CN110459745A - A kind of Ni3S2@VO2The preparation method of nanocomposite - Google Patents
A kind of Ni3S2@VO2The preparation method of nanocomposite Download PDFInfo
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- CN110459745A CN110459745A CN201910737068.0A CN201910737068A CN110459745A CN 110459745 A CN110459745 A CN 110459745A CN 201910737068 A CN201910737068 A CN 201910737068A CN 110459745 A CN110459745 A CN 110459745A
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- nanocomposite
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- vanadium
- sulphur
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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
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 present invention relates to energy storage material field, specifically a kind of Ni3S2@VO2The preparation method of nanocomposite, for the method using sulphur source, vanadium source as presoma, deionized water is solvent, and pretreated nickel foam is substrate, after calcining by hydro-thermal reaction and in an inert atmosphere, synthesize described in Ni3S2@VO2Nanocomposite.The present invention improves its chemical property by constructing binary metal composite material, and then improve the capacity and stability of Zinc ion battery, material prepared by the present invention can be widely applied to Zinc ion battery by being combined together two kinds of metal cations.Preparation method of the present invention is easy to operate, abundant raw material, and preparation cost is low；Prepared Ni3S2@VO2Nanocomposite electrochemical performance, the comprehensive performance for improving Zinc ion battery have great meaning.
Description
Technical field
The present invention relates to energy storage material technical field, especially a kind of Ni3S2@VO2The preparation method of nanocomposite.
Background technique
Energy and environment problem has been acknowledged as most challenging two significant problems faced 21 century.With work
The fast development of industry and science and technology, world population explode, and people are growing day by day to the consumption of the energy and demand.The mankind are disappeared at present
The energy of consumption mainly includes petroleum, coal, natural gas etc., and wherein renewable energy is only accounted for less than 10%.It is aobvious according to related data
Show, between past 30 years, the consumption of petroleum is dramatically increased, and corresponding CO2 emissions also sharply increase.More worth note
Meaning, it was predicted that whole world reserves is only enough exploited 30~40 years, natural gas about 60 years.
It is developed other than finding the non-renewable energy resources new, renewable energy is to replace current sternness for this phenomenon
The energy stores and reforming unit of novel high-performance are also key point.
Again in past decades, a large amount of focus has been placed on new and effective electrochemical energy storage by numerous scientists
On device.Wherein, since zinc resource is abundant, at low cost, high (the 819mAh g of theoretical capacity-1) and the reasons such as environmentally friendly,
Metallic zinc is considered as most one of the negative electrode material of prospect in new energy device field.Therefore, water system Zinc ion battery
It is considered to have the energy storage device of new generation of very big prospect.However, regrettably, in addition to the dendrite that zinc load generates is asked
The positive electrode capacity of outlying, Zinc ion battery is low, and the factors such as cyclical stability difference also result in the capacity benefit of Zinc ion battery
With low and literary shining stability difference of rate etc..Therefore, in order to further develop Zinc ion battery, and promote its development, exploitation one
Kind of high capacity, high stability the positive electrode of Zinc ion battery be crucial.
Since with high electrical conductivity, (conductivity at normal temperature is 5.5 × 104S cm-1) and with reversible electrification
Performance is learned, nickel sulfide has been used preliminarily in Zinc ion battery as a kind of emerging electrode material.However, nickel sulfide is low
Hypovolemic and low stability limits its further development in Zinc ion battery.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of Ni3S2@VO2The preparation method of nanocomposite, this hair
It is bright to improve its chemical property by constructing binary metal composite material by being combined together two kinds of metal cations,
And then the capacity and stability of Zinc ion battery are improved, material prepared by the present invention can be widely applied to Zinc ion battery.
