CN109956500A - A kind of preparation method of the molybdenum disulfide material of the nano flower-like for lithium sode cell cathode - Google Patents
A kind of preparation method of the molybdenum disulfide material of the nano flower-like for lithium sode cell cathode Download PDFInfo
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- CN109956500A CN109956500A CN201910225167.0A CN201910225167A CN109956500A CN 109956500 A CN109956500 A CN 109956500A CN 201910225167 A CN201910225167 A CN 201910225167A CN 109956500 A CN109956500 A CN 109956500A
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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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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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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
- H01M4/36—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
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- H01M4/5815—Sulfides
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention provides a kind of preparation methods of the molybdenum disulfide material of nano flower-like for lithium sode cell cathode, and the dissolution of two molybdic acid hydrate sodium is stirred in deionized water;Thiocarbamide is added in configured solution and is stirred, surfactant cetyl trimethylammonium bromide is added, stirs to get solution;It is 1-7 that dilute hydrochloric acid, which is added dropwise, to adjust the range of pH to resulting solution, continues to stir;Acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner, hydro-thermal reaction is carried out;It cools to room temperature with the furnace, takes out reactant, wash, vacuum drying obtains the molybdenum disulfide material of nano flower-like structure;Material is placed in quartz boat, the carbonization treatment in the tube furnace of logical Ar gas obtains the good nano flower-like structure molybdenum disulfide material of crystallinity.Nanometer sheet thickness 10-20nm, length 100-200nm, small size molybdenum disulfide nano sheet improve molybdenum disulfide as lithium/anode material of lithium-ion battery cyclical stability.
Description
Technical field
The invention belongs to inorganic nano materials to synthesize field, be related to preparing nanometer sheet assemble nanometer flower with hydrothermal carbonization method
The molybdenum disulfide material of shape, more particularly to a kind of preparation of the molybdenum disulfide material of nano flower-like for lithium sode cell cathode
Method.
Background technique
With the development of society, people increasingly increase the demand of the energy, especially new energy.Compared to traditional energy
Speech, new energy have the advantages that it is environmentally protective, reproducible, therefore new energy exploitation storage and using become today's society research
Hot spot.Since last century end, lithium ion battery occupies energy storage field.Make since lithium ion battery can repeat charge and discharge
With, small in size, the service life is long, receive the favor of people.People assemble lithium ion battery in miscellaneous mobile device,
Such as motion bracelet, mobile phone, computer, hearing aid etc., it brings great convenience to people's production and life.But lithium
The shortage of resource will become an important factor for restricting its development.Therefore, the energy storage for needing to develop next-generation excellent combination property is electric
Pond body system.Sodium ion has physicochemical properties similar with lithium ion, and storage very abundant of the sodium resource in the earth's crust,
Therefore, sodium-ion battery becomes most potential replacer.
Lithium/sodium-ion battery composition can substantially be divided into negative electrode material, diaphragm, electrolyte, positive electrode and battery case.
Scientific research personnel has carried out long-term exploration to each section.It is highly-safe, the service life is long, lithium/sodium-ion battery of high capacity at
For the main target of people's research.The capacity contribution of battery is concentrated mainly on negative electrode material, therefore finds appropriate negative electrode material
As the key for obtaining high-capacity battery.Negative electrode material can be divided into carbon material, oxide, sulfide, phosphorus by the type of material
Compound and selenides etc..Sulfide theoretical capacity with higher becomes the hot spot material of people's research.
