs to ReO
3crystal formation, hexagonal system structure, its shortcoming is that electric conductivity is poor, and specific discharge capacity is low, and cycle performance is poor.At present mainly by FeF
3improve its electric conductivity with electric conducting material (as graphite, carbon black, active carbon etc.) mixing and ball milling.AmatucciG.G etc. are by the nanometer Fe F of preparation carbon coated
3/ C composite improves FeF
3electric conductivity, but its cycle performance still can not get improve.Badway F etc. has prepared FeF by the method for high-energy ball milling
3base nano-sized carbon metallic composite, in the voltage range of 2.8-3.4V, its capacity is up to 200mAh/g.Korea S Kang teach problem group adopts liquid phase method at the upper growth in situ FeF of carbon nano-tube (CNT)
3nanometer flowers, obtain CNT-FeF
3nano composite material, this material within the scope of 2.0-4.5V, with 20mA/g discharge and recharge, first discharge specific capacity is up to 210mAh/g, and material circulation better performances but its cycle-index is less, only has 30 weeks and the cost of raw material is higher, complicated process of preparation, the more difficult control of grain diameter growth.
In recent years, the FeF of rhombic system that had researcher to prepare
3(H
2o)
0.33material, a small amount of crystallization water contributes to improving the chemical property of material the relatively stable of holding structure and obtaining good cycle performance.CN:101222037A discloses a kind of preparation method of lithium secondary battery drop water ferric fluoride anode material.2011, Maier seminar for template introduces the Single Walled Carbon Nanotube (SWNT) of 5wt.% at low temperatures, formed SWNT/FeF with BmimBF4 ionic liquid
30.33H
2o composite material improves the conductivity of ferric flouride material further, and make material obtain better chemical property, first discharge specific capacity is up to 220mAh/g, but cycle performance is poor, and the capability retention after 50 times that circulates is 66%.
FeF
3the key of application solves its technology of preparing complexity and a difficult problem for the harsh length consuming time of condition, and improve its chemical property (conductivity, cyclicity and specific discharge capacity).At present, FeF
3preparation be obtained by anhydrous hydrofluoric acid or fluorine and ferric chloride reaction, or iron oxide at high temperature reacts obtained with hydrogen fluoride gas.And improve conductivity also mainly by improving its electric conductivity with electric conducting material (as graphite, carbon black, active carbon etc.) mixing and ball milling, fail its chemical property of radical change from structure and pattern.The positive electrode homogeneity of such preparation is poor, time consumption and energy consumption, and environmental pollution is large, and the higher and complex process of product pattern noncontrollable cost, is not used in suitability for industrialized production.
(3) summary of the invention
The object of the invention is for positive electrode FeF
3there is the problem that preparation process condition complexity is harsh, energy consumption is high, chemical property is poor, provide a kind of micron level spherical ferric fluoride anode material and preparation method thereof, this micron level spherical ferric fluoride anode material (FeF
3(H
2o)
0.33positive electrode) there is spherical morphology and excellent electrochemical performance, required reaction condition is gentle, and low cost, is easy to suitability for industrialized production.
The present invention is achieved through the following technical solutions:
A kind of micron level spherical ferric fluoride anode material, its special character is: be prepared from by the water/mixed alkoxide solution of molysite and aqueous solution containing fluoride.
A preparation method for micron level spherical ferric fluoride anode material described in basis, is characterized in that: comprise the following steps:
(1) at normal temperatures, the water/mixed alkoxide solution of preparation molysite, iron salt concentration is 0.5 ~ 0.6mol/L, then adds 0.02 ~ 0.025mol surfactant wherein, and wherein water and alcohol volume ratio are 1:1; The aqueous solution that fluoro-containing concentration is 1mol/L is prepared by the mol ratio 1:3 of iron ion and fluorine ion;
(2) joined respectively in the 150ml water/alcoholic solution containing 0.0055 mol/L dispersant by two kinds of solution in step (1), wherein water and alcohol volume ratio are 1:1, and two kinds of solution are ultrasonic respectively;
(3) at the uniform velocity stir after again two kinds of solution being mixed at normal temperatures and pressures;
(4) fully centrifugation after reaction, outwells supernatant, and with absolute ethyl alcohol repeatedly washing precipitate;
(5) sediment after washing is dry at 60-80 DEG C, obtain powder sample FeF
3(H
2o)
0.33.
