CN106981626B - A kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting cathode - Google Patents
A kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting cathode Download PDFInfo
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- 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
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The invention discloses a kind of tungsten disulfide/Super P sodium-ion battery self-supporting cathode preparation methods, and Super P is compressed into tablet form, electrode support is obtained；Then certain density WO is configured with tungsten powder and hydrogenperoxide steam generator2Solution, then acquired 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 composite material, 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 cathode with a certain amount of thiocarbamide by it.
Description
Technical field
The invention belongs to sodium ion self-supporting cathode preparation fields, and in particular to a kind of tungsten disulfide/Super P sodium ion
The preparation method of battery self-supporting cathode.
Background technique
Lithium ion battery is become with advantages such as high-energy density, high voltage, low self-discharge and excellent cycle performances and is disappeared
The main energy storage device of power-consuming subdomains.However, lithium resource is seldom on the earth, in addition the extensive use of lithium ion battery, so that
Lithium resource is shorter, holds at high price, and is not suitable for extensive stored energy application.Sodium and lithium belong to congeners and 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, have more stable
Chemical property and security performance.And sodium-ion battery and lithium ion battery have similar structure and working 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 there is unique two-dimensional layered structure.Have between tungsten atom and sulphur atom
Strong chemistry key connection, and be to be connected between the sulphur atom of interlayer and sulphur atom by weak molecular link, between layers
Binding force is still Van der Waals force, with MoS2It compares, WS2Interlamellar spacing it is bigger, coefficient of friction is lower, so that it is with a series of
Advantage: WS2It is all insoluble in most media, including water, oil, alkali and majority acid；WS2Thermal stability 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, have 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 is corrosive in medium, abundant surface WS2It can be used as the electrode material of battery, therefore, metal W S in recent years2As
Supercapacitor and sodium ion battery electrode material have received widespread attention.
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, precipitating reduction method etc., there is process conditions complexity to be difficult to control for these methods, equipment is wanted
Ask the problems such as high, reaction ratio is difficult to control, material crystals growth failure, impure, powder is easy to reunite crystallization.
Summary of the invention
The purpose of the present invention is to provide a kind of tungsten disulfide/Super P sodium-ion battery self-supporting cathode preparation sides
Method, to overcome the problems of the above-mentioned prior art, the present invention can prepare the sodium ion with three-dimensional porous connectivity structure
Battery self-supporting cathode.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting cathode, comprising the following steps:
1) it is dissolved in reacting in hydrogenperoxide steam generator after taking tungsten powder to grind and suspending liquid A is made；
2) isopropanol is added into suspending liquid A, stirs to obtain precursor B；
3) ground Super P is pressed into electrode support C；
4) by precursor B be transferred to hydro-thermal induction kettle in, be put into electrode support C, wherein in the B of every 60mL be added 0.1~
0.3g C after sealing kettle, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 400~600KHz by room temperature to
160~200 DEG C, and keep the temperature 4~6h and obtain WO2/ SuperP composite material D；
5) by WO2/ Super P composite material D is washed with deionized water and dehydrated alcohol respectively, is then dried to obtain E；
6) E is buried in thiocarbamide and is sintered to get tungsten disulfide/Super P lithium ion battery self-supporting cathode is arrived.
Further, 1.5g tungsten powder is added in step 1) in every 30mL hydrogenperoxide steam generator.
Further, the mass fraction of hydrogenperoxide steam generator is 30% in step 1).
Further, reaction temperature is 25~40 DEG C in step 1), reaction time 1h.
Further, isopropanol is that analysis is pure in step 2), and 30~40ml isopropanol is added in every 30ml suspending liquid A, makes
It is stirred with magnetic stirring apparatus, speed is 500~700 revs/min, and the time is 30~90min.
Further, pressing pressure is 20~30MPa in step 3), and electrode support C is wide with a thickness of 1mm, a length of 4mm
For 2.5mm.
Further, magnetic induction line of the electrode support C perpendicular to induction coil in hydro-thermal induction heating equipment in step 4)
It places in direction.
Further, at room temperature using deionized water and dehydrated alcohol to WO in step 5)2/ Super P composite material D
It is washed, dehydrated alcohol is that analysis is pure, and drying temperature is 160~200 DEG C, and the time is 8~12h.
