CN104332625A - Cobalt ferrite-nitrogen doped carbon composite negative electrode material for dynamic lithium battery and preparation method thereof - Google Patents
Cobalt ferrite-nitrogen doped carbon composite negative electrode material for dynamic lithium battery and preparation method thereof Download PDFInfo
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- CN104332625A CN104332625A CN201410427176.5A CN201410427176A CN104332625A CN 104332625 A CN104332625 A CN 104332625A CN 201410427176 A CN201410427176 A CN 201410427176A CN 104332625 A CN104332625 A CN 104332625A
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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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
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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
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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 discloses a cobalt ferrite-nitrogen doped carbon composite negative electrode material for dynamic lithium battery and a preparation method thereof. The negative electrode material is composed of cobalt ferrite nano particles which are coated by nitrogen-doped carbon. The particle size of the negative electrode material is 20 to 50 nm, the thickness of the nitrogen-doped carbon is 2.5 to 3.5 nm, the CoFe2O4 content is 65.2 wt%, the FeCo content is 19.7 wt%, the Co content is 4.6 wt%, and the nitrogen doped carbon content is 10.54 wt%. The preparation method comprises the following steps: placing cobalt ferrite powder into a high pressure reactor, dropwise adding an organic carbon source to soak the powder; sealing the reactor, placing the sealed reactor into a resistor furnace, heating to a temperature of 450 to 600 DEG C, maintaining the temperature for 4 to 8 hours; and washing the reaction products after the furnace cools down so as to obtain the composite negative electrode material. Because the nitrogen doped carbon layer has an effective buffering function and an electro-conductive property, the obtained cobalt ferrite-nitrogen doped carbon composite negative electrode material has better electrode integrity and a smoother electrode kinetic property than those of the pure cobalt ferrite negative electrode, and the provided material has excellent cycling stability and capacity recovering performance. Moreover, the preparation method of the composite material is simple and is easy for massive production.
Description
Technical field
The present invention relates to a kind of cobalt ferrite negative material and preparation method thereof, particularly a kind of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material and preparation method.
Background technology
Along with flourish from miniaturized electronics to electric motor car of lithium ion battery, have higher requirement to its portability and energy density in market, existing business negative material-graphite has obviously been difficult to satisfied such requirement, for this reason, the researchers of various countries are proposed plurality of replaceable negative material, these materials can be divided into insert type, alloy-type and conversion hysteria three class storage lithium mechanism.Insert type negative pole has good cyclical stability, but the lower (TiO of capacity
2and Li
4ti
5o
12reversible capacity respectively lower than 250 and 175mAh/g), be unfavorable for the realization of lithium ion cell high-capacity and power density.The theoretical capacity of alloy-type negative electrodes high (Si and SnO2 be respectively 4200 and 1495mAh/g), but there is huge change in volume in structure cell in alloy ~ removal alloying process, this will make active material break, pulverize, final disengaging collector, causes capacity to be decayed rapidly, although effectively can alleviate change in volume with methods such as carbon-based material compounds, improve cyclical stability, fail safe remains the application bottleneck of alloy-type negative electrodes.2000, the electrochemistry performance of a series of transition metal oxide negative pole of Poizot reported first, thus pulled open the prelude of conversion hysteria negative pole research, compared to alloy-type, conversion hysteria negative pole can show the capacity far above graphite cathode equally, and change in volume in charge and discharge process is lower, better fail safe can be realized, therefore be more suitable for following lithium electricity market.From the angle of practicality and cost, the metal oxides of First Transition system is the conversion hysteria negative material of most potentiality, wherein, tri-iron tetroxide and cobaltosic oxide two class low cost, high power capacity, the inverse spinel material that synthesis controllability is high is the lithium electricity potentiality negative pole being well suited for Synthesis and applications, also therefore becomes the study hotspot of lithium electrician authors.