Molybdenum disulfide has two-dimensional layered structure, there is important application in terms of photoelectricity, catalysis, energy storage.Class graphene
The molybdenum disulfide theoretical capacity of structure is 670mAh g-1, higher theoretical capacity, rich reserves and unique structure feature are in crowd
There is competitive advantage very much in polysulfide.But during lithium/sodium ion insertion, deviating from, molybdenum disulfide is easy to happen structure
Rupture, causes the irreversibility of material energy storage.Currently, researcher has been many work, Li to the research of molybdenum sulfide
(Ping Li,Jong Yeob Jeong,Bingjun Jin,Kan Zhang,*and Jong Hyeok Park.Advanced
Energy Materials.2018,1703300,1-8) etc. by molybdenum disulfide growth in situ on the graphene film that N is adulterated, pole
The earth improves cyclical stability.Although the appropriate compound stability that material can be improved of carbon material, due to carbon material sheet
The capacity that body is contributed is limited, therefore the theoretical specific capacity that will cause composite material reduces.Changed from the structure of material itself
Property improves the stability of material, and the energy density of material can be kept not change.According to pertinent literature, when material
When size reaches nanoscale, there is great effect to the stability of material.Therefore the nano material of suitable dimension, tool are designed
There is important meaning.
Summary of the invention
The purpose of the present invention is prepare two flower-shaped sulphur of nanometer sheet assemble nanometer through carbonization treatment by using hydro-thermal method
Change molybdenum material.The material is assembled by molybdenum disulfide nano sheet, and wherein the thickness of nanometer sheet is in 10-20nm, and length is in 100-
200nm, the molybdenum disulfide nano sheet of small size is due to the effect of surfactant, and several nanometer sheets are by mutually overlapping self assembly
At nano flower, diameter is in 2.8um or so.The molybdenum disulfide nano sheet of small size greatly improves the steady of specific surface area and structure
It is qualitative, to improve molybdenum disulfide as lithium/anode material of lithium-ion battery cyclical stability.
The present invention provides a kind of molybdenum disulfide material flower-shaped using hydro-thermal method synthesis nanometer sheet assemble nanometer, by carbonization
Processing can be applicable to lithium/sodium-ion battery.
Technical scheme is as follows:
A kind of preparation method of the molybdenum disulfide material of the nano flower-like for lithium sode cell cathode, comprises the following steps that
1) stirs the dissolution of two molybdic acid hydrate sodium in deionized water, is prepared into the molybdenum that concentration is 0.02-0.09mol/L
Acid sodium aqueous solution;
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution molar concentration and sodium molybdate aqueous solution
Molar concentration rate is 1.5:1.0-2.5:1.0, and surfactant cetyl trimethylammonium bromide is added, wherein being added in stirring
The molar concentration and sodium molybdate aqueous solution molar concentration rate of cetyl trimethylammonium bromide are 0.5:1.0-1:1.0, are stirred
To solution;
3) it is 1-7 that is added dropwise dilute hydrochloric acid to adjust the range of pH to the resulting solution of step 2), continues to stir;
4) step 3) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
After kettle sealing, hydro-thermal reaction is carried out;It cools to room temperature with the furnace, takes out reactant, with dehydrated alcohol and deionized water centrifuge washing,
Vacuum drying, obtains the molybdenum disulfide material of nano flower-like structure;
5) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, cools to room temperature with the furnace, obtains the molybdenum disulfide material of the good nano flower-like structure of crystallinity.
Preferred speed of agitator 200-400r/min, mixing time 0.5-1h in the step 1), step 2) or step 3).
The middle step 4) hydrothermal reaction condition is preferred: being heated to 180-220 DEG C, keeps the temperature 12-36h.
Dehydrated alcohol and deionized water centrifuge washing 6-8 times are preferably used in the middle step 4), are dried in vacuo 10-12h.
Carbonization treatment condition is preferably in the middle step 5): heating rate is 2-5 DEG C/min, is protected at 700-900 DEG C
Warm 2-5h.
The concentration of the middle step 3) preferably dilute hydrochloric acid are as follows: 0.1-1mol/L.
Method of the invention is prepared into the molybdenum disulfide material of nanometer sheet assemble nanometer flower-like structure, molybdenum disulfide nano sheet
With a thickness of 10-20nm, length is mutually overlapped in 100-200nm, the molybdenum disulfide nano sheet of small size, forms three-dimensional flower-shaped knot
Structure.
Method of the invention is prepared into the molybdenum disulfide material of nanometer sheet assemble nanometer flower-like structure for lithium ion battery
Or sodium-ion battery cathode.