Further, E is buried in thiocarbamide completely in step 6), sintering condition are as follows: argon atmosphere, with the liter of 10 DEG C/min
Warm rate keeps the temperature 2h after being warming up to 500 DEG C, then cooled to room temperature.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention uses the WS of hydro-thermal induction heating preparation2The method of/Super P self-supporting electrode.The advantage is that: one
Aspect, prepared WS2WS on/Super P self-supporting electrode2With nanometer chip architecture, uniform small size and fine dispersion
Property, biggish specific surface area is made it have, WS is not only improved2High density filling, and make WS2Nanometer sheet is not easy to fall off, can be with
More sodium storage locations are provided and promote sodium ion in WS2Intercalation/deintercalation in/Super P self-supporting electrode and 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 binder, conductive agent are not used, the capacity of battery is not influenced, shortens 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 heated to higher temperature in a relatively short period of time at first, and active material can be made to be easier to be nucleated in supporting body surface in this way
Growth, so as to improve two alternate interface cohesions, improves the being firmly combined property of electrode, further improves prepared by the present invention
The stability of electrode.
The characteristics of present invention is heated using supporter itself come prepare with excellent interface combine WS2/ Super P is certainly
Electrode is supported, gives full play to the synergistic effect between supporter and active material, and utilize the electrode of invention preparation, interface knot
Close and stablize, nanosizing degree is high, even aperture distribution, overcome conventional electrode materials defect easy to reunite, former capital show compared with
High capacity, excellent cycle performance and high rate performance.
Detailed description of the invention
Fig. 1 is X/ x ray diffraction (XRD) map of sodium-ion battery self-supporting cathode prepared by the embodiment of the present invention 1；
Fig. 2 is scanning electron microscope (SEM) photo (amplification of sodium-ion battery self-supporting cathode 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 cathode prepared by the embodiment of the present invention 1,3.
Specific 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 cathode, comprising the following steps:
1) in the hydrogenperoxide steam generator that the mass fraction for being dissolved in 30mL after taking the tungsten powder of 1.5g to grind is 30%, make its temperature
25~40 DEG C are maintained at, forms suspending liquid A by the reaction of 1h；
2) analytically pure isopropanol is added to A, 30~40ml isopropanol is added in every 30ml suspending liquid A, uses magnetic agitation
Device stirs 30~90min with 500~700 revs/min of speed and forms precursor B；
3) ground Super P is pressed into a thickness of 1mm with the pressure of 20~30MPa using powder compressing machine, it is long
For 4mm, width is the electrode support C of 2.5mm；
4) B is entered in hydro-thermal induction kettle, then C is put perpendicular to the magnetic induction line of induction coil in hydro-thermal induction heating equipment
Enter, wherein 0.1~0.3g C is added in the B of every 60mL, after kettle is sealed, is placed in hydro-thermal induction heating equipment, with 400~
The induction frequencies of 600KHz by room temperature to 160~200 DEG C, and keep the temperature 4~6h obtain WO2/ Super P composite material D；
5) by D respectively with the deionized water and the soft washing of analytically pure dehydrated alcohol that temperature is room temperature, then 160~
Dry 8~12h obtains WO in 200 DEG C of temperature2/ Super P composite material E；
6) E is buried in completely in thiocarbamide, is put into alumina crucible, in tube-type atmosphere furnace (argon gas), with 10 DEG C/min
Heating rate, after being warming up to 500 DEG C keep the temperature 2h obtain the tungsten disulfide with three-dimensional porous connectivity structure/Super P sodium from
Sub- battery self-supporting cathode.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
(1) in the hydrogenperoxide steam generator that the mass fraction for being dissolved in 30mL after taking the tungsten powder of 1.5g to grind is 30%, make its temperature
Degree is maintained at 35 DEG C, forms suspending liquid A by the reaction of 1h；
(2) the analytically pure isopropanol of 35mL is added to A, 60min is stirred with 600 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P is pressed into a thickness of 1mm with the pressure of 25MPa using powder compressing machine, it is a length of
4mm, width are the electrode support C of 2.5mm；
(4) precursor B of 60ml is entered in hydro-thermal induction kettle, by 0.2g C perpendicular to incuding in hydro-thermal induction heating equipment
The magnetic induction line of coil is put into, and after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 500KHz by room temperature liter
Temperature keeps the temperature 5h and obtains WO to 180 DEG C2/ Super P composite material D；
(5) by D respectively with the deionized water and the soft washing of analytically pure dehydrated alcohol that temperature is room temperature, then 180
DEG C temperature in dry 10h obtain WO2/ Super P composite material 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, 2h is kept the temperature after being warming up to 500 DEG C and obtains the tungsten disulfide with three-dimensional porous structure/Super P sodium ion electricity
Pond self-supporting cathode.