The technical solution of the present invention is as follows: a kind of Ni3S2@VO2The preparation method of nanocomposite, the method is with sulphur
Source, vanadium source are presoma, and deionized water is solvent, and pretreated nickel foam is substrate, by hydro-thermal reaction and in indifferent gas
After calcining in atmosphere, the Ni is synthesized3S2@VO2Nanocomposite；
Specifically includes the following steps:
S1), nickel foam is successively immersed in acetone, 3mol L-1Be cleaned by ultrasonic respectively in hydrochloric acid, ethyl alcohol 10min, 5min,
5min is placed in hydrothermal reaction kettle；
S2), sulphur source and vanadium source are dissolved in deionized water, are poured into this hydrothermal reaction kettle after mixing evenly, 100~
2~8h is reacted in 220 DEG C of baking oven, is taken out, through distilled water flushing, 60 DEG C of drying；
S3), sample obtained in step S2) is placed in the small tube furnace for being connected with the inert atmosphere that flow velocity is 200sccm,
100~400 DEG C at a temperature of carry out 0.5~3h of calcining, take out to get the Ni is arrived3S2@VO2Material.
Preferably, in the above method, the sulphur source be thioacetamide, thiocarbamide, vulcanized sodium, cysteine etc. one kind or
A variety of mixing.
Preferably, in the above method, the concentration of the sulphur source is 0.01~0.2mol L-1。
It is furthermore preferred that the sulphur source is thioacetamide in the above method.
It is furthermore preferred that the concentration of the sulphur source is 0.05mol L in the above method-1。
Preferably, in the above method, the vanadium source is one kind or more of sodium vanadate, ammonium vanadate, sodium metavanadate, potassium vanadate etc.
The mixing of kind.
Preferably, in the above method, the concentration in the vanadium source is 0.01~0.2mol L-1。
It is highly preferred that the vanadium source is sodium vanadate in the above method.
It is highly preferred that the concentration in the vanadium source is 0.05mol L in the above method-1。
Preferably, in the above method, the inert atmosphere is nitrogen, one kind of argon gas or 2 kinds of mixing.
Preferably, in the above method, the atmosphere flow velocity is 50~400sccm.
It is highly preferred that the inert atmosphere is nitrogen in the above method.
It is highly preferred that the atmosphere flow velocity is 200sccm in the above method.
Preferably, in the above method, the hydrothermal temperature is 180 DEG C, and the hydro-thermal reaction time is 4h.
Preferably, in the above method, the calcination temperature is 200 DEG C, and the calcination time is 1h.
The invention has the benefit that
1, preparation method is easy to operate, abundant raw material, and preparation cost is low；
2, prepared Ni3S2@VO2Nanocomposite electrochemical performance, for improving the synthesis of Zinc ion battery
Performance has great meaning.
3, the present invention is improved by being combined together two kinds of metal cations by constructing binary metal composite material
Its chemical property, and then the capacity and stability of Zinc ion battery are improved, material prepared by the present invention can be widely applied to zinc
Ion battery.
Detailed description of the invention
Fig. 1 is high and low multiplying power scanning electron microscope (SEM) figure of material prepared by the embodiment of the present invention 1 and 2, wherein a is
Ni3S2High and low multiplying power scanning electron microscope (SEM) figure, be (b) Ni in embodiment 13S2@VO2High and low multiplying power scanning electron microscope (SEM)
Figure；
Fig. 2 is Ni in the embodiment of the present invention 1,23S2And Ni3S2@VO2X-ray diffraction (XRD) spectrogram；
Ni in Fig. 3 embodiment 13S2@VO2Energy dispersion X-ray spectrum (EDX) figure and element mapping image
(Mapping)；
Fig. 4 is the Ni in embodiment 13S2@VO2With the Ni in embodiment 23S2It is 6mol L in electrolyte-1In KOH solution
With the cyclic voltammetry curve figure swept under speed；
Fig. 5 is the Ni in embodiment 13S2@VO2With the Ni in embodiment 23S2Constant current charge and discharge under same current density
Electric curve graph；
Fig. 6 is with the Ni in embodiment 13S2@VO2For positive electrode, zinc metal sheet is the nickel-zinc cell of negative electrode material assembling not
With the constant current charge-discharge curve graph under current density；
Fig. 7 is with the Ni in embodiment 13S2@VO2For positive electrode, zinc metal sheet is times of the nickel-zinc cell of negative electrode material assembling
Rate performance map；
Fig. 8 is respectively with the Ni in embodiment 13S2@VO2With the Ni in embodiment 23S2For positive electrode, zinc metal sheet is cathode
Material, the nickel-zinc cell assembled are 40mA cm in current density-2Under stable circulation performance figure.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing:
Embodiment 1
A kind of Ni3S2@VO2The preparation method of nanocomposite, comprising the following steps:
S1), the nickel foam of 2cm × 3cm is successively immersed in acetone, 3mol L-1It is cleaned by ultrasonic respectively in hydrochloric acid, ethyl alcohol
10min, 5min, 5min are placed in hydrothermal reaction kettle；
It S2), will be 0.05mol L by concentration-1Sodium vanadate and 0.05mol L-1Thioacetamide is dissolved in 60mL deionized water
In, it is poured into this hydrothermal reaction kettle after mixing evenly, 4h is reacted in 180 DEG C of baking oven, taken out, through distilled water flushing, 60 DEG C
Drying；
S3), sample obtained in step S2) is placed in the small tube furnace for being connected with the nitrogen atmosphere that flow velocity is 200sccm,