Effect of the invention, which is hydro-thermal method, is assembled into nano flower-like through the carbonization treatment preparation good nanometer sheet of crystallinity
Molybdenum disulfide material.The material is assembled by the molybdenum disulfide nano sheet of small size, and wherein the thickness of nanometer sheet is in 10-
20nm, for length in 100-200nm, several nanometer sheets are self-assembled into nano flower by mutually overlap joint, and diameter is small in 2.8um or so
The molybdenum disulfide nano sheet of size greatly improves specific surface area, and agglomeration does not occur for extra small nanometer sheet, thus
Molybdenum disulfide is improved as lithium/anode material of lithium-ion battery cyclical stability.In being applied to lithium ion battery,
100mA g-1Current density under test its chemical property, its specific capacity is up to 1000mA h g after circulation 100 times-1With
On, coulombic efficiency is close to 100%;When being applied to sodium-ion battery, in 5A g-1Current density under test its electrochemistry
Can, its specific capacity is up to 320mA h g after circulation 300 times-1More than, coulombic efficiency is close to 100%.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram for the molybdenum disulfide material that nanometer sheet prepared by embodiment 1 is assembled into nano flower-like, figure
Middle displaying diffraction maximum is at 14.2 ° of angle of diffraction, 32.9 °, 39.5 °, 58.7 ° of (002) with molybdenum disulfide, (100), (103),
(110) crystal face matches, and illustrates that prepared product is made of molybdenum disulfide, wherein molybdenum disulfide has excellent crystallization
Property.
Fig. 2 is the scanning electron microscopic picture for the molybdenum disulfide material that nanometer sheet prepared by embodiment 2 is assembled into nano flower-like, from
As can be seen that the material is assembled by minimum molybdenum disulfide nano sheet in figure.
Fig. 3 is the scanning electron microscopic picture of the flower-shaped molybdenum disulfide material of nanometer sheet assemble nanometer prepared by embodiment 3, from figure
In as can be seen that the flower-shaped molybdenum disulfide material of nanometer sheet assemble nanometer scanning electron microscopic picture, the thickness of nanometer sheet is in 10-
20nm, length is in 100-200nm.
Specific embodiment
Embodiment 1:
1) dissolves two molybdic acid hydrate sodium in deionized water, stirs 0.5h with 200r/min revolving speed, being prepared into concentration is
0.02mol/L sodium molybdate aqueous solution;
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution concentration be 0.3mol/L, continue with
After 200r/min revolving speed stirs 0.5h, surfactant cetyl trimethylammonium bromide, cetyl trimethyl bromination is added
The concentration of ammonium is 0.01mol/L, continues to stir 0.5h with 200r/min revolving speed;
3) is added dropwise the dilute hydrochloric acid that concentration is 0.1mol/L to the resulting solution of step 2) and adjusts pH=7, continues with 200r/
Min revolving speed stirs 0.5h;
4) step 3) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
Kettle sealing, hydrothermal condition: being heated to 180 DEG C, keeps the temperature 36h.After reaction, it cools to room temperature with the furnace, reactant is taken out, with nothing
Water-ethanol and deionized water centrifuge washing 6 times are dried in vacuo 10h, obtain the flower-shaped molybdenum disulfide material of nanometer sheet assemble nanometer;
5) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, Carbonization Conditions are: heating rate is 2 DEG C/min, 2h is kept the temperature at 700 DEG C, it is good to obtain crystallinity for furnace cooling
The flower-shaped molybdenum disulfide material of good nanometer sheet assemble nanometer.
As shown in Figure 1, the product of preparation is molybdenum disulfide, there is excellent crystallinity.In lithium ion battery,
100mAg-1Current density under test its performance, its specific capacity is up to 850mA h g after circulation 100 times-1More than;Sodium from
In sub- battery, in 100mAg-1Current density under test its performance, its specific capacity is up to 363mA h g after circulation 80 times-1
More than.
