CN106299304A - A kind of carbon cladding molybdenum sulfide composite and preparation method and application and a kind of sodium-ion battery - Google Patents
A kind of carbon cladding molybdenum sulfide composite and preparation method and application and a kind of sodium-ion battery Download PDFInfo
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- CN106299304A CN106299304A CN201610861221.7A CN201610861221A CN106299304A CN 106299304 A CN106299304 A CN 106299304A CN 201610861221 A CN201610861221 A CN 201610861221A CN 106299304 A CN106299304 A CN 106299304A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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 kind of carbon cladding molybdenum sulfide composite and preparation method and application and a kind of sodium-ion battery.This preparation method first passes through hydro-thermal reaction and prepares molybdenum sulfide presoma, then vapour deposition carbon coated obtains carbon cladding molybdenum sulfide composite.The carbon cladding molybdenum sulfide composite obtained is as anode material of lithium-ion battery, and prepared sodium-ion battery has the chemical property of excellence.The carbon cladding molybdenum sulfide composite material and preparation method thereof technique of the present invention is simple, with low cost, and environmental friendliness, there is the chemical property of excellence, be the most potential anode material of lithium-ion battery of one.
Description
Technical field
The invention belongs to technical field of new energies, be specifically related to anode material of lithium-ion battery and preparation method thereof and answer
With.
Background technology
Lithium ion battery has the series of advantages such as voltage height, specific capacity height, discharge and recharge life-span length, important as a class
Chemical energy storage technology, is widely used in mancarried electronic aid, space flight and aviation, electric automobile field.However as science and technology continuous
Progressive, the demand of lithium also gets more and more.But, on the earth, lithium resource reserves are limited, expensive, limit the long-term big of lithium
Sizable application.Metallic sodium and lithium metal belong to same main group, have similar physicochemical properties, therefore, sodium-ion battery by
Gradually cause the concern of many scholars.Due to sodium rich reserves, take up an area 2.64 % of ball element total amount, compare lithium (0.006 %)
For have in terms of extensive energy storage and have great advantage, there is boundless application prospect.
The theoretical lithium storage content of business-like graphite as anode material for lithium-ion battery is 372 mAh/g (6C+Li++e-↔
LiC6).But graphite reacts with sodium and can be only formed NaC64, and bigger sodium ion radius makes deintercalation sodium process slow, therefore makees
For anode material of lithium-ion battery, graphite storage sodium capacity is the lowest.For meeting, high power capacity long circulating sodium-ion battery is constantly increased
Long demand, it is good that exploitation one has capacity height, good stability, safety, and eco-friendly anode material of lithium-ion battery is
The problem needing solution at present badly.
Molybdenum sulfide as the typical transition-metal sulphides of one, have with graphite-like as two-dimensional slice structure, molybdenum
Atom is between two-layer sulphur atom, forms a kind of sandwich structure, connects with weak Van der Waals force between layers.Molybdenum sulfide leads to
Cross and carry out the storage (MoS of capacity with sodium generation conversion reaction2 +4Na+ +4e- — Mo + 2Na2S), theoretical capacity is up to 670
mAh/g.But, molybdenum sulfide is that a kind of semi-conducting material, electronic conduction ability, and bigger sodium ion radius make its power
Learning slowly, therefore to be faced with actual capacity as anode material of lithium-ion battery low for molybdenum sulfide, the challenges such as circulation is unstable.For
Such problem, this patent proposes a kind of carbon cladding molybdenum sulfide sodium-ion battery composite negative pole material.The present invention is by chemistry gas
Phase sedimentation realizes the carbon cladding of molybdenum sulfide, and on the one hand material with carbon element is as excellent electronic conductor, improves leading of composite
Electrically, the on the other hand change in volume in the cladding available buffer cyclic process of material with carbon element, thus obtain high capacity and stable
Cycle performance.
Summary of the invention
It is an object of the invention to provide a kind of carbon cladding molybdenum sulfide composite and preparation method thereof, the present invention also provides for
This composite is as negative material applying and the sodium-ion battery of preparation in sodium-ion battery.
A kind of preparation method of carbon cladding molybdenum sulfide composite, first Hydrothermal Synthesis molybdenum sulfide, then pass through chemical gaseous phase
Deposition process deposits carbon on molybdenum sulfide surface, obtains described carbon cladding molybdenum sulfide composite.