It will be seen from figure 1 that self-supporting cathode good crystallinity prepared by the present embodiment 1, purity are higher；It can from Fig. 2
Out, the tungsten disulfide/Super P self-supporting electrode prepared in step (6) has a nanometer chip architecture, uniform small size and fine
Dispersibility；From figure 3, it can be seen that tungsten disulfide/Super P self-supporting cathode prepared by the present embodiment 1 is shown in the battery
Higher capacity, stable cycle performance.
Embodiment 2
(1) in the hydrogenperoxide steam generator that the mass fraction for being dissolved in 30mL after taking the tungsten powder of 1.5g to grind is 30%, make its temperature
Degree is maintained at 40 DEG C, forms suspending liquid A by the reaction of 1h；
(2) the analytically pure isopropanol of 30mL is added to A, 90min is stirred with 500 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P is pressed into a thickness of 1mm with the pressure of 20MPa using powder compressing machine, it is a length of
4mm, width are the electrode support C of 2.5mm；
(4) precursor B of 60ml is entered in hydro-thermal induction kettle, then by 0.3g C perpendicular to feeling in hydro-thermal induction heating equipment
It answers the magnetic induction line of coil to be put into, after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 600KHz by room temperature
200 DEG C are warming up to, and keeps the temperature 4h and obtains WO2/ Super P composite material D；
(5) by D respectively with the deionized water and the soft washing of analytically pure dehydrated alcohol that temperature is room temperature, then 200
DEG C temperature in dry 8h obtain WO2/ Super P composite material 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, 2h is kept the temperature after being warming up to 500 DEG C and obtains the tungsten disulfide with three-dimensional porous structure/Super P sodium ion electricity
Pond self-supporting cathode.
Embodiment 3
(1) in the hydrogenperoxide steam generator that the mass fraction for being dissolved in 30mL after taking the tungsten powder of 1.5g to grind is 30%, make its temperature
Degree is maintained at 35 DEG C, forms suspending liquid A by the reaction of 1h；
(2) the analytically pure isopropanol of 35mL is added to A, 60min is stirred with 600 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P is pressed into a thickness of 1mm with the pressure of 25MPa using powder compressing machine, it is a length of
4mm, width are the electrode support C of 2.5mm；
(4) B is entered in hydro-thermal induction kettle, then by 0.2gC perpendicular to the magnetic strength of induction coil in hydro-thermal induction heating equipment
Line is put into, and after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 500KHz by room temperature to 160 DEG C,
And it keeps the temperature 6h and obtains WO2/ Super P composite material D；
(5) by D respectively with the deionized water and the soft washing of analytically pure dehydrated alcohol that temperature is room temperature, then 160
DEG C temperature in dry 12h obtain WO2/ Super P composite material 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, 2h is kept the temperature after being warming up to 500 DEG C and obtains the tungsten disulfide with three-dimensional porous structure/Super P sodium ion electricity
Pond self-supporting cathode.
Embodiment 4
(1) in the hydrogenperoxide steam generator that the mass fraction for being dissolved in 30mL after taking the tungsten powder of 1.5g to grind is 30%, make its temperature
Degree is maintained at 25 DEG C, forms suspending liquid A by the reaction of 1h；
(2) the analytically pure isopropanol of 40mL is added to A, 30min is stirred with 700 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P is pressed into a thickness of 1mm with the pressure of 30MPa using powder compressing machine, it is a length of
4mm, width are the electrode support C of 2.5mm；
(4) precursor B of 60ml is entered in hydro-thermal induction kettle, then by 0.1g C perpendicular to feeling in hydro-thermal induction heating equipment
It answers the magnetic induction line of coil to be put into, after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 400KHz by room temperature
160 DEG C are warming up to, and keeps the temperature 6h and obtains WO2/ Super P composite material D；
(5) by D respectively with the deionized water and the soft washing of analytically pure dehydrated alcohol that temperature is room temperature, then 160
DEG C temperature in dry 12h obtain WO2/ Super P composite material 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, 2h is kept the temperature after being warming up to 500 DEG C and obtains the tungsten disulfide with three-dimensional porous structure/Super P sodium ion electricity
Pond self-supporting cathode.