Embodiment 2:
1) dissolves two molybdic acid hydrate sodium in deionized water, stirs 0.8h with 300r/min revolving speed, being prepared into concentration is
0.05mol/L sodium molybdate aqueous solution;
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution concentration be 0.1mol/L, continue with
After 300r/min revolving speed stirs 0.8h, surfactant cetyl trimethylammonium bromide, cetyl trimethyl bromination is added
The concentration of ammonium is 0.04mol/L, continues to stir 0.8h with 300r/min revolving speed;
3) is added dropwise the dilute hydrochloric acid that concentration is 0.5mol/L to the resulting solution of step 2) and adjusts pH=3, continues with 300r/
Min revolving speed stirs 0.8h;
4) step 3) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
Hydrothermal condition: kettle sealing is heated to 200 DEG C, heat preservation is for 24 hours.After reaction, it cools to room temperature with the furnace, reactant is taken out, with nothing
Water-ethanol and deionized water centrifuge washing 7 times are dried in vacuo 11h, obtain the molybdenum disulfide of nanometer sheet assemble nanometer flower-like structure
Material;
5) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, Carbonization Conditions are: heating rate is 3 DEG C/min, 3h is kept the temperature at 800 DEG C, it is good to obtain crystallinity for furnace cooling
The molybdenum disulfide material of good nanometer sheet assemble nanometer flower-like structure.
As shown in Fig. 2, nanometer sheet assemble nanometer flower-like structure of the product by small size, wherein the thickness of nanometer sheet is in 10-
20nm, length is in 100-200nm.For in lithium ion battery, in 100mA g-1Current density under test its chemical property,
Its specific capacity is up to 950mA h g after circulation 100 times-1More than, coulombic efficiency is close to 100%;In sodium-ion battery,
100mA g-1Current density under test its performance, its specific capacity is up to 400mA h g after circulation 100 times-1More than, coulomb
Efficiency is close to 100%.
Embodiment 3:
1) dissolves two molybdic acid hydrate sodium in deionized water, stirs 1h with 400r/min revolving speed, being prepared into concentration is
0.09mol/L sodium molybdate aqueous solution;
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution concentration be 0.225mol/L, continue with
After 400r/min revolving speed stirs 1h, surfactant cetyl trimethylammonium bromide, cetyl trimethylammonium bromide is added
Concentration be 0.09mol/L, continue with 400r/min revolving speed stir 1h;
3) is added dropwise 1.0mol/l dilute hydrochloric acid to the resulting solution of step 2) and adjusts pH=1, and continuation is stirred with 400r/min revolving speed
Mix 1h;
4) step 3) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
Kettle sealing, hydrothermal condition: being heated to 220 DEG C, keeps the temperature 12h.After reaction, it cools to room temperature with the furnace, reactant is taken out, with nothing
Water-ethanol and deionized water centrifuge washing 8 times are dried in vacuo 12h, obtain the molybdenum disulfide of nanometer sheet assemble nanometer flower-like structure
Material;
5) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, Carbonization Conditions are: heating rate is 5 DEG C/min, keeps the temperature 2h at 900 DEG C, cools to room temperature with the furnace, is tied
The flower-shaped molybdenum disulfide material of the good nanometer sheet assemble nanometer of crystalline substance.
As shown in figure 3, what product was assembled by the nanometer sheet of small size, wherein the thickness of nanometer sheet is in 10-20nm, length
Degree is in 100-200nm.For in lithium ion battery, in 100mA g-1Current density under test its chemical property, circulation 100
Its specific capacity is up to 1000mA h g after secondary-1More than, coulombic efficiency is close to 100%;In sodium-ion battery, in 5A g-1
Current density under test its chemical property, its specific capacity is up to 320mA h g after circulation 300 times-1More than, coulombic efficiency
Close to 100%.
To sum up the attached drawing of embodiment can also clearly be found out, product prepared by the present invention is that small size nanometer sheet is assembled into
The molybdenum disulfide material of nano flower-like.
