CN106981626A - A kind of preparation method of tungsten disulfide/SuperP sodium-ion battery self-supporting negative poles - Google Patents
A kind of preparation method of tungsten disulfide/SuperP sodium-ion battery self-supporting negative poles Download PDFInfo
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- CN106981626A CN106981626A CN201710262552.3A CN201710262552A CN106981626A CN 106981626 A CN106981626 A CN 106981626A CN 201710262552 A CN201710262552 A CN 201710262552A CN 106981626 A CN106981626 A CN 106981626A
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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
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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- H—ELECTRICITY
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- 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
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting negative poles, Super P are compressed into tablet form, electrode support is obtained；Then certain density WO is configured with tungsten powder and hydrogenperoxide steam generator2Solution, then resulting solution and isopropanol, electrode support are put into water heating kettle, using hydro-thermal induction heating equipment heating and thermal insulation certain time, washing is drying to obtain the WO with three-dimensional porous structure2/ Super P composites, then calcining a period of time in tube-type atmosphere furnace (argon gas) obtains the tungsten disulfide with three-dimensional porous structure/Super P sodium-ion battery self-supporting negative poles with a certain amount of thiocarbamide by it.
Description
Technical field
The invention belongs to sodium ion self-supporting negative pole preparation field, and in particular to a kind of tungsten disulfide/Super P sodium ions
The preparation method of battery self-supporting negative pole.
Background technology
Lithium ion battery is turned into advantages such as high-energy-density, high voltage, low self-discharge and excellent cycle performances and disappeared
The main energy storage device of power-consuming subdomains.However, lithium resource seldom, adds the extensive use of lithium ion battery on the earth so that
Lithium resource is shorter, holds at high price, and is not suitable for extensive stored energy application.Sodium belongs to congeners, and lithium with lithium
With similar physico-chemical property, rich reserves, cheap (the basic raw material trona of sodium is about than the raw material carbonic acid of lithium
Cheap 30~40 times of lithium), and its electrode potential (Na+/ Na) compared with (Li of lithium ion+/ Li) high 0.3V, with what is more stablized
Chemical property and security performance.And sodium-ion battery and lithium ion battery have similar structure and operation principle, therefore, from
Cost, energy consumption, resource angularly for, sodium-ion battery in terms of scale energy storage have bigger market competition advantage.
WS2Crystal structure and MoS2It is similar, all with unique two-dimensional layered structure.Have between tungsten atom and sulphur atom
Strong chemical bond connection, and be connected by weak molecular link between the sulphur atom of interlayer and sulphur atom, between layers
Adhesion is still Van der Waals force, with MoS2Compare, WS2Interlamellar spacing it is bigger, coefficient of friction is lower so that it has a series of
Advantage：WS2All do not dissolved in most media, including water, oil, alkali and majority acid；WS2Heat endurance might as well, in an atmosphere
Decomposition temperature is 510 DEG C, 539 DEG C of rapid oxidations, and decomposition temperature is 1150 DEG C in vacuum；WS2Radiation resistance be better than graphite,
MoS2, with good greasy property, be applicable not only to lubricating condition, be also used as high temperature, high pressure, Gao Zhenrong, high load capacity,
There is radiation and be corrosive in medium, abundant surface WS2Can as battery electrode material, therefore, metal W S in recent years2As
Ultracapacitor and sodium ion battery electrode material are of great interest.
Current existing preparation method has vacuum impregnation technology, gas-phase presulfiding reaction method, chemical vapour deposition technique, surface-active
Agent assisting alcohol-hydrothermal method, thermal decomposition method, precipitation reducing process etc., these methods exist process conditions complexity be difficult to control to, equipment will
Ask high, reaction ratio is difficult to control to, material crystals growth failure, crystallize the problems such as impure, powder is easily reunited.
