CN108565429A - A kind of anode material of lithium-ion battery NaFeS2The preparation method of/C composite - Google Patents

A kind of anode material of lithium-ion battery NaFeS2The preparation method of/C composite Download PDF

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CN108565429A
CN108565429A CN201810354012.2A CN201810354012A CN108565429A CN 108565429 A CN108565429 A CN 108565429A CN 201810354012 A CN201810354012 A CN 201810354012A CN 108565429 A CN108565429 A CN 108565429A
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sodium
nafes
composite
preparation
ion battery
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CN108565429B (en
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何文
张合钰
张旭东
王春莲
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JIANGSU CORE-CIRCLES AMPEREX TECHNOLOGY Co.,Ltd.
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Qilu University of Technology
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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
    • 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
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • 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
    • 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 present invention relates to a kind of anode material of lithium-ion battery NaFeS2The preparation method of/C composite.This method includes：Sodium sulphur source, source of iron and carbon source are taken in proportion, absolute ethyl alcohol are added after mixing, slurry is made；It is dried after ball milling, then grinds to obtain presoma；By presoma under nitrogen atmosphere protection, is heated up and be heat-treated using two-part, obtain NaFeS2/ C composite.This method is heat-treated through solid phase carbon thermal reduction, so that carbon source is become carbon skeleton and is made NaFeS2It is attached on carbon skeleton, is conducive to the transmission of sodium ion and increases electric conductivity；At low cost, preparation process is simple, is used as its performance of anode material of lithium-ion battery better than FeS2Material.