Claims (7)
1. a kind of preparation method of the molybdenum disulfide material of the nano flower-like for lithium sode cell cathode, it is characterized in that step is such as
Under:
1) stirs the dissolution of two molybdic acid hydrate sodium in deionized water, is prepared into the sodium molybdate that concentration is 0.02-0.09mol/L
Aqueous solution;
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution molar concentration and sodium molybdate aqueous solution mole
Concentration ratio is 1.5:1.0-2.5:1.0, and surfactant cetyl trimethylammonium bromide is added in stirring, wherein being added 16
The molar concentration and sodium molybdate aqueous solution molar concentration rate of alkyl trimethyl ammonium bromide are 0.5:1.0-1:1.0, are stirred to get molten
Liquid;
3) it is 1-7 that is added dropwise dilute hydrochloric acid to adjust the range of pH to the resulting solution of step 2), continues to stir;
4) step 3) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and close using stainless steel cauldron
It is honored as a queen, carries out hydro-thermal reaction;It cools to room temperature with the furnace, reactant is taken out, with dehydrated alcohol and deionized water centrifuge washing, vacuum
It is dry, obtain the molybdenum disulfide material of nano flower-like structure;
5) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to carbon in the tube furnace for being connected with Ar gas
Change processing, cools to room temperature with the furnace, obtains the molybdenum disulfide material of the good nano flower-like structure of crystallinity.
2. the method as described in claim 1, it is characterized in that speed of agitator 200- in the step 1), step 2) or step 3)
400r/min, mixing time 0.5-1h.
3. the method as described in claim 1, it is characterized in that the middle step 4) hydrothermal reaction condition: it is heated to 180-220 DEG C,
Keep the temperature 12-36h.
4. the method as described in claim 1, it is characterized in that being washed in the middle step 4) with dehydrated alcohol and deionized water centrifugation
It washs 6-8 times, is dried in vacuo 10-12h.
5. the method as described in claim 1, it is characterized in that carbonization treatment condition is in the middle step 5): heating rate 2-
5 DEG C/min, 2-5h is kept the temperature at 700-900 DEG C.
6. method of claim 1 is prepared into the molybdenum disulfide material of nanometer sheet assemble nanometer flower-like structure, molybdenum disulfide nano
Piece with a thickness of 10-20nm, length is mutually overlapped in 100-200nm, the molybdenum disulfide nano sheet of small size, formed it is three-dimensional flower-shaped
Structure.
7. method of claim 1 is prepared into the molybdenum disulfide material of nanometer sheet assemble nanometer flower-like structure for lithium ion battery
Or sodium-ion battery cathode.
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CN110311117A (en) * | 2019-07-08 | 2019-10-08 | 陕西科技大学 | A kind of MoS2The double salt ion cell positive materials of@EG magnesium-lithium and its construction method |
CN111883753A (en) * | 2020-07-16 | 2020-11-03 | 樊梦林 | MoS with hierarchical shell-core structure2Negative active material of-C composite porous microsphere |
CN111883753B (en) * | 2020-07-16 | 2021-11-09 | 上海鼎瀛信息科技有限公司 | MoS with hierarchical shell-core structure2Negative active material of-C composite porous microsphere |
CN112551585A (en) * | 2020-12-24 | 2021-03-26 | 齐鲁工业大学 | Surfactant-induced MoS2Preparation method and application of nanoflower electrode material |
CN112713012A (en) * | 2021-01-26 | 2021-04-27 | 重庆茨文科技有限公司 | Zn-doped Co9S8Loaded MoS2Method for producing composite material and use thereof |
CN113247954A (en) * | 2021-05-12 | 2021-08-13 | 中山大学 | Large-interlayer-distance molybdenum disulfide material and preparation method and application thereof |
CN114588849A (en) * | 2022-02-22 | 2022-06-07 | 兰州城市学院 | Method for preparing 3D nanoflower composite material by hydrothermal method |
CN116216780A (en) * | 2023-03-01 | 2023-06-06 | 淮北师范大学 | Broken shell-shaped MoS 2 Nanosphere material and preparation method and application thereof |
CN116216780B (en) * | 2023-03-01 | 2024-04-26 | 淮北师范大学 | Broken shell-shaped MoS2Nanosphere material and preparation method and application thereof |
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