CN110010872A - A kind of MoS2@CuS hetero-junctions anode of magnesium ion battery material and preparation method and application - Google Patents
A kind of MoS2@CuS hetero-junctions anode of magnesium ion battery material and preparation method and application Download PDFInfo
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- CN110010872A CN110010872A CN201910276450.6A CN201910276450A CN110010872A CN 110010872 A CN110010872 A CN 110010872A CN 201910276450 A CN201910276450 A CN 201910276450A CN 110010872 A CN110010872 A CN 110010872A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/58—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
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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
A kind of MoS2@CuS hetero-junctions anode of magnesium ion battery material and preparation method and application, MoS2Account for x=60~80wt%, remaining be CuS material, preparation method include respectively weighed sodium molybdate, hydroxylamine hydrochloride and thiocarbamide be dissolved in deionized water, obtain solution A；Using magnetic agitation, the cetyl trimethylammonium bromide (CTAB) being added in Xiang Shangshu solution A adjusts PH with hydrochloric acid, obtains solution B；Under the conditions of magnetic agitation, CuCl is added in Xiang Shangshu solution B2·2H2O obtains solution C；Above-mentioned solution C is transferred to hydrothermal reaction kettle, hydro-thermal reaction is carried out, cools down after reaction, product is cleaned with deionized water and ethyl alcohol after reaction, and it is dry, obtain nano flower-like MoS2@CuS heterojunction composite, the present invention are formed by positive electrode in conjunction with firm, stable structure, should not collapse, can be obviously improved the cyclical stability of battery.
Description
Technical field
The present invention relates to secondary power battery material technical field, in particular to a kind of MoS2@CuS hetero-junctions magnesium ion electricity
Pond positive electrode and preparation method and application.
Background technique
The high speed development of world economy has benefited from the extensive use of fossil energy, but fossil energy is non-renewable and uses
Cheng Zhonghui discharge it is a large amount of harmful other, cause environmental pollution, and fossil energy will certainly face exhausted ask in the near future
Topic.The problems such as alleviating energy crisis and environmental pollution, the clean reproducible energy for finding alternative fossil energy has become
The task of top priority.
Lithium ion battery is since its high capacity and stable cycle life are by various electronic equipments (such as digital camera, hand
Mechanical, electrical brain etc.) it is widely used.Science and technology is constantly progressive, and Mobile portable equipment increasingly increases, to the demand and requirement of energy storage device
It is continuously improved.However, lithium ion battery is increasingly significant because of the disadvantages of its cost is excessively high, resource is limited, safety, limited capacity.
Lithium ion battery will not be able to the requirement for meeting equipment in the near future, and lithium ion battery will be unable to better " driving " future
Life.In order to better meet people's life requirement, it is necessary to research and develop the energy-storage battery of novel high-capacity safety.Mg, Al
With the batteries such as Ca because of itself remarkable advantage, causes people and greatly pay close attention to.Wherein, rechargeable magnesium cell because its Gao Tianran it is rich
Degree, air stability, low cost, high capacity, high security and ecology friendly and be considered as most potential ion battery
One of.2205mAhg may be implemented in Mg ion battery-1High theoretical specific capacity and up to 3833mAhcm-3Volume hold
Amount.Most of all, Mg metal electrode avoids forming skeleton in cyclic process, the safety of battery is improved, is had
Effect reduces the risk in battery use process.Chalcogen compound is relatively low ionic and show huge due to it
Advantage.But due to Mg2+There are two unit positive charges for ion itself band, cause charge density higher, Mg2+Ion and main body
The effect of storeroom coulomb is larger, makes Mg2+Ion spreads difficulty in interstitial void, causes the electrochemical utilization rate and multiplying power of material
Performance is poor.