Embodiment 5
(1) in the hydrogenperoxide steam generator that the mass fraction for being dissolved in 30mL after taking the tungsten powder of 1.5g to grind is 30%, make its temperature
Degree is maintained at 35 DEG C, forms suspending liquid A by the reaction of 1h；
(2) the analytically pure isopropanol of 35mL is added to A, 60min is stirred with 600 revs/min of speed with magnetic stirring apparatus
Form precursor B；
(3) ground Super P is pressed into a thickness of 1mm with the pressure of 25MPa using powder compressing machine, it is a length of
4mm, width are the electrode support C of 2.5mm；
(4) precursor B of 60ml is entered in hydro-thermal induction kettle, then by 0.1g C perpendicular to feeling in hydro-thermal induction heating equipment
It answers the magnetic induction line of coil to be put into, after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 500KHz by room temperature
180 DEG C are warming up to, and keeps the temperature 5h and obtains WO2/ Super P composite material D；
(5) by D respectively with the deionized water and the soft washing of analytically pure dehydrated alcohol that temperature is room temperature, then 180
DEG C temperature in dry 10h obtain WO2/ Super P composite material 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, 2h is kept the temperature after being warming up to 500 DEG C and obtains the tungsten disulfide with three-dimensional porous structure/Super P sodium ion electricity
Pond self-supporting cathode.
Claims (8)
1. a kind of tungsten disulfide/Super P sodium-ion battery self-supporting cathode preparation method, which is characterized in that including following
Step:
1) it is dissolved in reacting in hydrogenperoxide steam generator after taking tungsten powder to grind and suspending liquid A is made；
2) isopropanol is added into suspending liquid A, stirs to obtain precursor B；
3) ground Super P is pressed into electrode support C；
4) precursor B is transferred in hydro-thermal induction kettle, is put into electrode support C, wherein 0.1~0.3g is added in the B of every 60mL
C after sealing kettle, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 400~600KHz by room temperature to 160~
200 DEG C, and keep the temperature 4~6h and obtain WO2/ Super P composite material D；
5) by WO2/ Super P composite material D is washed with deionized water and dehydrated alcohol respectively, is then dried to obtain E；
6) E is buried in completely in thiocarbamide and is sintered, sintering condition are as follows: argon atmosphere, with the heating rate liter of 10 DEG C/min
Temperature is to 2h is kept the temperature after 500 DEG C, and then cooled to room temperature is to get negative to tungsten disulfide/Super P lithium ion battery self-supporting
Pole.
2. a kind of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting cathode preparation method,
It is characterized in that, 1.5g tungsten powder is added in step 1) in every 30mL hydrogenperoxide steam generator.
3. a kind of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting cathode preparation method,
It is characterized in that, the mass fraction of hydrogenperoxide steam generator is 30% in step 1).
4. a kind of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting cathode preparation method,
It is characterized in that, reaction temperature is 25~40 DEG C in step 1), reaction time 1h.
5. a kind of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting cathode preparation method,
It is characterized in that, isopropanol is that analysis is pure in step 2), 30~40ml isopropanol is added in every 30ml suspending liquid A, uses magnetic force
Blender is stirred, and speed is 500~700 revs/min, and the time is 30~90min.
6. a kind of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting cathode preparation method,
It is characterized in that, pressing pressure is 20~30MPa in step 3), electrode support C is with a thickness of 1mm, a length of 4mm, width
2.5mm。
7. a kind of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting cathode preparation method,
It is characterized in that, electrode support C is put perpendicular to the magnetic induction line direction of induction coil in hydro-thermal induction heating equipment in step 4)
It sets.
8. a kind of tungsten disulfide according to claim 1/Super P sodium-ion battery self-supporting cathode preparation method,
It is characterized in that, at room temperature using deionized water and dehydrated alcohol to WO in step 5)2/ Super P composite material D is washed
It washs, dehydrated alcohol is that analysis is pure, and drying temperature is 160~200 DEG C, and the time is 8~12h.
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| 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 |
| CN111081983B (en) * | 2019-12-26 | 2021-01-29 | 陕西科技大学 | Co9S8Preparation method of self-supporting cathode of carbon felt sodium ion battery |
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