Ternary spinel-type cobalt negative pole combines the advantage of cobaltosic oxide and tri-iron tetroxide, high electrochemical activity (theoretical capacity is up to 914mAh/g) is achieved while reducing costs, and making electrode more stable owing to introducing diversified element, is therefore the very promising lithium cell negative pole material of one equally.The same with binary oxide, the main method overcoming this ternary oxide electrodes collapse and capacity fade problem with carbon-based material compound, cobalt ferrite/the carbon nano-tube had been reported, the composite negative poles such as cobalt ferrite/Graphene all have good cyclical stability and multiplying power performance, but the preparation technology of these compounds consuming time and be difficult to control, carbon source cost used is too high, is difficult to popularize.In addition, because N doping introduces more storage lithium position, and further increase the conductivity of carbon, nitrogen-doped carbon material has better electrochemistry to show than pure carbon, therefore, exploitation is a kind of simple, and the cobalt ferrite/nitrogen carbon dope composite negative pole production technology being easy to realize is the key realizing the cobalt ferrite industrialization of lithium-ion-power cell high power capacity and popularization and application at present.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the invention provides a kind of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material and preparation method, gained composite particles is tiny, evenly, particle diameter is at 20 ~ 50nm, and achieve good nitrogen carbon dope covered effect, show excellent circulation and capacity restorability.
For realizing above-mentioned technical purpose, the present invention is achieved through the following technical solutions:
A kind of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material, formed by the coated cobalt ferrite nano particle of nitrogen carbon dope, the particle diameter of this negative material is 20 ~ 50nm, and it is 2.5 ~ 3.5nm (preferred 3nm), wherein CoFe that nitrogen mixes agraphitic carbon layer thickness
2o
4, FeCo, Co, N content of mixing C is respectively 65.2,19.7,4.6 and 10.54wt%.
The preparation method of above-mentioned dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material, comprises the following steps:
(1) by 150 ~ 200 object cobalt ferrite powder, be placed in autoclave, drip organic carbon source subsequently and infiltrate powder, the volume ratio of described cobalt ferrite powder quality and organic carbon source is (0.5 ~ 2.0): (0.1 ~ 1.5);
(2) reactor sealing is placed in resistance furnace, under 450 ~ 600 DEG C of (preferably 500 DEG C) conditions, is incubated 4 ~ 8h (preferred 6h); (3) after stove cooling, cleaning (preferably using ethanol) product, obtains nanoscale cobalt ferrite ~ nitrogen carbon dope composite negative pole material.
Described organic carbon source is that the one or more than one in pyrroles, pyridine, thiophene mixes with arbitrary proportion.
The preparation method of above-mentioned cobalt ferrite powder, comprises the steps:
(1) by cobalt source and source of iron soluble in water, wherein the concentration of cobalt ions is 0.1 ~ 1M, and the concentration of iron ion is 0.2 ~ 2M;
(2) add the reaction of isopyknic alkaline sodium solution in above-mentioned solution after, by water cleaning gained precipitation, precipitation is placed at 40 ~ 60 DEG C (preferably 50 DEG C) dry 15 ~ 30h (preferred 24h), the concentration of described alkaline sodium solution is 0.8 ~ 9M; Preferably in above-mentioned solution, dropwise add isopyknic alkaline sodium solution while stirring, after vigorous stirring 5 ~ 15min (preferred 10min), gained precipitate with deionized water is cleaned, then at 50 DEG C of dry 24h.
(3) dried above-mentioned precipitation is placed in Muffle furnace, under 350 ~ 600 DEG C of (preferably 450 DEG C) conditions, keeps 4 ~ 8h (preferred 6h), obtain the block cobalt ferrite of black;
(4) grinding of gained cobalt ferrite is sieved, obtain cobalt ferrite powder.
Described cobalt source is cobalt chloride, cobaltous sulfate, and one or more in cobalt acetate mix with arbitrary proportion.
Described source of iron is iron chloride, ferric nitrate, ferrous sulfate, ferrous sulfate amine, the one in frerrous chloride more than one mix with arbitrary proportion.
Described alkaline sodium is sodium carbonate, NaOH, and one or more in sodium acetate mix with arbitrary proportion.