The content of the invention
It is an object of the invention to provide a kind of preparation side of tungsten disulfide/Super P sodium-ion battery self-supporting negative poles
Method, to overcome the defect that above-mentioned prior art is present, the present invention can prepare the sodium ion with three-dimensional porous connectivity structure
Battery self-supporting negative pole.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting negative poles, comprises the following steps：
1) take tungsten powder to be dissolved in after grinding in hydrogenperoxide steam generator and react obtained suspending liquid A；
2) isopropanol is added into suspending liquid A, precursor B is stirred to obtain；
3) ground Super P are pressed into electrode support C；
4) by precursor B be transferred to hydro-thermal sensing kettle in, be put into electrode support C, wherein per 60mL B in add 0.1~
0.3g C, after kettle is sealed, are placed in hydro-thermal induction heating equipment, with 400~600KHz induction frequencies by room temperature to
160~200 DEG C, and 4~6h of insulation obtains WO2/ SuperP composites D；
5) by WO2/ Super P composites D is washed with deionized water and absolute ethyl alcohol respectively, is then dried to obtain E；
6) E is buried in thiocarbamide and be sintered, that is, obtain tungsten disulfide/Super P lithium ion battery self-supporting negative poles.
Further, step 1) in per 30mL hydrogenperoxide steam generators in add 1.5g tungsten powders.
Further, step 1) in hydrogenperoxide steam generator mass fraction be 30%.
Further, step 1) in reaction temperature be 25~40 DEG C, the reaction time is 1h.
Further, step 2) in isopropanol it is pure to analyze, per 30ml suspending liquid As in add 30~40ml isopropanols, make
It is stirred with magnetic stirring apparatus, speed is 500~700 revs/min, the time is 30~90min.
Further, step 3) in pressing pressure be 20~30MPa, electrode support C thickness be 1mm, a length of 4mm, it is wide
For 2.5mm.
Further, step 4) in electrode support C induction coils in hydro-thermal induction heating equipment magnetic induction line
Place in direction.
Further, step 5) at room temperature using deionized water and absolute ethyl alcohol to WO2/ Super P composites D
Washed, absolute ethyl alcohol is pure to analyze, drying temperature is 160~200 DEG C, the time is 8~12h.
Further, step 6) in E be buried in completely in thiocarbamide, sintering condition is：Argon atmosphere, with 10 DEG C/min liter
Warm speed is warming up to after 500 DEG C and is incubated 2h, then naturally cools to room temperature.
Compared with prior art, the present invention has following beneficial technique effect：
The WS that the present invention is prepared using hydro-thermal sensing heating2The method of/Super P self-supporting electrodes.It the advantage is that：One
Aspect, prepared WS2WS on/Super P self-supporting electrodes2With nanometer chip architecture, uniform small size and fine dispersion
Property, larger specific surface area is made it have, WS is not only improved2High density filling, WS is made again2Nanometer sheet do not allow it is easy to fall off, can be with
More sodium storage locations are provided and promote sodium ion in WS2/ Super P self-supportings electrodes and the intercalation/deintercalation in electrolyte
Reaction, greatly improves the capacity, high rate performance and cycle performance of battery；On the other hand, Super P/WS2Compound method is exempted from
The step of having removed conventional electrode materials film, and without using binding agent, conductive agent, the capacity of battery is not influenceed, shorten production
Cost has been saved while process.
In addition, the present invention is changed in tradition reaction by the way of heat transfer using hydro-thermal induction heating technique, supporter sheet
Body is interior in the short period of time to be heated to higher temperature at first, so active material can be made to be more easy in supporting body surface nucleation
Growth, so as to improve two alternate interface cohesions, improves the being firmly combined with property of electrode, further increases prepared by the present invention
The stability of electrode.
The present invention using supporter in itself heated feature come prepare with excellent interface combination WS2/ Super P are certainly
Electrode is supported, the synergy between supporter and active material, and the electrode prepared using the invention, interface knot is given full play to
Close stable, nanosizing degree is high, even aperture distribution, overcome the defect that conventional electrode materials are easily reunited, former capital show compared with
High capacity, excellent cycle performance and high rate performance.