Description

A kind of anode material of lithium-ion battery NaFeS2The preparation method of/C composite
Technical field
The present invention relates to a kind of anode material of lithium-ion battery NaFeS2The preparation method of/C composite, belongs to sodium ion Cell negative electrode material technical field.
Background technology
Lithium ion battery have energy density is big, have extended cycle life, operating voltage height, memory-less effect, naturally electric discharge it is small, The advantages that operating temperature range is wide.And as lithium ion battery is gradually applied to electric vehicle, the demand of lithium will increase greatly Add, and the reserves of lithium are limited, and is unevenly distributed, this intelligent grid cheap for demand for development, safe and can be again It is a bottleneck problem for the extensive energy storage amount long-life energy-storage battery in production-goods source.Therefore, there is an urgent need for development comprehensive performance is excellent Different energy-storage battery new system, for comparing lithium resource, sodium reserves very abundant, and be widely distributed.Metallic sodium and metal There is lithium similar chemical property, sodium-ion battery and lithium ion battery also to have similar charge-discharge principle.But compared to Sodium ion radius is larger for lithium ion, causes sodium ion intercalation/deintercalation in electrode material difficult, chemical property is poor.Cause This, finding suitable electrode material becomes the key point of sodium-ion battery development.
The FeS of Pyrite-type2Have many advantages, such as that resourceful, cheap, nontoxic and theoretical capacity is high, it is a kind of with pole The sodium-ion battery pole material for having application prospect, causes extensive concern and the research of people.However due to FeS2Semiconductor category Since the intercalation/deintercalation of sodium ion causes material structure to cave in property and charge and discharge process, lead to FeS2Sodium-ion battery is negative Pole material capacity decaying is poor with high rate performance quickly.And FeS2/ C using small particle size and carbon flexibility can weaken because The abjection of active material and the embedded stress variation for generating bulk effect and bringing, to weaken the powder of electrode material, enhancing Cycle performance.With Fe (NO3)3And CH3CSNH2For raw material, pass through the other FeS of hydro-thermal method synthesizing micron-grade2Material is used as sodium When ion battery cathode material, in 100mA g-1Current density under, for the first time discharge capacity be 718mAhg-1, in current density For 5000mAg-1When, it can also keep 323mAh g-1Capacity, referring to Kongyao Chen et al., Mechanism of Capacity Fade in Sodium Storage and the Strategies of Improvement for FeS2Anode, ACS Appl.Mater.Interfaces 9 (2017) 1536-1541.；But the FeS of this method synthesis2Material is Micron level, grain size is larger, the FeS in charge and discharge process2Material structure is easy to cave in.Patent document CN107452951A is announced One kind preparing FeS by solvent-thermal method2Nano material, and it is applied to the method for sodium-ion battery cathode.This method is logical It crosses FeSe2It is coated on FeS2Core-shell particles electrode material is formed on material, when making sodium-ion battery cathode, in 100mAg-1's Under current density, discharge capacity is 600mAh g for the first time-1.By above-mentioned prior art data as it can be seen that FeS2Make negative material, electricity Chemical property is general.
NaFeS is not yet found in the natural environment2This substance, it is a kind of substance with mixed valence, chemically Matter and physical property depend on the oxidation state of iron.Wu Hua is strong etc. to be reported a kind of microwave assisting method and prepares threadiness NaFeS2 Nano-particle, referring to《Spectroscopic methodology and spectrum analysis》The 6th phase of volume 25, in June, 2005.But related NaFeS is had no so far2 Make the report of negative material.
Invention content
In view of the deficiencies of the prior art, technical assignment of the invention is to provide a kind of novel anode material of sodium-ion battery NaFeS2/ C, the present invention also provides a kind of NaFeS with excellent chemical property2The preparation method of/C composite.
The present invention uses solid phase method, and sodium source, source of iron, sulphur source and carbon source mix grinding is uniform, and NaFeS is synthesized through high-temperature calcination2/ C is used for the negative material of sodium-ion battery.
Technical scheme is as follows：
A kind of NaFeS2The preparation method of/C composite, including step：
(1) according to molar ratio Na:Fe:S:C=1:1:2:3~6, sodium-sulphur source, source of iron and carbon source are taken, is added after mixing Enter appropriate absolute ethyl alcohol and slurry is made；
(2) slurry of step (1) is fitted into ball grinder, in 1000~1800r min-1Rotating speed under grinding 80~ 150min
Afterwards, in 50-60 DEG C of drying, it is then ground to powder, obtains presoma；
(3) by the presoma in step (2) nitrogen atmosphere protection under, be heated to 260~400 DEG C heat preservation 100~ 300min, after being continuously heating to 550~800 DEG C of 300~600min of heat preservation, cooled to room temperature obtains NaFeS2/ C is compound Material.
Above step (3) makes presoma be heat-treated through solid phase carbon thermal reduction, so that carbon source is become carbon skeleton, and make NaFeS2It is attached It on carbon skeleton, this is conducive to the transmission of sodium ion and increases electric conductivity.
According to currently preferred, in step (1), the sodium-sulphur source is sodium thiosulfate or vulcanized sodium, preferably thio sulphur Sour sodium；
According to currently preferred, in step (1), the source of iron is ferrous oxalate, frerrous chloride or iron chloride, preferably careless It is sour ferrous；
According to currently preferred, in step (1), the carbon source is sodium lignin sulfonate, glucose or sucrose, preferably sugarcane Sugar；
According to currently preferred, in step (1), the Na:Fe:S:C=1：1：2：3.5-5.5 molar ratio；Most preferably, Na:Fe:S:C=1：1：2：4.2-4.6 molar ratio.
According to currently preferred, in step (2), the grinding revolution is 1200r min-1, milling time 100min.
According to currently preferred, in step (3), the heat treatment temperature be 300 DEG C of soaking times be 200min and 600 DEG C of soaking times are 480min.
The most preferred scheme of the present invention is technical solution described in embodiment 1.
According to the novel anode material NaFeS of sodium-ion battery prepared by above method2/ C composite.
NaFeS produced by the present invention2Application of/the C composite as the negative material of sodium-ion battery.Concrete application side Method is as follows：