The high theoretical specific capacity of sulphur and sulphur composite material becomes very attractive anode of magnesium ion battery material.Sulphur
Changing copper has moderate theoretical specific capacity (560m Ah g-1) and good conductivity (10-3S·cm-1).Therefore, CuS has more
High active material utilization and higher coulombic efficiency.MoS2It is a kind of promising two-dimentional (2D) graphite alkenes stratiform knot of tool
Structure, S-Mo-S layers are linked together by weak Van der Waals force.MoS2Big middle layer (0.62nm) not only promote ion layer it
Between space in be freely embeddable and deviate from, and volume caused by also acting as buffer matrix to mitigate because of ion intercalation/deintercalation
Variation.But simple MoS2Part magnesium ion can not deviate from from host structure in material, after being suitably introduced into copper ion, magnesium from
Son can all be deviate from from host structure, to promote the coulombic efficiency and charge/discharge capacity of example battery.At present by from
Son doping can improve the above problem, but doping way is often the extensive technique such as ball milling, and there are doping problem of non-uniform, separately
Outside, after doping, contact of the ion with basis material be not firm, and repeatedly after circulation, electrode material structure is often because ion is embedding
Enter stress caused by deviating from and collapse, so as to cause circulating battery capacity attenuation.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of MoS2@CuS hetero-junctions magnesium from
Sub- cell positive material and preparation method and application enhances the electric conductivity of Magnesium ion battery and provides more activity
Site, and the present invention uses a step hydro-thermal mode originally for synthesis CuS MoS2Hetero-junctions, be formed by positive electrode combine it is firm,
Stable structure should not collapse, and can be obviously improved the cyclical stability of battery.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of MoS2@CuS hetero-junctions anode of magnesium ion battery material, the MoS2@CuS hetero-junctions Magnesium ion battery is just
In the material of pole, MoS2X=60~80wt% is accounted for, remaining is CuS material.
A kind of MoS2The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, includes the following steps；
Step 1:
The thiocarbamide for weighing the sodium molybdate of 0.5~1.0g, the hydroxylamine hydrochloride of 0.6~1.2g and 1.0~2.0g respectively is dissolved in
In 50mL deionized water, solution A is obtained；
Step 2:
Using magnetic agitation, the cetyl trimethylammonium bromide of 0.03~0.18g is added in Xiang Shangshu solution A
(CTAB), it is 6 or so with the hydrochloric acid adjustment PH of 2mol/L, obtains solution B；
Step 3:
Under the conditions of magnetic agitation, the CuCl of 0.1~0.2g is added in Xiang Shangshu solution B2·2H2O obtains solution C；
Step 4:
Above-mentioned solution C is transferred to hydrothermal reaction kettle, hydro-thermal reaction is carried out, cools down after reaction, product is used after reaction
Deionized water and ethyl alcohol cleaning, it is dry, obtain nano flower-like MoS2@CuS heterojunction composite.
Magnetic agitation condition is 400rap/min in the step two.
Magnetic agitation condition is 600rap/min in the step three.
In the step four, high temperature hydrothermal temperature be 180 DEG C~220 DEG C, the reaction time be 16~for 24 hours.
The drying temperature is 80 DEG C.
A kind of MoS2The application of@CuS anode of magnesium ion battery material nano structure, by the nano flower-like MoS of 70wt%2@
The binder of CuS heterojunction composite, the conductive auxiliary agent (Super P) of 15wt% and 15wt%, which is put into mortar, sufficiently to be ground
Mill, by the sample mud blade coating mixed on copper foil, is subsequently placed into 12h in 120 DEG C of vacuum drying ovens, keeps it sufficiently dry
Dry, fibreglass diaphragm is battery diaphragm, is assembled into button cell；After assembled button cell is stood 12h,
LANDCT2100A carries out electrochemical property test, and test voltage is 0.01V~3.0V, current density 100mA/g.
Beneficial effects of the present invention:
Invention enhances the electric conductivity of Magnesium ion battery, proportion of the present invention by control reaction dissolvent, reaction temperature
The size for improving hetero-junctions, pattern and structure are spent with soaking time.MoS prepared by the present invention2@CuS hetero-junctions nanostructure
Large specific surface area, have in charge and discharge process very large space store magnesium ion, be conducive to Mg2+Cation diffusion and storage.
Invention enhances the electric conductivity of Magnesium ion battery and more active sites are provided, and the present invention uses a step hydro-thermal side
Formula was synthesis CuS MoS originally2Hetero-junctions is formed by positive electrode in conjunction with firm, stable structure, should not collapse, can significantly mention
Rise the cyclical stability of battery.CuS@MoS2The flower-shaped heterojunction material of composite Nano is living as a kind of novel magnesium ion anode
Property material, is expected to the advantage respectively by chemically combined two kinds of sulfide, the i.e. electric conductivity of CuS and MoS2Layer structure and
Activity promotes ion intercalation/deintercalation dynamics problem, so as to improve the charge/discharge capacity of Magnesium ion battery, dynamics and circulation
Stability problem.
Detailed description of the invention
Fig. 1 is synthesized CuS@MoS2The shape appearance figure of the flower-shaped heterojunction structure of composite Nano.
Fig. 2 is the face power spectrum mapping figure under transmission electron microscope.
Fig. 3 is the distribution map of element sulphur S in face power spectrum mapping figure.