Brief description of the drawings
Fig. 1 is X/ x ray diffractions (XRD) collection of illustrative plates of sodium-ion battery self-supporting negative pole prepared by the embodiment of the present invention 1；
Fig. 2 is ESEM (SEM) photo (amplification of sodium-ion battery self-supporting negative pole prepared by the embodiment of the present invention 1
20000 times)；
Fig. 3 is the high rate performance figure of sodium-ion battery self-supporting negative pole prepared by the embodiment of the present invention 1,3.
Embodiment
Embodiments of the present invention are described in further detail below：
A kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting negative poles, comprises the following steps：
1) take 1.5g tungsten powder to be dissolved in after grinding in the hydrogenperoxide steam generator that 30mL mass fraction is 30%, make its temperature
25~40 DEG C are maintained at, suspending liquid A is formed by 1h reaction；
2) added to A in analytically pure isopropanol, every 30ml suspending liquid As and add 30~40ml isopropanols, use magnetic agitation
Device stirs 30~90min formation precursor Bs with 500~700 revs/min of speed；
3) ground Super P are pressed into as 1mm by thickness using 20~30MPa pressure using powder compressing machine, it is long
For 4mm, a width of 2.5mm electrode support C；
4) B is entered in hydro-thermal sensing kettle, then the magnetic induction line of induction coil is put in hydro-thermal induction heating equipment by C
Enter, wherein adding 0.1~0.3g C in the B per 60mL, after kettle is sealed, be placed in hydro-thermal induction heating equipment, with 400~
600KHz induction frequencies by room temperature to 160~200 DEG C, and be incubated 4~6h obtain WO2/ Super P composites D；
5) by D respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then 160~
8~12h is dried in 200 DEG C of temperature and obtains WO2/ Super P composites E；
6) E is buried in thiocarbamide completely, is put into alumina crucible, in tube-type atmosphere furnace (argon gas), with 10 DEG C/min
Heating rate, be warming up to after 500 DEG C be incubated 2h obtain the tungsten disulfide with three-dimensional porous connectivity structure/Super P sodium from
Sub- battery self-supporting negative pole.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
(1) take 1.5g tungsten powder to be dissolved in after grinding in the hydrogenperoxide steam generator that 30mL mass fraction is 30%, make its temperature
Degree is maintained at 35 DEG C, and suspending liquid A is formed by 1h reaction；
(2) the analytically pure isopropanols of 35mL are added to A, 60min is stirred with 600 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P are pressed into as 1mm by thickness using 25MPa pressure using powder compressing machine, it is a length of
4mm, a width of 2.5mm electrode support C；
(4) 60ml precursor B is entered in hydro-thermal sensing kettle, 0.2g C is sensed in hydro-thermal induction heating equipment
The magnetic induction line of coil is put into, after kettle is sealed, and is placed in hydro-thermal induction heating equipment, with 500KHz induction frequencies by room temperature liter
Temperature is incubated 5h and obtains WO to 180 DEG C2/ Super P composites D；
(5) by D respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then 180
DEG C temperature in dry 10h obtain WO2/ Super P composites E；
(6) E is buried in thiocarbamide completely, is put into alumina crucible, in tube-type atmosphere furnace (argon gas), with 10 DEG C/min
Heating rate, be warming up to after 500 DEG C and be incubated 2h and obtain the tungsten disulfide with three-dimensional porous structure/Super P sodium ions electricity
Pond self-supporting negative pole.
It will be seen from figure 1 that self-supporting negative pole good crystallinity prepared by the present embodiment 1, purity is higher；Can from Fig. 2
Go out, the tungsten disulfide/Super P self-supporting electrodes prepared in step (6) have a nanometer chip architecture, uniform small size and fine
Dispersiveness；From figure 3, it can be seen that tungsten disulfide/Super P self-supporting negative poles prepared by the present embodiment 1 are shown in the battery
Higher capacity, stable cycle performance.