200 DEG C at a temperature of carry out calcining 1h, take out to get the Ni is arrived3S2@VO2Material.
Embodiment 2
Ni3S2The preparation of material
S1), the nickel foam of 2cm × 3cm is successively immersed in acetone, 3mol L-1It is cleaned by ultrasonic respectively in hydrochloric acid, ethyl alcohol
10min, 5min, 5min are placed in hydrothermal reaction kettle；
It S2), will be 0.05mol L by concentration-1Thioacetamide be dissolved in 60mL deionized water, pour into after mixing evenly
In this hydrothermal reaction kettle, 4h is reacted in 180 DEG C of baking oven, is taken out, through distilled water flushing, 60 DEG C of drying；
S3), sample obtained in step S2) is placed in the small tube furnace for being connected with the nitrogen atmosphere that flow velocity is 200sccm,
200 DEG C at a temperature of carry out calcining 1h, take out to get the Ni is arrived3S2Material.
Performance test
Ni prepared by embodiment 1 and embodiment 23S2@VO2Material and Ni3S2Flied emission scanning electron microscopy electricity is carried out
Mirror test, test results are shown in figure 1, it can be seen from the figure that scanning electron microscopy electron microscope shows that two kinds of materials are all
Nano-bar material；
Fig. 2 uses X-ray diffraction and tests the material prepared to embodiment 1 and embodiment 2, it can be seen from the figure that institute
The electrode material of preparation synthesis is Ni3S2And Ni3S2@VO2。
Fig. 3 is Ni3S2@VO2Energy dispersion X-ray spectrum (EDX) figure and element mapping image (Mapping), from
As can be seen that illustrating the presence of Ni, S, V, O element in figure.
Fig. 4 uses the cyclic voltammetry in electrochemical method, and Fig. 5 uses the constant current charge-discharge in electrochemical method
To study its capacitive property, (electrolyte is 6mol L for test-1KOH), by being calculated, Ni3S2@VO2Electrode material is in electric current
Density is 40mA cm-2When area ratio capacitance be 0.33mAh cm-2, it is Ni3S2Electrode material is below same current density
Product specific capacitance value (0.06mAh cm-2) 5.5 times.
Fig. 6 is with Ni3S2@VO2For positive electrode, zinc metal sheet is negative electrode material, and the nickel-zinc cell assembled is in different electric currents
Constant current charge-discharge curve under density, Fig. 7 are with Ni3S2@VO2For positive electrode, zinc metal sheet is the nickel zinc electricity of negative electrode material assembling
The high rate performance in pond, Fig. 8 are respectively with Ni3S2@VO2And Ni3S2For positive electrode, zinc metal sheet is negative electrode material, the nickel assembled
Zinc battery (is denoted as Ni respectively3S2@VO2//Zn and Ni3S2//Zn) stable circulation performance, by being calculated, ultrasonic vulcanization is obtained
The Ni arrived3S2@VO2//Zn battery is 40mA cm in current density-2Under, after 2000 cycle charge-discharges, capacitance without
Significantly sacrificing, and Ni3S2Capacity retention ratio of the //Zn battery after 2000 cycle charge-discharges is only 70.66%.Show to pass through
The Ni that ultrasonic vulcanization obtains3S2@VO2Electrode material have good energy-storage property, this for improve nickel-zinc cell comprehensive performance
With great meaning.