The preparation method of a kind of carbon cladding molybdenum sulfide composite, specifically includes following steps:
Molybdenum source and sulfur source are dissolved in the water, prepare molybdenum sulfide presoma through hydro-thermal reaction；Molybdenum sulfide presoma is placed in tubular type
In stove, it is passed through carbon source, at molybdenum sulfide presoma surface chemistry vapour deposition carbon, obtains described carbon cladding molybdenum sulfide composite.
Further, described molybdenum source is more than one in sodium molybdate, ammonium molybdate and molybdenum trioxide, preferably sodium molybdate.
Further, described sulfur source is more than one in thiourea, thioacetamide, ammonium sulfide and sodium sulfide, is preferably
Thiourea.
Further, described sulfur source is 2:1～12:1, preferably 2.4:1 with the mol ratio in molybdenum source.
Further, the temperature of described hydro-thermal reaction is 160 DEG C～240 DEG C, preferably 220 DEG C.
Further, the time of described hydro-thermal reaction is 6h～24h, preferably 24h.
Further, described carbon source is methanol, ethanol, toluene, saccharide, oils and fats, organic acid, organic acid esters and small molecular alcohol
In more than one, preferably ethanol.
Further, the temperature of described chemical gaseous phase deposition is 400 DEG C～1000 DEG C.
Further, the temperature of described chemical gaseous phase deposition is 500 DEG C, 600 DEG C, 700 DEG C or 800 DEG C.
Further, the time of described chemical gaseous phase deposition is 1h～10h, preferably 2h.
Further, described chemical gaseous phase deposition is carried out under inert gas atmosphere, preferably argon.
The carbon cladding molybdenum sulfide composite prepared by the described preparation method of any of the above-described item.
The carbon cladding molybdenum sulfide composite application in sodium-ion battery prepared, described carbon cladding molybdenum sulfide composite wood
Expect as anode material of lithium-ion battery, be 8 in mass ratio by described carbon cladding molybdenum sulfide composite, binding agent, conductive agent:
1:1 is mixed and made into slurry in a solvent, coats, is dried, and obtains carbon cladding molybdenum sulfide composite negative pole.
Further, described binding agent is Kynoar (PVDF), polyacrylic acid (PAA), sodium carboxymethyl cellulose
(CMC), more than one in sodium alginate (SA) and butadiene-styrene rubber (SBR).
Further, more than one during described conductive agent is white carbon black, conductive black (Super-P) and Ketjen black.
Further, more than one during described solvent is water and N-Methyl pyrrolidone (NMP).
A kind of sodium-ion battery based on above-mentioned carbon cladding molybdenum sulfide composite negative pole, is coated with molybdenum sulfide including described carbon
Composite negative pole, to electrode metal sodium, barrier film and electrolyte system；Described electrolyte system is organic solvent electrolyte or poly-
Polymer electrolyte, preferably organic solvent electrolyte.
Further, described electrolyte system is the organic solvent electrolyte of sodium salt, the organic solvent electrolysis of described sodium salt
In liquid, the concentration of sodium salt is 1 M.
Further, described sodium salt is NaPF6、NaClO4、NaBF4, one in NaTf, NaFSI and NaTFSI with
On, preferably NaPF6Or NaClO4。
Further, described organic solvent is Merlon (PC), ethylene carbonate (EC), dimethyl carbonate (DMC), second
More than one in glycol dimethyl ether (DME), diethyl carbonate (DEC), oxolane (THF) and triethylene glycol dimethyl ether., preferably
Mixed solvent for PC Yu EC.
Further, containing additive in described electrolyte system, described additive includes fluorinated ethylene carbonate
(FEC), the addition of described additive is 5wt% ~ 10wt%.
