CN106410154A - Preparation method of carbon-coated iron borate material and application of carbon-coated iron borate material in sodium ion batteries - Google Patents
Preparation method of carbon-coated iron borate material and application of carbon-coated iron borate material in sodium ion batteries 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 preparation method of carbon-coated iron borate material and application of the carbon-coated iron borate material in sodium ion batteries; carbon-coated iron borate is prepared by: dispersing and stirring well iron borate and a carbon source, sintering at the temperature of 300-900 DEG C in an inert atmosphere for 1-15 h, cooling, and grinding. The materials used in the method have a wide range of origin, the preparation method is simple, the prepared carbon-coated iron borate material exhibits excellent cycle stability and rate performance when applied to sodium ion battery anode materials; therefore, the method of the invention is an effective method to improve electrochemical properties of a sodium ion battery.
Description
Technical field
The invention belongs to chemical field, it is related to a kind of energy storage material, especially relate to a kind of carbon coating boric acid iron material
Preparation method and its application in sodium-ion battery.
Background technology
Growth with population in the world and the growth requirement of society, the unprecedented energy crisis of facing mankind and environment are asked
Topic, be allowed to solar energy, wind energy, tide energy etc. have green, environmental protection, sustainable development feature novel energy put into big
The concern of amount, but can not be incorporated directly in existing power utilization network because such energy has intermittent feature.People
Exploring the device improving energy conversion rate and storage always.Electrochmical power source, as a kind of energy storage of excellent performance and converting means
Put, be widely applied to all many-sides such as life, industry and national defence.
Lithium ion battery due to having the advantages such as memory-less effect, high power capacity and long circulation life, from 90 years last century
Since commercialization, the industries such as portable electric appts, electric motor car have been widely applied to it.But the finiteness due to lithium resource and
The increase of exploitation difficulty, its price rises year by year it is impossible to meet large-scale application.The attention of people gradually transfers to exploitation
On the novel secondary battery of alternative lithium ion battery.Sodium, as the same major element adjoining with lithium, has similar physics
Chemical property, and sodium-ion battery has the energy storage mechnism similar compared with lithium ion battery.Secondly, sodium resource due to widely distributed, carry
Refining is simple, is more easy to be utilized by the mankind.Simply sodium ion due to there is the radius more much bigger than lithium ion and more difficult in tradition
Lithium ion battery material in carry out reversible embedded/embedding go out, and easily cause the destruction of material structure and lead to declining of capacity
Subtract.Therefore, seek a kind of new Stability Analysis of Structures, excellent performance electrode material of crucial importance.
As a kind of polyanion type compound, borate (BO3 3-) molal weight less, only 58.8g/mol.
Therefore, lithium-containing transition metal borate LiMBO3(M=Fe, Mn, Co etc.) is possible to be had than other polyanion type positive pole materials
Expect higher specific capacity, for example, LiFeBO3Theoretical specific capacity be up to 220mA h/g, compare LiFePO4About exceed 50mA h/
g.Additionally, LiMBO3Have higher electronic conductivity (Journal of advanced Materials, 2010,22 (
32):3583- 3587), such as LiFeBO3Electronic conductivity be 3.9 × 10-7S/cm, this develops into power-type for borate
Lithium ion battery electrode material provides theoretical foundation.The high electronegativity of boron element leads to the inductive effect of polyanion larger,
Make the embedding de- lithium current potential of borate material of a relatively high, and the theoretical specific capacity of borate positive electrode is high, therefore theoretical
Energy density is high.Additionally, boron atom has the oxytropism of height, a series of atomic radical can be formed with oxygen atom ligand,
BO3 3-、BO5 4-And BO9 6-Deng.These groups form ring-type, caged then repolymerization chaining, piece, netted with oxygen atom again, this
The multiformity of structure brings diversified performance, such as nonlinear optics, ferroelectricity, piezoelectricity and quasiconductor behavior etc., in a word, metal boron
Hydrochlorate has larger application potential in terms of electrochemistry.