Fig. 4 is the distribution map of copper Cu in face power spectrum mapping figure.
Fig. 5 is the distribution map of molybdenum element Mo in face power spectrum mapping figure.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1
A kind of MoS2The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, includes the following steps；
Step 1:
The thiocarbamide for weighing the sodium molybdate of 0.5g, the hydroxylamine hydrochloride of 0.6g and 1.0g respectively is dissolved in 50mL deionized water,
Obtain solution A；
Step 2:
Using magnetic agitation, magnetic agitation condition is 400rap/min, and the hexadecane of 0.03g is added in Xiang Shangshu solution A
Base trimethylammonium bromide (CTAB) is 6 or so with the hydrochloric acid adjustment PH of 2mol/L, obtains solution B；
Step 3:
Under the conditions of magnetic agitation, the CuCl of 0.1g is added in 600rap/min, Xiang Shangshu solution B2·2H2O obtains solution C；
Step 4:
Above-mentioned solution C is transferred to hydrothermal reaction kettle, carries out hydro-thermal reaction, high temperature hydrothermal temperature is 180 DEG C, reaction
Time is 16h, is cooled down after reaction, and product is cleaned with deionized water and ethyl alcohol after reaction, dry at a temperature of 80 DEG C, is received
Popped rice shape MoS2@CuS heterojunction composite.
Embodiment 2
A kind of MoS2The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, includes the following steps；
Step 1:
The thiocarbamide for weighing the sodium molybdate of 1.0g, the hydroxylamine hydrochloride of 1.2g and 2.0g respectively is dissolved in 50mL deionized water,
Obtain solution A；
Step 2:
Using magnetic agitation, magnetic agitation condition is 400rap/min, and the hexadecane of 0.18g is added in Xiang Shangshu solution A
Base trimethylammonium bromide (CTAB) is 6 or so with the hydrochloric acid adjustment PH of 2mol/L, obtains solution B；
Step 3:
Under the conditions of magnetic agitation, the CuCl of 0.2g is added in 600rap/min, Xiang Shangshu solution B2·2H2O obtains solution C；
Step 4:
Above-mentioned solution C is transferred to hydrothermal reaction kettle, carries out hydro-thermal reaction, high temperature hydrothermal temperature is 220 DEG C, reaction
Time is for 24 hours, to cool down after reaction, and product is cleaned with deionized water and ethyl alcohol after reaction, dry at a temperature of 80 DEG C, is received
Popped rice shape MoS2@CuS heterojunction composite.
Embodiment 3
A kind of MoS2The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, includes the following steps；
Step 1:
The thiocarbamide for weighing the sodium molybdate of 0.8g, the hydroxylamine hydrochloride of 1.0g and 1.5g respectively is dissolved in 50mL deionized water,
Obtain solution A；
Step 2:
Using magnetic agitation, magnetic agitation condition is 400rap/min, and the hexadecane of 0.10g is added in Xiang Shangshu solution A
Base trimethylammonium bromide (CTAB) is 6 or so with the hydrochloric acid adjustment PH of 2mol/L, obtains solution B；
Step 3:
Under the conditions of magnetic agitation, the CuCl of 0.15g is added in 600rap/min, Xiang Shangshu solution B2·2H2O obtains solution
C；
Step 4:
Above-mentioned solution C is transferred to hydrothermal reaction kettle, carries out hydro-thermal reaction, high temperature hydrothermal temperature is 200 DEG C, reaction
Time is 20h, is cooled down after reaction, and product is cleaned with deionized water and ethyl alcohol after reaction, dry at a temperature of 80 DEG C, is received
Popped rice shape MoS2@CuS heterojunction composite.
As shown in Figure 1, using the CuS@MoS of a step hydrothermal synthesis2The flower-shaped heterojunction structure of composite Nano, nanometer is presented in material
Colored size is in 500nm or so.
The CuS@MoS of a step hydrothermal synthesis is used as shown in Figure 22In composite Nano heterojunction structure, MoS2Uniformly divide with CuS
Cloth.
Result as shown in figure 3, figure 4 and figure 5, it can be seen that step hydro-thermal hair works well, and is formed by MoS2 and CuS receives
The alternately uniformly arrangement of rice piece, forms the nano flower-like pattern of heterojunction structure.
CuS@MoS2The flower-shaped heterojunction material of composite Nano is expected to as a kind of novel magnesium ion battery anode active material
By the advantage of chemically combined two kinds of sulfide respectively, the i.e. electric conductivity of CuS and MoS2Layer structure and activity, promoted from
Sub- intercalation/deintercalation dynamics problem, so as to improve the charge/discharge capacity of Magnesium ion battery, dynamics and cyclical stability problem.