Compared with prior art, the invention have the advantages that and beneficial effect:
(1) preparation technology of the carbon cladding molybdenum sulfide composite of the present invention is simple, with low cost, environmental friendliness；
(2) the carbon cladding molybdenum sulfide composite of the present invention shows the electrochemistry of excellence as anode material of lithium-ion battery
Can, the sodium-ion battery prepared has higher reversible capacity and preferable cycle performance, be the most potential sodium of one from
Sub-cell negative electrode material.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of carbon cladding molybdenum sulfide composite in embodiment 1；
Fig. 2 a and Fig. 2 b is the scanning electron microscope (SEM) photograph of carbon cladding molybdenum sulfide composite in embodiment 1；
Fig. 3 is the transmission electron microscope picture of carbon cladding molybdenum sulfide composite in embodiment 1；
Fig. 4 is the cycle performance figure of the sodium-ion battery that carbon cladding molybdenum sulfide composite makes in embodiment 5；
Fig. 5 is the charging and discharging curve of the sodium-ion battery that carbon cladding molybdenum sulfide composite makes in embodiment 5.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not
It is limited to this.
Embodiment 1
Prepare carbon cladding molybdenum sulfide composite:
Sulfur molybdenum atom is dissolved in deionized water with thiourea than the ammonium molybdate being 2.4, after stirring and dissolving, mixed solution is shifted
In 50 ml reactors, at 220 DEG C, it is incubated 24h, through washing, filter, obtaining molybdenum sulfide forerunner after drying after natural cooling
Body, is then placed in tube furnace, logical ethanol, is incubated 2h vapour deposition carbon at argon gas atmosphere 700 DEG C, obtains carbon cladding
Molybdenum sulfide composite.
By X-ray diffractometer (Empyrean Cu K alpha ray), complex is carried out the sign of crystal structure, XRD's
As it is shown in figure 1, as shown in Figure 1, product is molybdenum sulfide to result, due to deposition carbon ratio small amount and be non crystalline structure, the most also
The peak of carbon does not occur.
By scanning electron microscope, the surface topography of complex is characterized, characterization result such as Fig. 2 a and Fig. 2 b institute
Showing, the thickness of sulfuration molybdenum sheet is 1-50 nm.
More specifically structural characterization is carried out to compound by transmission electron microscope, as it is shown on figure 3, at molybdenum sulfide lamella table
There is the thinnest carbon-coating in face.
Embodiment 2
Prepare carbon cladding molybdenum sulfide composite:
Sulfur molybdenum atom is dissolved in deionized water with thiourea than the ammonium molybdate being 2, after stirring and dissolving, mixed solution is transferred to
In 50 ml reactors, at 160 DEG C, be incubated 6h, after natural cooling through washing, filter, obtain presoma molybdenum sulfide after drying and receive
Rice sheet, is then placed in tube furnace, logical ethanol, is incubated 1h vapour deposition carbon, obtains carbon bag at argon gas atmosphere 400 DEG C
Cover molybdenum sulfide composite.
Molybdenum sulfide lamellar spacing in the carbon cladding molybdenum sulfide composite obtained is 1-50nm, in molybdenum sulfide sheet surfaces
There is the thinnest carbon-coating, and be non crystalline structure.
Embodiment 3
Prepare carbon cladding molybdenum sulfide composite:
Sulfur molybdenum atom is dissolved in deionized water with thiourea than the ammonium molybdate being 12, after stirring and dissolving, mixed solution is shifted
In 50 ml reactors, at 240 DEG C, it is incubated 24h, through washing, filter, obtaining presoma molybdenum sulfide after drying after natural cooling
Nanometer sheet, is then placed in tube furnace, logical ethanol, is incubated 10 h vapour deposition carbon at argon gas atmosphere 1000 DEG C,
It is coated with molybdenum sulfide composite to carbon.
Molybdenum sulfide lamellar spacing in the carbon cladding molybdenum sulfide composite obtained is 1-50nm, in molybdenum sulfide sheet surfaces
There is the thinnest carbon-coating, and be non crystalline structure.
Embodiment 4
Prepare carbon cladding molybdenum sulfide composite:
Sulfur molybdenum atom is dissolved in deionized water with thiourea than the ammonium molybdate being 2.4, after stirring and dissolving, mixed solution is shifted
In 50ml reactor, at 220 DEG C, it is incubated 12h, through washing, filter, obtaining presoma molybdenum sulfide after drying after natural cooling
Nanometer sheet, is then placed in tube furnace, logical ethanol, is incubated 2h vapour deposition carbon, obtains carbon at argon gas atmosphere 800 DEG C
Cladding molybdenum sulfide composite.