Iron borate (Fe3BO6) as a kind of transition metal borate, be explored for lithium ion battery negative material,
Calendar year 2001, study as lithium ion battery negative material first, find that it has the discharge capacity first of 965mAh/g, but
It is that there is poor cyclical stability (Journal of power sources, 97-98,2001,254-257).Therefore, by one
Kind of simple mode is extremely important lifting iron borate chemical property.
Content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation side of carbon coating boric acid iron material
Method and its application in sodium-ion battery, the described preparation method of this carbon coating boric acid iron material and its sodium-ion battery
In application to solve the not good technical problem of iron borate cyclical stability of the prior art.
The invention provides a kind of preparation method of carbon coating iron borate, weigh iron borate and carbon source, boron according to mass ratio
Sour ferrum is 1 with the mass ratio of carbon source:(0.05~2)；It is uniformly dispersed, iron borate and carbon source mixing under an inert atmosphere, in temperature
Spend for sintering under conditions of 300 DEG C ~ 900 DEG C, the time is 1 ~ 15h, then cools down, grind and carbon coating iron borate is obtained.
More preferred scheme, prepare carbon coating iron borate when, carbon source select one of Oleic acid, glucose, sucrose or
Person is multiple；Boric acid iron material is 1 with the mass ratio of carbon source:(0.2~1).Process for dispersing is in planetary type ball-milling and solvent dispersion
One or two kinds of；Inert atmosphere is nitrogen；Sintering temperature is 400 DEG C ~ 800 DEG C.
Present invention also offers a kind of application in sodium-ion battery for carbon coating boric acid iron material, by the carbon of above-mentioned acquisition
Cladding boric acid iron material, binding agent and conductive agent mixing, prepared slurry, slurry are applied to collection liquid surface, dry and make electrode
Pole piece.
Further, the mass ratio of carbon coating boric acid iron material, binding agent and conductive agent is (80-95)：（2~10）：（3~
10）；Described binding agent is hydroxymethyl cellulose（CMC）, Kynoar（PVDF）In any one；Collector is Copper Foil
Or any one in the middle of nickel foam；Drying temperature is 50 ~ 130 DEG C；Drying mode is vacuum drying or forced air drying
A kind of.
Iron borate and carbon source are passed through dispersion, are uniformly mixed by the present invention, under an inert atmosphere, permanent at a certain temperature
Temperature keeps a period of time, after cooling, grinds and carbon coating negative material is obtained.By mixing carbon coating boric acid iron material, binding agent
The slurry being obtained with conductive agent is coated in collection liquid surface, dries and makes electrode plates.Method of the present invention raw material sources are extensive, system
Standby technique is simple, and prepared carbon coating boric acid iron material shows excellent stable circulation and multiplying power in sodium-ion battery application
Performance.Therefore, the present invention is to provide a kind of preparation method of sodium-ion battery excellent electrochemical performance electrode material.
The present invention compares with prior art, and its technological progress is significant.Introduced by carbon coating and compound method
Material with carbon element, on the one hand can effectively prevent boric acid iron material directly and electrolyte contacts, on the other hand, can effectively alleviate
The problem of the electrode material volumetric expansion that should bring in charge and discharge process, can effectively improve the electrochemistry of iron borate
Energy.Shown by electro-chemical test, carbon coating iron borate disclosed by the invention has excellent cycling as sodium ion negative material
Performance and high rate performance.The preparation method process is simple of the present invention, carbon source material wide material sources, cheap, safe.
Brief description
The charge and discharge cycles curve chart of the carbon coating boric acid iron material that Fig. 1 prepares for embodiment 1.
The charge and discharge cycles curve chart of the carbon coating boric acid iron material that Fig. 2 prepares for embodiment 2.
Circulating ratio curve chart under different discharge currents for the boric acid iron material that Fig. 3 prepares for embodiment 1.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
The preparation of sodium-ion battery and electrochemical property test：
The preparation of sodium-ion battery：It is to electrode with metallic sodium；Mass ratio is dissolved in for 1 with 1mol/L：1 ethylene carbonate
（EC）/ dimethyl carbonate（DMC）Mixed solution in NaClO4Saline solution is as electrolyte；It is assembled into button in argon glove box
Formula battery.