Embodiment 3-14
It influences to close by regulating and controlling different precursor concentration, hydrothermal reaction condition and calcination condition based on embodiment 1
At Ni3S2@VO2Performance, relationship is as shown in table 1.
The synthesis of 1 embodiment 3-14 of table adjusts and result
Wherein, embodiment 1,3~6 illustrates precursor concentration to Ni3S2@VO2Chemical property influenced, embodiment
1,7~10 and 1,11~14 it hydrothermal reaction condition and calcination condition are respectively illustrated can also influence Ni to a certain extent3S2@
VO2Chemical property.Ni in the embodiment 2~143S2Chemical property not as good as embodiment 1.
The above embodiments and description only illustrate the principle of the present invention and most preferred embodiment, is not departing from this
Under the premise of spirit and range, various changes and improvements may be made to the invention, these changes and improvements both fall within requirement and protect
In the scope of the invention of shield.
Claims (10)
1. a kind of Ni3S2@VO2The preparation method of nanocomposite, the method is using sulphur source, vanadium source as presoma, deionization
Water is solvent, and pretreated nickel foam is substrate, after calcining by hydro-thermal reaction and in an inert atmosphere, synthesize described in
Ni3S2@VO2Nanocomposite；
Specifically includes the following steps:
S1), nickel foam is successively immersed in acetone, 3mol L-1It is cleaned by ultrasonic 10min, 5min, 5min respectively in hydrochloric acid, ethyl alcohol, puts
It sets in hydrothermal reaction kettle；
S2), sulphur source and vanadium source are dissolved in deionized water, are poured into this hydrothermal reaction kettle after mixing evenly, at 100~220 DEG C
Baking oven in react 2~8h, take out, through distilled water flushing, 60 DEG C of drying；
S3), sample obtained in step S2) is placed in the small tube furnace for being connected with the inert atmosphere that flow velocity is 200sccm, In
0.5~3h of calcining is carried out at a temperature of 100~400 DEG C, is taken out to get the Ni is arrived3S2@VO2Material.
2. a kind of Ni according to claim 13S2@VO2The preparation method of nanocomposite, it is characterised in that: the sulphur
Source is one or more mixing of thioacetamide, thiocarbamide, vulcanized sodium, cysteine etc..
3. a kind of Ni according to claim 23S2@VO2The preparation method of nanocomposite, it is characterised in that: the sulphur
The concentration in source is 0.01~0.2mol L-1。
4. a kind of Ni according to claim 33S2@VO2The preparation method of nanocomposite, it is characterised in that: the sulphur
Source is thioacetamide, and the concentration of the sulphur source is 0.05mol L-1。
5. a kind of Ni according to claim 13S2@VO2The preparation method of nanocomposite, it is characterised in that: the vanadium
Source is one or more mixing of sodium vanadate, ammonium vanadate, sodium metavanadate, potassium vanadate etc..
6. a kind of Ni according to claim 53S2@VO2The preparation method of nanocomposite, it is characterised in that: the vanadium
The concentration in source is 0.01~0.2mol L-1。
7. a kind of Ni according to claim 63S2@VO2The preparation method of nanocomposite, it is characterised in that: the vanadium
Source is sodium vanadate, and the concentration in the vanadium source is 0.05mol L-1。
8. a kind of Ni according to claim 13S2@VO2The preparation method of nanocomposite, it is characterised in that: described lazy
Property atmosphere be nitrogen, one kind of argon gas or 2 kinds of mixing, the atmosphere flow velocity be 50~400sccm.
9. a kind of Ni according to claim 83S2@VO2The preparation method of nanocomposite, it is characterised in that: described lazy
Property atmosphere be nitrogen, the atmosphere flow velocity be 200sccm.
10. a kind of Ni according to claim 13S2@VO2The preparation method of nanocomposite, it is characterised in that: described
Hydrothermal temperature is 180 DEG C, and the hydro-thermal reaction time is 4h；
The calcination temperature is 200 DEG C, and the calcination time is 1h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113802139A (en) * | 2021-09-13 | 2021-12-17 | 陕西科技大学 | Nickel sulfide based electrocatalytic material with core-shell structure and preparation method and application thereof |
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