Claims (7)
1. a kind of MoS2@CuS hetero-junctions anode of magnesium ion battery material, which is characterized in that the MoS2@CuS hetero-junctions magnesium from
In sub- cell positive material, MoS2X=60~80wt% is accounted for, remaining is CuS material.
2. a kind of MoS2The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, which is characterized in that include the following steps；
Step 1:
The thiocarbamide for weighing the sodium molybdate of 0.5~1.0g, the hydroxylamine hydrochloride of 0.6~1.2g and 1.0~2.0g respectively is dissolved in 50mL
In deionized water, solution A is obtained；
Step 2:
Using magnetic agitation, the cetyl trimethylammonium bromide (CTAB) of 0.03~0.18g is added in Xiang Shangshu solution A, uses
The hydrochloric acid adjustment PH of 2mol/L is 6 or so, obtains solution B；
Step 3:
Under the conditions of magnetic agitation, the CuCl of 0.1~0.2g is added in Xiang Shangshu solution B2·2H2O obtains solution C；
Step 4:
Above-mentioned solution C is transferred to hydrothermal reaction kettle, hydro-thermal reaction is carried out, cools down after reaction, after reaction product spend from
Sub- water and ethyl alcohol cleaning, it is dry, obtain nano flower-like MoS2@CuS heterojunction composite.
3. a kind of MoS according to claim 22The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, feature
It is, magnetic agitation condition is 400rap/min in the step two.
4. a kind of MoS according to claim 22The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, feature
It is, magnetic agitation condition is 600rap/min in the step three.
5. a kind of MoS according to claim 22The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, feature
Be, in the step four, high temperature hydrothermal temperature be 180 DEG C~220 DEG C, the reaction time be 16~for 24 hours.
6. a kind of MoS according to claim 22The preparation method of@CuS hetero-junctions anode of magnesium ion battery material, feature
It is, the drying temperature is 80 DEG C.
7. a kind of MoS2The application of@CuS anode of magnesium ion battery material nano structure, by the nano flower-like MoS of 70wt%2@CuS
The binder of heterojunction composite, the conductive auxiliary agent (Super P) of 15wt% and 15wt%, which is put into mortar, to be fully ground, will
The sample mud blade coating mixed is subsequently placed into 12h in 120 DEG C of vacuum drying ovens on copper foil, keeps it sufficiently dry, glass
Glass fibre diaphragm is battery diaphragm, is assembled into button cell；After assembled button cell is stood 12h, in LANDCT2100A
Electrochemical property test is carried out, test voltage is 0.01V~3.0V, current density 100mA/g.
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Cited By (4)
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| CN110787814A (en) * | 2019-11-07 | 2020-02-14 | 汕头大学 | Layered hollow ZnCdS/MoS2Heterojunction cage and preparation and application thereof |
| CN111403743A (en) * | 2020-03-25 | 2020-07-10 | 陕西科技大学 | MoS2@ CuS @ EG nano hollow flower-shaped magnesium-lithium double-salt battery positive electrode material and preparation method and application thereof |
| CN111874938A (en) * | 2020-08-04 | 2020-11-03 | 安徽乐橙信息科技有限公司 | Preparation method of magnesium-copper hydroxy sulfate nano flower-like material |
| CN114843109A (en) * | 2022-05-13 | 2022-08-02 | 福州大学 | Sea urchin shaped MoS 2 Foamed nickel composite capacitor electrode material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787814A (en) * | 2019-11-07 | 2020-02-14 | 汕头大学 | Layered hollow ZnCdS/MoS2Heterojunction cage and preparation and application thereof |
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| CN111403743A (en) * | 2020-03-25 | 2020-07-10 | 陕西科技大学 | MoS2@ CuS @ EG nano hollow flower-shaped magnesium-lithium double-salt battery positive electrode material and preparation method and application thereof |
| CN111874938A (en) * | 2020-08-04 | 2020-11-03 | 安徽乐橙信息科技有限公司 | Preparation method of magnesium-copper hydroxy sulfate nano flower-like material |
| CN114843109A (en) * | 2022-05-13 | 2022-08-02 | 福州大学 | Sea urchin shaped MoS 2 Foamed nickel composite capacitor electrode material and preparation method thereof |
| CN114843109B (en) * | 2022-05-13 | 2023-09-29 | 福州大学 | Sea urchin-shaped MoS 2 Foam nickel composite capacitor electrode material and preparation method thereof |
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Application publication date: 20190712 |
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