Electrochemical property test, charging/discharging voltage scope are carried out using Wuhan Lan electricity company CT2001A type cell tester
For 0.01V ~ 3.0V (vs.Na+/Na).Test temperature is 25 DEG C.
Embodiment 1
By 1gFe3BO6, 0.79g Oleic acid and ethanol in proper amount, by electromagnetic agitation 4h, after drying under the conditions of 60 DEG C, in nitrogen atmosphere
Under, with tube furnace, with the ramp of 5 DEG C/min, to 500 DEG C and constant temperature keeps 5h, grinds carbon coating boron is obtained after natural cooling
Sour iron material.
Prepared by negative pole：By the carbon coating iron borate negative material of above-mentioned preparation, conductive carbon black and binding agent carboxymethyl cellulose
Element（CMC）In mass ratio 80:10:10 mix homogeneously, are coated on Copper Foil, strike out electrode slice, in 100 DEG C of forced air dryings after being dried
24h.
Fig. 1 is the charge and discharge cycles curve chart in 400mA/g electric current density for the button cell of above-mentioned negative pole preparation.As schemed
Show, in the range of the discharge and recharge of 0.01-3.0V, carbon coating boric acid iron material first time discharge capacity is up to 517mAh/g, relatively
Less in the discharge capacity first of pure phase boric acid iron material, this is to be due to, with the presence of due to carbon, circulating electric discharge second
312mAh/g, also few compared with pure phase, but after 200 circulations, pure phase iron borate material discharging capacity is only 71.7mAh/g, only
It is in the 17.2% of second discharge capacity, carbon coating boric acid iron material capacity after 200 circulations still can keep 255.5mAh/
G, relatively second discharge capacity is compared, and capability retention is 81.9% it may be said that the iron borate of bright carbon coating has excellent circulation
Stability.Fig. 3 be the preparation of above-mentioned negative pole button cell under different electric current densities circulating ratio curve chart, as illustrated,
In the range of the charging/discharging voltage of 0.01-3.0V, under 400mA/g discharge current, after 65 circulations, the capacity of iron borate is maintained for up to
292.9mAh/g, when discharge current density is increased to 800mA/g, 1600mA/g, 4000mA/g and 6000mA/g, iron borate
Charge specific capacity remains 266.5mAh/g, 229.4mAh/g, 162.6mAh/g and 121.2mA/g respectively.When electric current density is returned
When arriving 400mA/g again, battery charge specific capacity still can be returned to 297.4mAh/g.Illustrate to invent this material have excellent forthright again
Energy.
Embodiment 2
By 1gFe3BO6, 0.5g Oleic acid and ethanol in proper amount, by electromagnetic agitation 4h, after drying under the conditions of 60 DEG C, in nitrogen atmosphere
Under, with tube furnace, with the ramp of 5 DEG C/min, to 600 DEG C and constant temperature keeps 5h, grinds carbon coating boron is obtained after natural cooling
Sour iron material.
Prepared by negative pole：By the carbon coating iron borate negative material of above-mentioned preparation, conductive carbon black and binding agent carboxymethyl cellulose
Element（CMC）In mass ratio 80:10:10 mix homogeneously, are coated on Copper Foil, strike out electrode slice, in 80 DEG C of forced air dryings after being dried
24h.
Fig. 2 is the charge and discharge cycles curve chart in 400mA/g electric current density for the button cell of above-mentioned negative pole preparation.As schemed
Show, in the range of the discharge and recharge of 0.01-3.0V, carbon coating boric acid iron material first time discharge capacity is up to 614.2mAh/g, phase
Discharge capacity first for pure phase boric acid iron material is less, and this is to be due to, with the presence of due to carbon, circulating electric discharge second
373.5mAh/g, also few compared with pure phase, but after 137 circulations, pure phase iron borate material discharging capacity is only 231.8mAh/g,
For the 55.6% of second discharge capacity, and continuous decrement during following cycle, after 200 circulations, capacity is only possessed
71.7mA/g.Only in the 17.2% of second discharge capacity, carbon coating boric acid iron material capacity after 137 circulations still can be protected
Hold 372.2mAh/g, relatively second discharge capacity is compared, capability retention up to 99.6% is it may be said that the iron borate of bright carbon coating
There is excellent cyclical stability.