The preparation method of micron level spherical ferric fluoride anode material of the present invention, described molysite is Fe (NO
3)
39H
2o, FeCl
36H
2one in O.
The preparation method of micron level spherical ferric fluoride anode material of the present invention, described alcohol is the one in ethanol, ethylene glycol.
The preparation method of micron level spherical ferric fluoride anode material of the present invention, described surfactant is the one in oleic acid, octadecylamine.
The preparation method of micron level spherical ferric fluoride anode material of the present invention, described fluorine-containing material is the one in ammonium fluoride, ammonium acid fluoride.
The preparation method of micron level spherical ferric fluoride anode material of the present invention, dispersant is polyethylene glycol, and its molecular weight is 20000.
Beneficial effect: this preparation method carries out at normal temperatures and pressures, preparation technology is simple, and consuming time short, and energy consumption is low, with low cost, and environmental friendliness is easy to suitability for industrialized production; The FeF of preparation
3(H
2o)
0.33particle is that micron is spherical, improve the tap density of material, there is excellent mobility, dispersiveness, processability, be conducive to the coating making positive electrode slurry and electrode slice, this material tool one dimension tunnel structure is conducive to the migration of lithium ion simultaneously, add the conductivity of material, and a small amount of crystallization water maintains FeF in charge and discharge process
3stablizing, to realize good chemical property of structure.Compared to the method describing synthesis ferric flouride in CN 103151523A, this method has preparation condition gentleness, carries out at normal temperatures and pressures and the reaction time is short, energy consumption is low and be easy to the advantages such as industrialization.FeF
3(H
2o)
0.33discharge and recharge under 0.6C, first discharge specific capacity reaches 227.1 mAh/g, and close to theoretical capacity 237 mAh/g, after circulating 100 weeks, its specific discharge capacity is 167.2mAh/g; Under 1C, its first all specific discharge capacity of discharge and recharge still can reach 186.6 mAh/g, and after circulating 100 weeks, its capacity still can reach 141.6 mAh/g; Even if its first all specific discharge capacity of discharge and recharge still can reach 170.5 mAh/g under high magnification 2C, after circulating 100 weeks, its capacity still can reach 124.0 mAh/g, and capability retention is 72.7%, and its high rate performance is excellent.Comprehensive electrochemical is much better than the ferric fluoride anode material described in CN101222037A and US20040121235A1, is also better than the standby FeF of Maier project team system simultaneously
3(H
2o)
0.33(Maier et al., 2011).In addition, spherical product has higher bulk density and then improves the energy density of battery, and moreover spherical product has excellent mobility, dispersiveness, processability, is conducive to the coating making positive electrode slurry and electrode slice.FeF prepared in addition
3(H
2o)
0.33material does not need to obtain excellent chemical property with conductive agent (as material with carbon elements such as acetylene blacks) compound, and especially large high rate performance, has actual application prospect at electrokinetic cell and high-energy density type field of batteries.
(4) accompanying drawing explanation
The FeF that figure mono-is prepared for the present invention
3(H
2o)
0.33scanning electron microscope (SEM) photograph;
The FeF that figure bis-is prepared for the present invention
3(H
2o)
0.33x-ray diffraction spectrogram;
The FeF that figure tri-is prepared for the present invention
3(H
2o)
0.33for positive electrode, lithium sheet is negative material, is assembled into button cell, at room temperature with 0.6C, 1C and 2.0C multiplying power, and the cycle life curve in the voltage range of 2.0-4.5V.
(5) embodiment
Embodiment 1:
Preparing 40 mL concentration is 0.5 mol/L ferric nitrate (Fe (NO
3)
39H
2o) water/alcohol mixed solution (volume ratio of water and ethanol is 1:1), and add 0.02mol oleic acid wherein; 1:3 prepares 20 mL concentration is in molar ratio 1mol/L ammonium fluoride aqueous solution, then two kinds of solution being joined respectively 150 mL concentration is in the ethanolic solution of 0.0055 mol/L polyethylene glycol (molecular weight 20000), two kinds of solution ultrasonic 30min respectively, again by two kinds of solution mixing, under normal temperature and pressure, at the uniform velocity stir 2 h.Centrifugally outwell supernatant, and with ethanol cyclic washing sediment repeatedly, after 60 DEG C of dry 8h, obtain pure phase product FeF
3(H
2o)
0.33.