Embodiment 2
(1) take 1.5g tungsten powder to be dissolved in after grinding in the hydrogenperoxide steam generator that 30mL mass fraction is 30%, make its temperature
Degree is maintained at 40 DEG C, and suspending liquid A is formed by 1h reaction；
(2) the analytically pure isopropanols of 30mL are added to A, 90min is stirred with 500 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P are pressed into as 1mm by thickness using 20MPa pressure using powder compressing machine, it is a length of
4mm, a width of 2.5mm electrode support C；
(4) 60ml precursor B is entered in hydro-thermal sensing kettle, then 0.3g C is felt in hydro-thermal induction heating equipment
Answer the magnetic induction line of coil to be put into, after kettle is sealed, be placed in hydro-thermal induction heating equipment, with 600KHz induction frequencies by room temperature
200 DEG C are warming up to, and is incubated 4h and obtains WO2/ Super P composites D；
(5) by D respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then 200
DEG C temperature in dry 8h obtain WO2/ Super P composites E；
(6) E is buried in thiocarbamide completely, is put into alumina crucible, in tube-type atmosphere furnace (argon gas), with 10 DEG C/min
Heating rate, be warming up to after 500 DEG C and be incubated 2h and obtain the tungsten disulfide with three-dimensional porous structure/Super P sodium ions electricity
Pond self-supporting negative pole.
Embodiment 3
(1) take 1.5g tungsten powder to be dissolved in after grinding in the hydrogenperoxide steam generator that 30mL mass fraction is 30%, make its temperature
Degree is maintained at 35 DEG C, and suspending liquid A is formed by 1h reaction；
(2) the analytically pure isopropanols of 35mL are added to A, 60min is stirred with 600 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P are pressed into as 1mm by thickness using 25MPa pressure using powder compressing machine, it is a length of
4mm, a width of 2.5mm electrode support C；
(4) B is entered in hydro-thermal sensing kettle, then by the magnetic strength of 0.2gC induction coils in hydro-thermal induction heating equipment
Line is put into, after kettle is sealed, and is placed in hydro-thermal induction heating equipment, with 500KHz induction frequencies by room temperature to 160 DEG C,
And be incubated 6h and obtain WO2/ Super P composites D；
(5) by D respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then 160
DEG C temperature in dry 12h obtain WO2/ Super P composites E；
(6) E is buried in thiocarbamide completely, is put into alumina crucible, in tube-type atmosphere furnace (argon gas), with 10 DEG C/min
Heating rate, be warming up to after 500 DEG C and be incubated 2h and obtain the tungsten disulfide with three-dimensional porous structure/Super P sodium ions electricity
Pond self-supporting negative pole.
Embodiment 4
(1) take 1.5g tungsten powder to be dissolved in after grinding in the hydrogenperoxide steam generator that 30mL mass fraction is 30%, make its temperature
Degree is maintained at 25 DEG C, and suspending liquid A is formed by 1h reaction；
(2) the analytically pure isopropanols of 40mL are added to A, 30min is stirred with 700 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P are pressed into as 1mm by thickness using 30MPa pressure using powder compressing machine, it is a length of
4mm, a width of 2.5mm electrode support C；
(4) 60ml precursor B is entered in hydro-thermal sensing kettle, then 0.1g C is felt in hydro-thermal induction heating equipment
Answer the magnetic induction line of coil to be put into, after kettle is sealed, be placed in hydro-thermal induction heating equipment, with 400KHz induction frequencies by room temperature
160 DEG C are warming up to, and is incubated 6h and obtains WO2/ Super P composites D；
(5) by D respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then 160
DEG C temperature in dry 12h obtain WO2/ Super P composites E；
(6) E is buried in thiocarbamide completely, is put into alumina crucible, in tube-type atmosphere furnace (argon gas), with 10 DEG C/min
Heating rate, be warming up to after 500 DEG C and be incubated 2h and obtain the tungsten disulfide with three-dimensional porous structure/Super P sodium ions electricity
Pond self-supporting negative pole.