Embodiment 3
By 1gFe3BO6, 0.4g sucrose and appropriate amount of deionized water, by electromagnetic agitation 4h, after drying under the conditions of 60 DEG C, in nitrogen
Under atmosphere, with tube furnace, with the ramp of 5 DEG C/min, to 600 DEG C and constant temperature keeps 4h, grinds carbon bag is obtained after natural cooling
Cover boric acid iron material.
Prepared by negative pole：By the carbon coating iron borate negative material of above-mentioned preparation, conductive carbon black and binding agent Kynoar
（PVDF）In mass ratio 75:10:15 mix homogeneously, are coated on Copper Foil, strike out electrode slice, in 70 DEG C of forced air dryings after being dried
24h.
Embodiment 4
By 1gFe3BO6, 0.33g glucose and appropriate amount of deionized water, by electromagnetic agitation 4h, after drying under the conditions of 60 DEG C, in nitrogen
Under gas atmosphere, with tube furnace, with the ramp of 5 DEG C/min, to 400 DEG C and constant temperature keeps 8h, grinds carbon is obtained after natural cooling
Cladding boric acid iron material.
Prepared by negative pole：By the carbon coating iron borate negative material of above-mentioned preparation, conductive carbon black and binding agent carboxymethyl cellulose
Element（CMC）In mass ratio 80:10:10 mix homogeneously, are coated on Copper Foil, strike out electrode slice, in 80 DEG C of forced air dryings after being dried
24h.
In the range of the discharge and recharge of 0.01-3.0V, under the test electric current density of 400mA/g, carbon coating boric acid iron material
Initial charge specific capacity is up to 381.3mAh/g, and after 200 circulations, charge specific capacity remains 354.9mAh/g.
Embodiment 5
By 1gFe3BO6, 0.17g Colophonium and appropriate oxolane, manually grind 30min, after drying under the conditions of 50 DEG C,
Under nitrogen atmosphere, with tube furnace, with the ramp of 4 DEG C/min, to 800 DEG C and constant temperature keeps 5h, grinds and be obtained after natural cooling
Carbon coating boric acid iron material.
Prepared by negative pole：By the carbon coating iron borate negative material of above-mentioned preparation, conductive carbon black and binding agent hydroxylmethyl cellulose
Element（CMC）In mass ratio 85:10:5 mix homogeneously, are coated on Copper Foil, strike out electrode slice, in 90 DEG C of forced air dryings after being dried
10h.
Embodiment 6
By 1gFe3BO6, 0.4g sucrose and appropriate amount of deionized water, by electromagnetic agitation 2h, after drying under the conditions of 70 DEG C, in nitrogen
Under atmosphere, with tube furnace, with the ramp of 3 DEG C/min, to 500 DEG C and constant temperature keeps 2h, grinds carbon bag is obtained after natural cooling
Cover boric acid iron material.
Prepared by negative pole：By the carbon coating iron borate negative material of above-mentioned preparation, conductive carbon black and binding agent hydroxylmethyl cellulose
Element（CMC）In mass ratio 80:10:10 mix homogeneously, are coated on Copper Foil, strike out electrode slice, in 70 DEG C of forced air dryings after being dried
24h.
In the range of the discharge and recharge of 0.01-3.0V, under the test electric current density of 400mA/g, carbon coating boric acid iron material
Initial charge specific capacity is up to 390.3mAh/g, and after 200 circulations, charge specific capacity remains 363.2mAh/g.
Embodiment 7
By 1gFe3BO6, 0.2g sucrose and appropriate amount of deionized water, 4h is disperseed by solution, after drying under the conditions of 70 DEG C, in nitrogen
Under atmosphere, with tube furnace, with the ramp of 8 DEG C/min, to 600 DEG C and constant temperature keeps 4h, grinds carbon bag is obtained after natural cooling
Cover boric acid iron material.
