CN106423218A - Synthesis method of molybdenum disulfide/carbon nano composite material - Google Patents
Synthesis method of molybdenum disulfide/carbon nano composite material Download PDFInfo
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- CN106423218A CN106423218A CN201610849294.4A CN201610849294A CN106423218A CN 106423218 A CN106423218 A CN 106423218A CN 201610849294 A CN201610849294 A CN 201610849294A CN 106423218 A CN106423218 A CN 106423218A
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- composite material
- carbon nano
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- molybdenum bisuphide
- carbon
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 29
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 24
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title abstract description 6
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title abstract description 5
- 238000001308 synthesis method Methods 0.000 title abstract 2
- 239000000243 solution Substances 0.000 claims abstract description 23
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 21
- 239000011591 potassium Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 22
- 239000011733 molybdenum Substances 0.000 claims description 22
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 238000010189 synthetic method Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000000975 co-precipitation Methods 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract 2
- 239000002028 Biomass Substances 0.000 abstract 1
- VSOYJNRFGMJBAV-UHFFFAOYSA-N N.[Mo+4] Chemical compound N.[Mo+4] VSOYJNRFGMJBAV-UHFFFAOYSA-N 0.000 abstract 1
- 229910052786 argon Inorganic materials 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 239000002073 nanorod Substances 0.000 abstract 1
- 229910052755 nonmetal Inorganic materials 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000003245 coal Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- -1 graphite alkene Chemical class 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 239000012620 biological material Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- XACAZEWCMFHVBX-UHFFFAOYSA-N [C].[Mo] Chemical compound [C].[Mo] XACAZEWCMFHVBX-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 125000004151 quinonyl group Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/40—
-
- 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
-
- 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
Abstract
The invention discloses a synthesis method of a molybdenum disulfide/carbon composite material for preparing potassium humate, belonging to the field of inorganic non-metal materials. The method comprises the following steps: dissolving a soluble molybdenum salt ammonium molybdate tetrahydrate in water, adding potassium humate into the solution, reversely dropping the mixed solution into nitric acid, and regulating the pH value to 1-3 to prepare a precipitate; and roasting in argon or any other inert atmosphere by a fused salt roasting process to generate carbon thermal reaction, thereby obtaining the composite structure on which nanorods with the length of 100nm or so are carried on the carbon film. The method has the advantages of simple technique and low cost. The biomass material potassium humate is used as the carbon source to directly synthesize the loaded nano composite structure.
Description
Technical field
The invention belongs to new inorganic non-metallic materials research and development technology field, specifically disclose one kind and be related to molybdenum bisuphide/carbon and receive
The co-precipitation of nano composite material and the synthetic method of fuse salt roasting.
Background technology
Molybdenum bisuphide has the layer structure of similar graphite and stable physicochemical properties, is widely used in solid lubrication
Agent, hydrogen storage material, battery electrode material, catalysis material etc..Nanometer class molybdenum disulfide material, because its high adsorption capacity, catalysis are anti-
The feature such as active height should be used as coal liquefaction, coal pyrolysis, hydrodesulfurization, the catalyst of sulphur removal denitrification in oil.But by
Little in nanoparticle size, surface energy is high, is susceptible to reunite between particle, nano material dispersion in media as well and steady
Determine to become one of subject matter limiting it in commercial Application.In order to improve the reunion of nano molybdenum disulfide particle, in recent years, stone
Black alkene or graphene oxide become the focus that people study.At present, method predominantly organic tool stripping method, the reduction of Graphene are prepared
The synthetic methods such as graphite oxide method, epitaxial growth method and metal catalysed processes.However, graphenic surface assumes stable inertia, indissoluble
Solution is in solvent it more difficult to equably be combined with other organic or inorganic materials.Therefore, prepare graphene composite material, be mostly
First graphene oxide is combined with nano material, then will compound after material reduction obtain graphene composite material.This preparation
Complex steps, product property is often difficult to meet application demand, therefore, it is necessary to exploitation one kind directly obtains graphene-supported list
The preparation method of dispersing nanoparticles.