1. by NaFeS2/ C is fully ground after mixing with conductive agent and binder, and it is molten that N-Methyl pyrrolidone is added Agent obtains precoating slurries after stirring evenly；
2. above-mentioned precoating slurries are coated on copper foil, up to sodium-ion battery cathode after being then dried electrode slice Electrode slice, gained sodium-ion battery negative electricity pole piece are used for button-type battery sodium-ion battery.
Conductive agent and binder described above press the prior art, such as acetylene black and Kynoar.
Sodium-ion battery composite negative pole material NaFeS prepared by the method for the present invention2/ C, charging/discharging voltage be 0.01~ 3.0V and 1A g-1First discharge specific capacity under electric current is 1156.07mA hg-1, exceed theoretical specific capacity, after recycling 50 times Specific discharge capacity is 507.43mAh g-1。
Beneficial effects of the present invention are as follows：
By sodium source, sulphur source, source of iron and carbon source, mixing and ball milling makes carbon to the present invention through solid phase carbon thermal reduction heat treatment in proportion Source becomes carbon skeleton, and makes NaFeS2It is attached on carbon skeleton, this is conducive to the transmission of sodium ion and increases electric conductivity；In addition, NaFeS2Sodium distribution in structure is used as sodium ion battery electrode material between Fe-S tetrahedrons and shared tetrahedron When, the better intercalation/deintercalation of sodium ion energy, and stable structure；And can effectively reduce sulfide by carbon coating and be dissolved in has Machine electrolyte, reduce polysulfide insulating layer is formed other than electrode, can effectively improve in this way material charge/discharge capacity and Cycle performance.
The NaFeS that the present invention passes through easy-to-use Solid phase synthesis2/ C composite, at low cost, preparation process is simple, As anode material of lithium-ion battery, its performance is better than FeS2Material has applications well foreground.
Description of the drawings
Fig. 1 is the NaFeS prepared in embodiment 12The XRD diagram of/C composite, wherein ordinate are intensity, and abscissa is Angle of diffraction (2 θ).
Fig. 2 is the NaFeS prepared in embodiment 12The EDS analysis charts of/C composite.
Fig. 3 is the NaFeS prepared in embodiment 12The electrochemistry cycle performance figure of/C composite.
Specific implementation mode
Below by specific embodiment and in conjunction with attached drawing, the present invention will be further described, but not limited to this.
Raw materials used in embodiment is raw material purchased in market.
Embodiment 1, Na:Fe:S:C=1:1:2:4.4 molar ratio
It takes the sucrose of the sodium thiosulfate of 2.482g, the ferrous oxalate of 1.799g and 0.685g to mix, absolute ethyl alcohol is added Solid powder is not crossed, is put into ball grinder after stirring, in 1200r min-1Rotating speed under grinding 100min after obtain paste mixing Object；Grind into powder after it is dried at 60 DEG C, obtains presoma；It is finally heated to 300 DEG C of guarantors in a nitrogen atmosphere Warm 200min then proceedes to be warming up to 600 DEG C of heat preservation 480min, and natural cooling obtains NaFeS2/ C composite.It prepares NaFeS2It is as depicted in figs. 1 and 2 that/C receives the XRD diagram of composite material, EDS analysis charts.By the XRD diagram of Fig. 1 it is found that synthetic product Main diffraction peak and NaFeS2The standard card of crystalline phase corresponds to, and without other crystalline phases；By the EDS analysis charts of Fig. 2 it is found that synthesizing The Main chemical component of product is Na, Fe, S, C, therefore synthetic product is NaFeS2/ C composite, wherein C are unformed Phase.
Electrochemical property test
By NaFeS made from the embodiment 12/ C composite is used for sodium-ion battery, and electrode is prepared using rubbing method.It will NaFeS2/ C, acetylene black and Kynoar (PVDF) press 8:1:1 mass ratio is fully ground mixing, and N- crassitudes are added Ketone solvent obtains precoating refined slurries after stirring evenly, and above-mentioned precoating, which is refined slurries, to be coated on copper foil, through 60 DEG C of dry 6h 12h are dried in vacuo with 120 DEG C, the disk of diameter 15mm is cut into after natural cooling using sheet-punching machine, that is, it is negative that sodium-ion battery is made Pole electrode slice.It is assembled successively according to the sequence of anode cover-electrode slice-electrolyte-diaphragm-electrolyte-lithium piece-gasket-negative electrode casing, Recycle sealing machine by cell sealing, you can CR2032 type button half-cells are made.It is finally high in A713-2008S-3TGF-A types Precision charge and discharge instrument carries out constant current charge-discharge test to battery.
NaFeS prepared by embodiment 1 utilized above2/ C negative materials charging/discharging voltage be 0.01~3.00V and Under 1000mA/g current densities, first discharge specific capacity is 1156mAh g-1, the discharge capacity after recycling 50 times is 507mAh g-1, as shown in Figure 3.
Embodiment 2, Na:Fe:S:C=1:1:2:3.5 molar ratio
4.604g vulcanized sodium, 1.988g frerrous chlorides, 1.149g glucose are taken, absolute ethyl alcohol is added and did not had solid powder, It is put into after mixing in not ball grinder, in 1800r min-1Rotating speed under grinding 80min after obtain paste mixture；By it in 60 DEG C Grind into powder after lower drying, obtains presoma；It is finally heated to 260 DEG C of heat preservation 300min in a nitrogen atmosphere, then 800 DEG C of heat preservation 300min are continuously heating to, natural cooling obtains NaFeS2/ C composite.It is used as sodium-ion battery cathode When material, the first discharge specific capacity under being 0.01~3.00V and 1000mA/g current densities in voltage is 852mAhg-1, cycle Discharge capacity after 50 times is 327mAh g-1。
Embodiment 3, Na:Fe:S:C=1:1:2:5.5 molar ratio
2.482g sodium thiosulfate, 2.703g iron chloride, 1.470g sodium lignin sulfonates are taken, it is excessively not solid that absolute ethyl alcohol is added Body powder is put into after mixing in not ball grinder, in 1000r min-1Rotating speed under grinding 150min after obtain paste mixture；It will Grind into powder after it is dried at 60 DEG C, obtains presoma；It is finally heated to 400 DEG C of heat preservations in a nitrogen atmosphere 100min then proceedes to be warming up to 550 DEG C of heat preservation 600min, and natural cooling obtains NaFeS2/ C composite.It is used as sodium When ion battery cathode material, the first discharge specific capacity under being 0.01~3.00V and 1000mA/g current densities in voltage is 747mAh g-1, discharge capacity is 442mAh g after recycling 50 times-1。