Embodiment 2:
Preparing 40 mL concentration is respectively 0.6 mol/L iron chloride (FeCl
36H
2o) water/ethanolic solution (volume ratio of water and ethanol is 1:1), and add 0.025mol oleic acid wherein; 1:3 prepares 24mL concentration is in molar ratio the 1mol/L ammonium acid fluoride aqueous solution, then two kinds of solution being joined respectively 150mL concentration is in 0.0055 mol/L polyethylene glycol (molecular weight 20000) ethanolic solution, two kinds of solution ultrasonic 30min respectively, again by two kinds of solution mixing, under normal temperature and pressure, at the uniform velocity stir 4 h.Centrifugally outwell supernatant, and with ethanol cyclic washing sediment repeatedly, after 60 DEG C of dry 12h, obtain pure phase product FeF
3(H
2o)
0.33.
Embodiment 3:
Preparing 40 mL concentration is 0.5 mol/L ferric nitrate (Fe (NO
3)
39H
2o) water/ethylene glycol mixed solution (volume ratio of water and ethylene glycol is 1:1), and add 0.02mol octadecylamine wherein; 1:3 prepares 20 mL concentration is in molar ratio 1mol/L ammonium fluoride aqueous solution, then two kinds of solution being joined respectively 150mL concentration is in the ethanolic solution of 0.0055 mol/L polyethylene glycol (molecular weight 20000), two kinds of solution ultrasonic 10min respectively, again by two kinds of solution mixing, under normal temperature and pressure, at the uniform velocity stir 2 h.Centrifugally outwell supernatant, and with ethanol cyclic washing sediment repeatedly, after 60 DEG C of dry 8h, obtain pure phase product FeF
3(H
2o)
0.33.
Embodiment 4:
Preparing 40 mL concentration is respectively 0.6 mol/L iron chloride (FeCl
36H
2o) water/ethylene glycol solution (volume ratio of water and ethylene glycol is 1:1), and add 0.025mol octadecylamine wherein; 1:3 prepares 24mL concentration is in molar ratio the 1mol/L ammonium acid fluoride aqueous solution, then two kinds of solution being joined respectively 150mL concentration is in 0.0055 mol/L polyethylene glycol (molecular weight 20000) ethanolic solution, two kinds of solution ultrasonic 20min respectively, again by two kinds of solution mixing, under normal temperature and pressure, at the uniform velocity stir 4 h.Centrifugally outwell supernatant, and with ethanol cyclic washing sediment repeatedly, after 60 DEG C of dry 12h, obtain pure phase product FeF
3(H
2o)
0.33.
Embodiment 5:
Preparing 40 mL concentration is 0.5 mol/L ferric nitrate (Fe (NO
3)
39H
2o) water/alcohol mixed solution (volume ratio of water and ethanol is 1:1), and add 0.02mol oleic acid wherein; 1:3.5 prepares 20 mL concentration is in molar ratio 1mol/L ammonium fluoride aqueous solution, then two kinds of solution being joined respectively 150 mL concentration is in the ethanolic solution of 0.0055 mol/L polyethylene glycol (molecular weight 20000), two kinds of solution ultrasonic 10min respectively, again by two kinds of solution mixing, then add ether 30ml, under normal temperature and pressure, at the uniform velocity stir 10min.Centrifugally outwell supernatant, and with ethanol: ether be the mixed liquor cyclic washing sediment of 1:1.2 repeatedly, after 60 DEG C of dry 20min, obtain pure phase product FeF
3(H
2o)
0.33.
The present embodiment is shorter compared with other embodiment processing times.
As shown in Figure 1, the FeF prepared by the present invention
3(H
2o)
0.33granule-morphology rule be micron level spherical, and particle dispersion is good, does not reunite.
As shown in Figure 2, the FeF prepared by the present invention
3(H
2o)
0.33x-ray diffraction spectrogram shows it, and without mixing, it exists mutually.
As shown in Figure 3, prepared FeF
3(H
2o)
0.33as positive electrode, lithium is negative material, assembling button cell, at voltage window 2.0-4.5 V, and cycle life curve under 0.6C, 1C and 2C multiplying power.FeF
3(H
2o)
0.33discharge and recharge under 0.6C, first discharge specific capacity reaches 227.1 mAh/g, and close to theoretical capacity 237 mAh/g, after circulating 100 weeks, its specific discharge capacity is 167.2mAh/g; Under 1C, its first all specific discharge capacity of discharge and recharge still can reach 186.6 mAh/g, and after circulating 100 weeks, its capacity still can reach 141.6 mAh/g; Even if its first all specific discharge capacity of discharge and recharge still can reach 170.5 mAh/g under high magnification 2C, after circulating 100 weeks, its capacity still can reach 124.0 mAh/g, and capability retention is 72.7%.