Embodiment 5
(1) take 1.5g tungsten powder to be dissolved in after grinding in the hydrogenperoxide steam generator that 30mL mass fraction is 30%, make its temperature
Degree is maintained at 35 DEG C, and suspending liquid A is formed by 1h reaction；
(2) the analytically pure isopropanols of 35mL are added to A, 60min is stirred with 600 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P are pressed into as 1mm by thickness using 25MPa pressure using powder compressing machine, it is a length of
4mm, a width of 2.5mm electrode support C；
(4) 60ml precursor B is entered in hydro-thermal sensing kettle, then 0.1g C is felt in hydro-thermal induction heating equipment
Answer the magnetic induction line of coil to be put into, after kettle is sealed, be placed in hydro-thermal induction heating equipment, with 500KHz induction frequencies by room temperature
180 DEG C are warming up to, and is incubated 5h and obtains WO2/ Super P composites D；
(5) by D respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then 180
DEG C temperature in dry 10h obtain WO2/ Super P composites E；
(6) E is buried in thiocarbamide completely, is put into alumina crucible, in tube-type atmosphere furnace (argon gas), with 10 DEG C/min
Heating rate, be warming up to after 500 DEG C and be incubated 2h and obtain the tungsten disulfide with three-dimensional porous structure/Super P sodium ions electricity
Pond self-supporting negative pole.
Claims (9)
1. the preparation method of a kind of tungsten disulfide/Super P sodium-ion battery self-supporting negative poles, it is characterised in that including following
Step：
1) take tungsten powder to be dissolved in after grinding in hydrogenperoxide steam generator and react obtained suspending liquid A；
2) isopropanol is added into suspending liquid A, precursor B is stirred to obtain；
3) ground Super P are pressed into electrode support C；
4) precursor B is transferred in hydro-thermal sensing kettle, is put into electrode support C, wherein adding 0.1~0.3g in the B per 60mL
C, after kettle is sealed, is placed in hydro-thermal induction heating equipment, with 400~600KHz induction frequencies by room temperature to 160~
200 DEG C, and 4~6h of insulation obtains WO2/ Super P composites D；
5) by WO2/ Super P composites D is washed with deionized water and absolute ethyl alcohol respectively, is then dried to obtain E；
6) E is buried in thiocarbamide and be sintered, that is, obtain tungsten disulfide/Super P lithium ion battery self-supporting negative poles.
2. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 1) in per 30mL hydrogenperoxide steam generators in add 1.5g tungsten powders.
3. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 1) in hydrogenperoxide steam generator mass fraction be 30%.
4. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 1) in reaction temperature be 25~40 DEG C, the reaction time is 1h.
5. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 2) in isopropanol it is pure to analyze, per 30ml suspending liquid As in add 30~40ml isopropanols, use magnetic force
Agitator is stirred, and speed is 500~700 revs/min, and the time is 30~90min.
6. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 3) in pressing pressure be 20~30MPa, electrode support C thickness be 1mm, a length of 4mm, it is a width of
2.5mm。
7. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 4) in electrode support C put in the magnetic induction line direction of induction coil in hydro-thermal induction heating equipment
Put.
8. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 5) at room temperature using deionized water and absolute ethyl alcohol to WO2/ Super P composites D is washed
Wash, absolute ethyl alcohol is pure to analyze, drying temperature is 160~200 DEG C, the time is 8~12h.
9. a kind of preparation method of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting negative poles,
Characterized in that, step 6) in E be buried in completely in thiocarbamide, sintering condition is：Argon atmosphere, with 10 DEG C/min heating rate
It is warming up to after 500 DEG C and is incubated 2h, then naturally cools to room temperature.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108110246A (en) * | 2017-12-22 | 2018-06-01 | 陕西科技大学 | A kind of extra small VS4/ Super P composite nano-powders and preparation method and application |
| CN108550846A (en) * | 2018-04-24 | 2018-09-18 | 中国科学院福建物质结构研究所 | Tungsten disulfide negative material for potassium ion secondary cell |
| CN111081983A (en) * | 2019-12-26 | 2020-04-28 | 陕西科技大学 | Co9S8Preparation method of self-supporting cathode of carbon felt sodium ion battery |
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| CN108110246A (en) * | 2017-12-22 | 2018-06-01 | 陕西科技大学 | A kind of extra small VS4/ Super P composite nano-powders and preparation method and application |
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| CN111081983A (en) * | 2019-12-26 | 2020-04-28 | 陕西科技大学 | Co9S8Preparation method of self-supporting cathode of carbon felt sodium ion battery |
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