The preferred deionized water of the water used in above-mentioned reaction.
The beneficial effect mistake that the present invention produces: gained dynamic lithium battery cobalt ferrite of the present invention-nitrogen carbon dope composite negative pole material particle is tiny, evenly, particle diameter is at 20 ~ 50nm, and achieve good nitrogen carbon dope covered effect, because N mixes effective cushioning effect and the conductivity of C layer, gained cobalt ferrite of the present invention-nitrogen carbon dope composite negative pole shows better electrode integrality and electrode kinetics more smoothly than pure cobalt ferrite negative pole, thus show excellent cyclical stability and capacity restorability, 0.1C circulates the 646.2mAh/g that still can to discharge after 80 times, after 0.2 ~ 2C high rate cyclic 120 times, capacity still can return to 662.8mAh/g.
This composite material and preparation method thereof is simple; be easy to large-scale production, as lithium cell negative pole, show excellent specific capacity, cyclical stability and capacity restorability; efficiently solving the problem of conventional graphite negative pole low capacity and bulk density, is a kind of lithium cell negative pole substitution material of great potential.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of embodiment 1 gained nanoscale cobalt ferrite-nitrogen carbon dope composite negative pole material;
Fig. 2 be embodiment 1 gained nanoscale cobalt ferrite-nitrogen carbon dope composite negative pole material transmission electron microscope picture;
Fig. 3 is circulation and the rate capability performance of embodiment 1 gained nanoscale cobalt ferrite-nitrogen carbon dope composite negative pole (CFO/NC);
Fig. 4 is circulation and the rate capability performance of pure cobalt ferrite negative pole (CFO).
Embodiment
Embodiment 1
Take 3.1293g CoSO
47H
2o and 5.5600g FeSO
47H
2o is dissolved in 100ml deionized water.In above-mentioned solution, dropwise add the sodium hydroxide solution of isopyknic 0.8M while stirring, after vigorous stirring 10min, gained precipitate with deionized water suction filtration cleans, then at 50 DEG C of dry 24h.The precipitation of gained drying is placed in Muffle furnace, at 500 DEG C, is incubated 6h, obtain the block cobalt ferrite of black.The block cobalt ferrite of grinding black crosses 200 mesh sieves, obtains cobalt ferrite powder.Take above-mentioned 1.0g cobalt ferrite powder and be placed in 30ml stainless steel autoclave, drip 0.25ml pyrroles subsequently by powder complete wetting.Reactor sealing be placed in resistance furnace, 600 DEG C insulation 4h, until stove cooling after, by products therefrom with ethanol purge once, obtain cobalt ferrite-nitrogen carbon dope compound.Fig. 1 is visible, except CoFe
2o
4peak outside, CFO/NC also shows three obvious FeCo peaks (2 θ=45,65.5 and 83 °) and two more weak Co peaks (2 θ=44,51.2 °), and this shows CoFe
2o
4be partially reduced in the coated process of carbon.Based on peak shape matching, elementary analysis and make earnest efforts analyzing the result of three, CoFe in compound
2o
4, the content of FeCO, Co and N carbon dope can be estimated as 65.2 respectively, and 19.7,4.6 and 10.54wt%.Fig. 2 is visible, and compound features goes out good carbon covered effect, and nano particle is completely wrapped in reticulated carbon material, and these carbon are close to particle surface or between particles dispersed; Fig. 3 is visible, pure CoFe
2o
4capacity with circulation rapidly decay, less than 150mAh g after 80 times
-1, on the contrary, CFO/NC is at the 10th circulation retained storage capacity 740mAh g
-1, after 80 times, possess 646.2mAh g
-1, show more than the stable circulation ability of CFO.Fig. 4 is visible, and after 10 0.1C, CFO/NC capacity in follow-up each circulation keeps stablizing and having up-trend, 0.2,0.4,0.8 and 1.6C the 15th discharge capacity be respectively 595,425.9,292.1 and 188.2mAh g
-1.After multiplying power is down to 0.1C, capacity can return to retained storage capacity 662.8mAh g after 95%, 80 different multiplying circulation of 0.1C capacity first
-1, show good capacity restorability.