Prepared by negative pole：By the carbon coating iron borate negative material of above-mentioned preparation, conductive carbon black and binding agent Kynoar
（PVDF）In mass ratio 75:10:15 mix homogeneously, are coated on Copper Foil, strike out electrode slice, in 80 DEG C of forced air dryings after being dried
24h.
Above said content is only the basic explanation under present inventive concept, and according to appointing that technical scheme is done
What equivalent transformation, all should belong to protection scope of the present invention.
Claims (4)
1. a kind of preparation method of carbon coating iron borate is it is characterised in that comprise the steps：
1）Weigh iron borate and carbon source according to mass ratio, iron borate is 1 with the mass ratio of carbon source:(0.05~2)；By iron borate and
Carbon source mixes, and is uniformly dispersed；
2）Under an inert atmosphere, sinter under conditions of temperature is 300 DEG C ~ 900 DEG C, the time is 1 ~ 15h, then cools down, grind
Prepared carbon coating iron borate.
2. carbon coating iron borate according to claim 1 preparation method it is characterised in that：Described carbon source be Oleic acid,
One of oleic acid derivatives, glucose, sucrose or Colophonium or two or more combinations；Described inert atmosphere is nitrogen
One of noble gases such as gas, argon or multiple.
3. a kind of application in sodium-ion battery for carbon coating boric acid iron material it is characterised in that：The carbon that claim 1 is obtained
Cladding boric acid iron material, binding agent and conductive agent mixing, prepared slurry, slurry are applied to collection liquid surface, dry and make electrode
Pole piece.
4. according to claim 3 application it is characterised in that：Described carbon coating boric acid iron material, binding agent and conduction
The mass ratio of agent is (75-95)：（2~10）：（3~15）；Described binding agent is hydroxymethyl cellulose（CMC）, Kynoar
（PVDF）, any one in sodium alginate；Collector is any one in the middle of Copper Foil or nickel foam；Drying temperature is 50
~130℃；Drying mode is any one of vacuum drying or forced air drying.
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Cited By (5)
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| CN110459737A (en) * | 2018-05-07 | 2019-11-15 | 福建师范大学 | A kind of preparation method and applications of the carbon coating boric acid ferrous iron of core-shell structure |
| CN110767887A (en) * | 2019-10-24 | 2020-02-07 | 华南理工大学 | Vanadium-manganese borate material, carbon-coated vanadium-manganese borate material, and preparation methods and applications thereof |
| CN111029570A (en) * | 2019-11-27 | 2020-04-17 | 长沙理工大学 | Cobalt borate/graphene composite material for lithium ion battery cathode and preparation method thereof |
| CN114171802A (en) * | 2021-12-08 | 2022-03-11 | 西安航空学院 | Lithium ion battery with low-temperature performance and preparation method thereof |
| CN115084484A (en) * | 2022-07-29 | 2022-09-20 | 湖北万润新能源科技股份有限公司 | Sodium-ion battery positive electrode material and preparation method and application thereof |
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| CN110459737A (en) * | 2018-05-07 | 2019-11-15 | 福建师范大学 | A kind of preparation method and applications of the carbon coating boric acid ferrous iron of core-shell structure |
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| CN110767887A (en) * | 2019-10-24 | 2020-02-07 | 华南理工大学 | Vanadium-manganese borate material, carbon-coated vanadium-manganese borate material, and preparation methods and applications thereof |
| CN111029570A (en) * | 2019-11-27 | 2020-04-17 | 长沙理工大学 | Cobalt borate/graphene composite material for lithium ion battery cathode and preparation method thereof |
| CN114171802A (en) * | 2021-12-08 | 2022-03-11 | 西安航空学院 | Lithium ion battery with low-temperature performance and preparation method thereof |
| CN114171802B (en) * | 2021-12-08 | 2023-11-03 | 西安航空学院 | Lithium ion battery with low-temperature performance and preparation method thereof |
| CN115084484A (en) * | 2022-07-29 | 2022-09-20 | 湖北万润新能源科技股份有限公司 | Sodium-ion battery positive electrode material and preparation method and application thereof |
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