Molybdenum sulfide lamellar spacing in the carbon cladding molybdenum sulfide composite obtained is 1-50nm, in molybdenum sulfide sheet surfaces
There is the thinnest carbon-coating, and be non crystalline structure.
Embodiment 5
Sodium-ion battery is assembled as anode material of lithium-ion battery using the carbon cladding molybdenum sulfide composite of embodiment 1 preparation,
Carry out electrochemical property test.
The carbon prepared cladding molybdenum sulfide composite is pressed with conductive agent (Super-P), binding agent (sodium alginate)
Mass ratio 8:1:1 uniformly mixes, and with deionized water as solvent, is coated uniformly on Copper Foil after making slurry, makes after vacuum drying
Become pole piece, with this pole piece, to electrode metal sodium, glass fiber filter (Whatman company of Britain GF/D) barrier film, be assembled into
Sodium-ion battery, electrolyte is 1 M NaClO4/ EC-PC(EC:PC=1:1 volume ratio), the FEC additive of 5wt%, at glove
In case, assembling obtains CR2016 button cell.
The battery of above-mentioned assembling carries out on LAND charge-discharge test instrument constant current charge-discharge test, and discharge and recharge interval is
3～0.01 V.
The result of electro-chemical test is as shown in Fig. 4 and Fig. 5, and battery has higher discharge capacity first and preferably follows
Ring stability.When electric current density is 500 mA/g, its first discharge capacity be 580.3 mAh/g, coulombic efficiency is 84.34
%, after circulating 200 times, discharge capacity remains at 366.6 mAh/g.
Embodiment 6
Different from embodiment 5 being, the charging and discharging currents density of the present embodiment is 100 mA/g, and other conditions are the most identical, assembles
Sodium-ion battery tests its chemical property, its first discharge capacity be 678mAh/g, coulombic efficiency is 84.56 %, circulation
After 150 times, discharge capacity remains at 434.1 mAh/g.
Embodiment 7
Different from embodiment 5 being, the charging and discharging currents density of the present embodiment is 1 A/g, and other conditions are the most identical, and it is first
Secondary discharge capacity is 577.4 mAh/g, and coulombic efficiency is 84.13 %, and after circulating 250 times, discharge capacity remains at
288.4 mAh/g。
Embodiment 8
Different from embodiment 5 being, in the present embodiment, electrolyte is 1 M NaClO4/ EC-PC(EC:PC=1:1 volume ratio),
The FEC additive of 10wt%, other conditions are the most identical, assemble sodium-ion battery and test its chemical property.In electric current density it is
During 500 mA/g, its first discharge capacity be 596 mAh/g, coulombic efficiency is 84.41 %, after circulating 200 times, electric discharge hold
Amount remains at 371 mAh/g.
Can draw, the carbon cladding molybdenum sulfide composite of preparation has higher storage as anode material of lithium-ion battery
Sodium capacity, all has the chemical property of excellence, and still has preferable electrification when big electric current under different electric current densities
Learn performance.In charge and discharge process, between molybdenum sulfide and sodium ion, realized the deintercalation of sodium ion by conversion reaction, the carbon of deposition
Layer has rock-steady structure, improves the effect of electric conductivity, makes composite have more excellent chemical property, be that one has very much
The anode material of lithium-ion battery of potentiality.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. the preparation method of a carbon cladding molybdenum sulfide composite, it is characterised in that comprise the steps:
Molybdenum source and sulfur source are dissolved in the water, prepare molybdenum sulfide presoma through hydro-thermal reaction；Molybdenum sulfide presoma is placed in tubular type
In stove, it is passed through carbon source, at molybdenum sulfide presoma surface chemistry vapour deposition carbon, obtains described carbon cladding molybdenum sulfide composite.
The preparation method of a kind of carbon the most according to claim 1 cladding molybdenum sulfide composite, it is characterised in that described molybdenum
Source is more than one in sodium molybdate, ammonium molybdate and molybdenum trioxide；Described sulfur source is thiourea, thioacetamide, ammonium sulfide and sulfur
Change in sodium more than one.