Prepare at present nano particle/graphite alkene main method have chemical reduction method, electrochemical deposition method, thermal evaporation,
Hydro-thermal method, sol-gel process etc..Some researchs show, select suitable carbon source and synthesis condition can directly obtain the stone of load
Black alkene.Humic acidss are a kind of natural macromolecular organic compound, are mainly adopted the side of " alkali extraction and acid precipitation " by weathered coal or brown coal
Method obtains.Humic acidss have uncertain molecular weight, contain multiple work such as carboxyl, hydroxyl, phenolic hydroxyl group, quinonyl, methoxyl group thereon
Property functional group.It has the functions such as good absorption, complexation, exchange.
Content of the invention
The purpose of the present invention is:In order to prove to select suitable carbon source, molybdenum bisuphide/carbon can be directly obtained nano combined
Material.Propose using humic acidss essence potassium complexing metal molybdenum ion, further by roasting after itself and sodium sulfate mixed grinding, preparation
The method of molybdenum bisuphide/carbon nano-composite material.
The technical scheme is that:A kind of synthetic method of molybdenum bisuphide/carbon nano-composite material, this synthetic method bag
Include following steps:(1)The four hydration Ammoniun Heptamolybdate Solution 40ml of configuration 0.25M, then it is added thereto to 2g humic acidss essence potassium, by two
Person is mixed and stirred for into mixed solution, standby;(2)The salpeter solution 100ml of configuration 0.5M, by step(1)Middle stirring obtains
Mixed solution is dropwise added drop-wise in the salpeter solution of 0.5M, and the pH adjusting solution is between 1-3, and standing was sunk after a period of time
Starch, standby;(3)By step(2)In the precipitate lyophilizing for preparing, press 1 with anhydrous sodium sulfate:10 mass ratio mixing is ground
Mill, under Ar gas atmosphere, under the conditions of 600 DEG C or 700 DEG C or 800 DEG C, with the heating gradient roasting 3h of 10 DEG C/min, naturally cold
But arrive room temperature, obtain the presoma of molybdenum bisuphide/carbon nano-composite material, standby;(4)By step(3)In the presoma that obtains
With water and each centrifuge washing of dehydrated alcohol five times, it is finally stored in dehydrated alcohol;Product is dried to obtain at 50 DEG C two sulfur
Change the powder body of molybdenum/carbon nano-composite material.Using the feature of humic acidss essence potassium " alkali extraction and acid precipitation ", adopt in fuse salt roasting system
With humic acidss essence this biological material of potassium as carbon source synthesis of carbon/molybdenum disulfide/carbon nano-composite material, described potassium humate purchase
Buy from Xinjiang Shuan Long humic acidss company.
Beneficial effect:The invention provides a kind of method directly obtaining molybdenum bisuphide/carbon nano-composite material, using from
The humic acidss essence this not only cheap but also efficient biological material of potassium extracting in weathered coal, as carbon source, is realized at utmost
The utilization of resources, be finally reached environmental conservation, the purpose of resource higher value application.
Brief description
Fig. 1:The X-ray of molybdenum bisuphide/carbon nano-composite material when T=600 DEG C of preparation method of the present invention(XRD) collection of illustrative plates;
Fig. 2:The transmission electron microscope figure spectrum of molybdenum bisuphide/carbon nano-composite material when T=600 DEG C of preparation method of the present invention
(TEM);
From the X-ray collection of illustrative plates of Fig. 1 it is recognised that the material obtaining when T=600 DEG C is molybdenum bisuphide/carbon nano-composite material.From
Molybdenum bisuphide/carbon nano-composite material obtained by the image of the transmission electron microscope of Fig. 2 can be seen that is 100nm
Nanometer rods be uniformly supported on the pattern on carbon film surface.It is therefore seen that, select suitable carbon source-humic acidss essence potassium, permissible
Directly obtain molybdenum bisuphide/carbon nano-composite material.