Embodiment 2
Take 23.7933g CoCl
26H
2o and 54.0680g FeCl
36H
2o is dissolved in 100ml deionized water, dropwise adds the sodium carbonate liquor of isopyknic 4.5M while stirring in above-mentioned solution, and after vigorous stirring 10min, gained precipitate with deionized water is cleaned repeatedly, then at 40 DEG C of dry 30h.The precipitation of gained drying is placed in Muffle furnace, at 450 DEG C, is incubated 8h, obtain the block cobalt ferrite of black.The block cobalt ferrite of the black that hand-ground obtains crosses 250 mesh sieves, obtains cobalt ferrite powder.Take 2g cobalt ferrite powder and be placed in 200ml stainless steel autoclave, drip 1.5ml pyridine subsequently by powder complete wetting.Reactor sealing be placed in resistance furnace, 500 DEG C insulation 6h, until stove cooling after, by products therefrom with ethanol purge once, obtain cobalt ferrite-nitrogen carbon dope compound.
Embodiment 3
Take 12.4467g Co (CH
3cOO)
24H
2o and 40.4000g Fe (NO
3)
39H
2o is dissolved in 100ml deionized water, in above-mentioned solution, dropwise add the sodium acetate solution of isopyknic 9M while stirring, after vigorous stirring 15min, gained precipitate with deionized water is cleaned, then at 60 DEG C of dry 15h.The presoma of gained drying is placed in Muffle furnace, at 350 DEG C, is incubated 8h, obtain the block cobalt ferrite of black.The block cobalt ferrite of the black that grinding obtains crosses 150 mesh sieves, obtains cobalt ferrite powder.Take 1.2g cobalt ferrite powder and be placed in 100ml stainless steel autoclave, drip 0.5ml thiophene subsequently by powder complete wetting.Reactor sealing be placed in resistance furnace, 450 DEG C insulation 8h, until stove cooling after, by products therefrom with ethanol purge once, obtain cobalt ferrite-nitrogen carbon dope compound.
With accompanying drawing, the specific embodiment of the present invention is described although above-mentioned in conjunction with the embodiments; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (9)
1. dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material, is characterized in that, is formed by the coated cobalt ferrite nano particle of nitrogen carbon dope, and the particle diameter of described negative material is 20 ~ 50nm, and nitrogen carbon dope thickness is 2.5 ~ 3.5nm, wherein CoFe
2o
4, FeCo, Co, N content of mixing C is respectively 65.2,19.7,4.6 and 10.54wt%.
2. dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claim 1, it is characterized in that, described nitrogen carbon dope thickness is 3nm.
3. the preparation method of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claim 1, is characterized in that, comprise the following steps:
(1) by 150 ~ 200 object cobalt ferrite powder, be placed in autoclave, drip organic carbon source and infiltrate powder, the volume ratio of described cobalt ferrite powder quality and organic carbon source is (0.5 ~ 2.0): (0.1 ~ 1.5), and described organic carbon source is that the one or more than one in pyrroles, pyridine, thiophene mixes with arbitrary proportion;
(2) reactor sealing is placed in resistance furnace, under 450 ~ 600 DEG C of conditions, is incubated 4 ~ 8h;
(3) after stove cooling, wash products, obtains nanoscale cobalt ferrite ~ nitrogen carbon dope composite negative pole material.
4. the preparation method of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claim 3, is characterized in that, described step 2) in be incubated 6h under 500 DEG C of conditions.
5. the preparation method of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claim 3, is characterized in that, described step 3) in use ethanol purge product.