The preparation method of a kind of carbon the most according to claim 1 cladding molybdenum sulfide composite, it is characterised in that described molybdenum
Source is sodium molybdate；Described sulfur source is thiourea.
The preparation method of a kind of carbon the most according to claim 1 cladding molybdenum sulfide composite, it is characterised in that described sulfur
Source is 2:1～12:1 with the mol ratio in molybdenum source；The temperature of described hydro-thermal reaction is 160 DEG C～240 DEG C, and the time is 6h～24h；Institute
Stating carbon source is more than one in methanol, ethanol, toluene, saccharide, oils and fats, organic acid, organic acid esters and small molecular alcohol；Describedization
The temperature learning vapour deposition is 400 DEG C～1000 DEG C, and the time is 1h～10h；Described chemical gaseous phase is deposited on inert gas atmosphere
Under carry out.
The preparation method of a kind of carbon the most according to claim 1 cladding molybdenum sulfide composite, it is characterised in that described sulfur
Source is 2.4:1 with the mol ratio in molybdenum source；The temperature of described hydro-thermal reaction is 220 DEG C, and the time is 24h；Described carbon source is ethanol；Institute
The temperature stating chemical gaseous phase deposition is 500 DEG C, 600 DEG C, 700 DEG C or 800 DEG C；The time of described chemical gaseous phase deposition is 2h；Institute
State chemical gaseous phase deposition to carry out under an argon atmosphere.
6. the carbon cladding molybdenum sulfide composite prepared by preparation method described in any one of claim 1 ~ 5.
7. the carbon cladding molybdenum sulfide composite application in sodium-ion battery described in claim 6, it is characterised in that described
Carbon cladding molybdenum sulfide composite as anode material of lithium-ion battery, by described carbon cladding molybdenum sulfide composite, binding agent,
Conductive agent is mixed and made into slurry in a solvent for 8:1:1 in mass ratio, coats, is dried, and obtains carbon cladding molybdenum sulfide composite
Negative pole.
Carbon cladding molybdenum sulfide composite application in sodium-ion battery the most according to claim 7, it is characterised in that institute
Stating binding agent is more than one in Kynoar, polyacrylic acid, carboxymethyl cellulose, sodium alginate and butadiene-styrene rubber；Institute
Stating conductive agent is more than one in white carbon black, conductive black and Ketjen black；Described solvent is in water and N-Methyl pyrrolidone
More than one.
9. the sodium-ion battery of the carbon cladding molybdenum sulfide composite negative pole obtained based on claim 7, it is characterised in that
This sodium-ion battery includes described carbon cladding molybdenum sulfide composite negative pole, to electrode metal sodium, barrier film and electrolyte system, institute
Stating electrolyte system is containing additive in organic solvent electrolyte or polyelectrolyte, and electrolyte system.
A kind of sodium-ion battery the most according to claim 9, it is characterised in that described electrolyte system is having of sodium salt
Machine dissolvent electrolytic solution, in the organic solvent electrolyte of sodium salt, the concentration of sodium salt is 1 M, and described sodium salt is NaPF6、NaClO4、
NaBF4, more than one in NaTf, NaFSI and NaTFSI；Described organic solvent is Merlon, ethylene carbonate, carbonic acid two
More than one in methyl ester, glycol dimethyl ether, diethyl carbonate, oxolane and triethylene glycol dimethyl ether.；Described additive bag
Including fluorinated ethylene carbonate, the addition of described additive is 5wt%-10 wt%.
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| CN106876702A (en) * | 2017-02-08 | 2017-06-20 | 大连理工大学 | A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation method and application of few layer molybdenum disulfide nano box |
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| CN106876702B (en) * | 2017-02-08 | 2019-10-22 | 大连理工大学 | A kind of preparation method and application of sodium-ion battery cathode |
| CN108878851A (en) * | 2018-07-09 | 2018-11-23 | 郑州轻工业学院 | α-manganese sulfide of one-dimensional porous diamond shape blank pipe shape/molybdenum sulfide@carbon composite preparation method and applications |
| CN108878851B (en) * | 2018-07-09 | 2021-01-26 | 郑州轻工业学院 | Preparation method and application of one-dimensional porous diamond hollow tubular alpha-manganese sulfide/molybdenum sulfide @ carbon composite material |
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