Claims (7)
1. a micron level spherical ferric fluoride anode material, is characterized in that: be prepared from by the water/mixed alkoxide solution of molysite and aqueous solution containing fluoride, and the ferric flouride pattern of preparation is micron level spherical.
2. a preparation method for micron level spherical ferric fluoride anode material according to claim 1, is characterized in that: comprise the following steps:
(1) at normal temperatures, the water/mixed alkoxide solution of preparation molysite, iron salt concentration is 0.5 ~ 0.6mol/L, then adds 0.02 ~ 0.025mol surfactant wherein, and wherein water and alcohol volume ratio are 1:1; The aqueous solution that fluoro-containing concentration is 1mol/L is prepared by the mol ratio 1:3 of iron ion and fluorine ion;
(2) joined respectively in the 150ml water/alcoholic solution containing 0.0055 mol/L dispersant by two kinds of solution in step (1), wherein water and alcohol volume ratio are 1:1, and two kinds of solution are ultrasonic respectively;
(3) at the uniform velocity stir after again two kinds of solution being mixed at normal temperatures and pressures;
(4) fully centrifugation after reaction, outwells supernatant, and with absolute ethyl alcohol repeatedly washing precipitate;
(5) sediment after washing is dry at 60-80 DEG C, obtain powder sample FeF
3(H
2o)
0.33.
3. the preparation method of micron level spherical ferric fluoride anode material according to claim 2, is characterized in that: described molysite is Fe (NO
3)
39H
2o, FeCl
36H
2one in O.
4. the preparation method of the micron level spherical ferric fluoride anode material according to Claims 2 or 3, is characterized in that: described alcohol is the one in ethanol, ethylene glycol.
5. the preparation method of the micron level spherical ferric fluoride anode material according to Claims 2 or 3, is characterized in that: described surfactant is the one in oleic acid, octadecylamine.
6. the preparation method of the micron level spherical ferric fluoride anode material according to Claims 2 or 3, is characterized in that: described fluorine-containing material is the one in ammonium fluoride, ammonium acid fluoride.
7. the preparation method of the micron level spherical ferric fluoride anode material according to Claims 2 or 3, is characterized in that: dispersant is polyethylene glycol, and its molecular weight is 20000.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025182A (en) * | 2016-08-03 | 2016-10-12 | 广东工业大学 | Titanium and chromium doped iron fluoride-carbon nanometer composite positive electrode material, and preparation method and application thereof |
| CN110554078A (en) * | 2019-09-27 | 2019-12-10 | 溧阳天目先导电池材料科技有限公司 | Method for detecting LATP (LATP) of solid electrolyte lithium titanium aluminum phosphate |
| CN113321243A (en) * | 2021-05-25 | 2021-08-31 | 常州赛得能源科技有限公司 | Lithium ion battery anode material with flower-shaped structure, preparation method and application |
-
2014
- 2014-12-31 CN CN201410846354.8A patent/CN104600295A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025182A (en) * | 2016-08-03 | 2016-10-12 | 广东工业大学 | Titanium and chromium doped iron fluoride-carbon nanometer composite positive electrode material, and preparation method and application thereof |
| CN106025182B (en) * | 2016-08-03 | 2019-05-10 | 广东工业大学 | A kind of titanium chromium doping ferric flouride-carbon nano composite anode material and its preparation method and application |
| CN110554078A (en) * | 2019-09-27 | 2019-12-10 | 溧阳天目先导电池材料科技有限公司 | Method for detecting LATP (LATP) of solid electrolyte lithium titanium aluminum phosphate |
| CN110554078B (en) * | 2019-09-27 | 2022-02-22 | 溧阳天目先导电池材料科技有限公司 | Method for detecting LATP (LATP) of solid electrolyte lithium titanium aluminum phosphate |
| CN113321243A (en) * | 2021-05-25 | 2021-08-31 | 常州赛得能源科技有限公司 | Lithium ion battery anode material with flower-shaped structure, preparation method and application |
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