6. the preparation method of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claim 3, it is characterized in that, the preparation method of described cobalt ferrite powder, comprises the steps:
(1) by cobalt source and source of iron soluble in water, wherein the concentration of cobalt ions is 0.1 ~ 1M, the concentration of iron ion is 0.2 ~ 2M, described cobalt source is that one or more in cobalt chloride, cobaltous sulfate, cobalt acetate mix with arbitrary proportion, and described source of iron is that one or more in iron chloride, ferric nitrate, ferrous sulfate, ferrous sulfate amine, frerrous chloride mix with arbitrary proportion;
(2) in step 1) solution in add isopyknic alkaline sodium solution reaction after, by water cleaning gained precipitation, precipitation is placed at 40 ~ 60 DEG C of drying 15 ~ 30h, described alkaline sodium is that one or more in sodium carbonate, NaOH, sodium acetate mix with arbitrary proportion, and the concentration of described alkaline sodium solution is 0.8 ~ 9M;
(3) dried above-mentioned precipitation is placed in Muffle furnace, under 350 ~ 600 DEG C of conditions, keeps 4 ~ 8h, obtain the block cobalt ferrite of black;
(4) grinding of gained cobalt ferrite is sieved, obtain cobalt ferrite powder.
7. the preparation method of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claim 6, it is characterized in that, described step 2) be specially: while stirring in step 1) dropwise add isopyknic alkaline sodium solution in gained solution, after vigorous stirring 5 ~ 15min, by water suction filtration cleaning gained precipitation, then at 50 DEG C of dry gained precipitation 24h.
8. the preparation method of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claim 6, is characterized in that, described step 3) under 450 DEG C of conditions, keep 6h.
9. the preparation method of dynamic lithium battery cobalt ferrite-nitrogen carbon dope composite negative pole material as claimed in claims 6 or 7, it is characterized in that, described water is deionized water.
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| CN106783208A (en) * | 2016-12-27 | 2017-05-31 | 江苏大学 | A kind of preparation method based on the mesoporous unformed cobalt ferrite electrode material of high-performance |
| CN107342413A (en) * | 2017-07-07 | 2017-11-10 | 东北师范大学 | A kind of ferrous acid cobalt nanometer particle of four oxygen two and its preparation method and application |
| CN108091835A (en) * | 2017-11-20 | 2018-05-29 | 南开大学 | Lithium-sulfur battery composite cathode material of cobalt ferrite sulfur loaded and preparation method thereof |
| CN108110227A (en) * | 2017-11-20 | 2018-06-01 | 南开大学 | Lithium-sulfur battery composite cathode material of nickel ferrite based magnetic loaded polar support and preparation method thereof |
| CN111450830A (en) * | 2020-04-26 | 2020-07-28 | 王二刚 | Nano CoFe2O4Oxygen reduction catalyst loaded with nitrogen-doped porous carbon and preparation method thereof |
| EP3960706A4 (en) * | 2019-04-25 | 2023-05-31 | Nittetsu Mining CO., LTD. | Method for producing cobalt ferrite particles and cobalt ferrite particles produced by same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN108091835A (en) * | 2017-11-20 | 2018-05-29 | 南开大学 | Lithium-sulfur battery composite cathode material of cobalt ferrite sulfur loaded and preparation method thereof |
| CN108110227A (en) * | 2017-11-20 | 2018-06-01 | 南开大学 | Lithium-sulfur battery composite cathode material of nickel ferrite based magnetic loaded polar support and preparation method thereof |
| CN108091835B (en) * | 2017-11-20 | 2020-10-02 | 南开大学 | Lithium-sulfur battery composite positive electrode material with sulfur loaded on cobalt ferrite and preparation method thereof |
| EP3960706A4 (en) * | 2019-04-25 | 2023-05-31 | Nittetsu Mining CO., LTD. | Method for producing cobalt ferrite particles and cobalt ferrite particles produced by same |
| CN111450830A (en) * | 2020-04-26 | 2020-07-28 | 王二刚 | Nano CoFe2O4Oxygen reduction catalyst loaded with nitrogen-doped porous carbon and preparation method thereof |
| CN111450830B (en) * | 2020-04-26 | 2021-12-03 | 吉南 | Nano CoFe2O4Oxygen reduction catalyst loaded with nitrogen-doped porous carbon and preparation method thereof |
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