Claims (10)

1. a kind of NaFeS2The preparation method of/C composite, including step：
(1) according to molar ratio Na:Fe:S:C=1:1:2:3~6, sodium-sulphur source, source of iron and carbon source are taken, is added after mixing suitable Slurry is made in amount absolute ethyl alcohol；
(2) slurry of step (1) is fitted into ball grinder, in 1000~1800r min-1Rotating speed under grind 80~150min Afterwards, in 50-60 DEG C of drying, it is then ground to powder, obtains presoma；
(3) by the presoma in step (2) under nitrogen atmosphere protection, 260~400 DEG C of 100~300min of heat preservation are heated to, after Continue after being warming up to 550~800 DEG C of 300~600min of heat preservation, cooled to room temperature obtains NaFeS2/ C composite.
2. the preparation method of NaFeS2/C composite materials as described in claim 1, it is characterised in that in step (1), the sodium- Sulphur source is sodium thiosulfate or vulcanized sodium, preferably sodium thiosulfate.
3. the preparation method of NaFeS2/C composite materials as described in claim 1, it is characterised in that in step (1), the iron Source is ferrous oxalate, frerrous chloride or iron chloride, preferably ferrous oxalate.
4. the preparation method of NaFeS2/C composite materials as described in claim 1, it is characterised in that in step (1), the carbon Source is sodium lignin sulfonate, glucose or sucrose.
5. the preparation method of NaFeS2/C composite materials as described in claim 1, it is characterised in that in step (1), the Na: Fe:S:C=1：1：2：3.5-5.5 molar ratio；Preferably, Na:Fe:S:C=1：1：2：4.2-4.6 molar ratio.
6. NaFeS as described in claim 12The preparation method of/C composite, which is characterized in that described to grind in step (2) Mill revolution is 1200r min-1, milling time 100min.
7. NaFeS as described in claim 12The preparation method of/C composite, it is characterised in that in step (3), the heat It is 200min and 600 DEG C of soaking time is 480min that treatment temperature, which is 300 DEG C of soaking times,.
8. the preparation method of NaFeS2/C composite materials as described in claim 1, which is characterized in that steps are as follows：
It takes the sucrose of the sodium thiosulfate of 2.482g, the ferrous oxalate of 1.799g and 0.685g to mix, absolute ethyl alcohol is added and did not had Solid powder is put into after stirring in ball grinder, in 1200r min-1Rotating speed under grinding 100min after obtain paste mixture；It will Grind into powder after it is dried at 60 DEG C, obtains presoma；It is finally heated to 300 DEG C of heat preservations in a nitrogen atmosphere 200min then proceedes to be warming up to 600 DEG C of heat preservation 480min, and natural cooling obtains NaFeS2/ C composite.
9. such as the negative material NaFeS of novel sodium-ion battery prepared by claim 1-8 any one of them methods2/ C is compound Material.
10. the NaFeS prepared such as claim 1-8 any one of them methods2Cathode of/the C composite as sodium-ion battery The application of material, method are as follows：
1. by NaFeS2/ C is fully ground after mixing with conductive agent and binder, and N-Methyl pyrrolidone solvent, stirring is added Precoating slurries are obtained after uniformly；
2. above-mentioned precoating slurries are coated on copper foil, up to sodium-ion battery negative electrode after being then dried electrode slice Piece, gained sodium-ion battery negative electricity pole piece are used for button-type battery sodium-ion battery.
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CN113140728A (en) * 2021-04-26 2021-07-20 燕山大学 Potassium iron sulfide thin film electrode and preparation method and application thereof
CN113578351A (en) * 2021-08-03 2021-11-02 齐鲁工业大学 Pyrite iron disulfide/titanium dioxide composite material and preparation method and application thereof

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CN113140728A (en) * 2021-04-26 2021-07-20 燕山大学 Potassium iron sulfide thin film electrode and preparation method and application thereof
CN113140728B (en) * 2021-04-26 2022-04-05 燕山大学 Potassium iron sulfide thin film electrode and preparation method and application thereof
CN113578351A (en) * 2021-08-03 2021-11-02 齐鲁工业大学 Pyrite iron disulfide/titanium dioxide composite material and preparation method and application thereof
CN113578351B (en) * 2021-08-03 2023-05-23 齐鲁工业大学 Pyrite iron disulfide/titanium dioxide composite material and preparation method and application thereof

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