Specific embodiment
The embodiment 1, (NH of configuration 0.25M4)6Mo7O24·4H2O solution 40ml, then it is added thereto to 2g humic acidss essence potassium,
It is reconfigured at the HNO of 0.5M3Solution 100ml.Under conditions of magnetic agitation, by (NH4)6Mo7O24·4H2O is mixed with humic acidss essence potassium
Close solution and be slowly reversely added drop-wise to HNO3In solution.After above turbid solution is stood, suction out the water on upper strata, then precipitate is entered
Row lyophilizing, takes the humic acidss after 1g lyophilizing essence potassium-molybdic acid presoma and 10g anhydrous sodium sulfate with 1:10 mass ratio is mixed
Grind, then under Ar gas atmosphere, under the conditions of 600 DEG C, with 10 DEG C/min heating gradient roasting 3h, naturally cool to room temperature, then
Respectively sample is carried out with water and ethanol with each five times of centrifuge washing, in ethanol by sample preservation, 50 DEG C of drying obtain sulfur finally
Change molybdenum/carbon nano-composite material
The embodiment 2, (NH of configuration 0.25M4)6Mo7O24·4H2O solution 40ml, then it is added thereto to 2g humic acidss essence potassium, then join
Set to 0 the HNO of .5M3Solution 100ml.Under conditions of magnetic agitation, by (NH4)6Mo7O24·4H2O mixes molten with humic acidss essence potassium
Liquid is slowly reversely added drop-wise to HNO3In solution.After above turbid solution is stood, suction out the water on upper strata, then precipitate is frozen
Dry, take the essence potassium-molybdic acid presoma of the humic acidss after 1g lyophilizing and 10g anhydrous sodium sulfate with 1:10 mass ratio carries out mixing and grinds
Mill, then under Ar gas atmosphere, under the conditions of 700 DEG C, with 10 DEG C/min heating gradient roasting 3h, naturally cools to room temperature, uses water
With ethanol, respectively sample is carried out with each five times of centrifuge washing, finally in ethanol by sample preservation, 50 DEG C of drying obtain molybdenum sulfide/
Carbon nano-composite material.
The embodiment 3, (NH of configuration 0.25M4)6Mo7O24·4H2O solution 40ml, then it is added thereto to 2g humic acidss essence potassium,
It is reconfigured at the HNO of 0.5M3Solution 100ml.Under conditions of magnetic agitation, by (NH4)6Mo7O24·4H2O is mixed with humic acidss essence potassium
Close solution and be slowly reversely added drop-wise to HNO3In solution.After above turbid solution is stood, suction out the water on upper strata, then precipitate is entered
Row lyophilizing, takes the humic acidss after 1g lyophilizing essence potassium-molybdic acid presoma and 10g anhydrous sodium sulfate with 1:10 mass ratio is mixed
Grind, then under Ar gas atmosphere, under the conditions of 800 DEG C, with 10 DEG C/min heating gradient roasting 3h, naturally cool to room temperature, then
Respectively sample is carried out with water and ethanol with each five times of centrifuge washing, in ethanol by sample preservation, 50 DEG C of drying obtain sulfur finally
Change molybdenum/carbon nano-composite material.
Potassium humate used by above-mentioned experiment is bought from Xinjiang Shuan Long humic acidss company.
Conclusion:By selecting suitable carbon source-humic acidss essence potassium, directly obtain molybdenum bisuphide/carbon nano-composite material,
Its pattern be 100 nm about nanometer rods be uniformly supported on carbon film surface.
The main technical content of the present invention is with Ammonium Molybdate Tetrahydrate and cheap humic acidss essence potassium mixed solution as raw material,
Back titration, in nitric acid, is obtained precipitation.Again with anhydrous sodium sulfate mixed grinding, using fuse salt roasting method, anti-through carbon heat
Should, using anhydrous sodium sulfate both as template agent, and as sulphur source, obtain 100nm about nanometer rods be uniformly supported on carbon
Molybdenum bisuphide/carbon nano-composite material on film surface.
Claims (2)
1. a kind of synthetic method of molybdenum bisuphide/carbon nano-composite material, this synthetic method comprises the following steps:
(1)Configuration 0.25M tetra- hydration ammonium heptamolybdate 40ml, then it is added thereto to 2g humic acidss essence potassium, both are mixed and stirred for
Become mixed solution, standby;
(2)Configure the salpeter solution 100ml of 0.5 M, by step(1)The mixed solution that middle stirring obtains dropwise is added drop-wise to 0.5M's
In salpeter solution, the pH adjusting solution is between 1-3, and standing is precipitated thing after a period of time, standby;
(3)By step(2)In the precipitate lyophilizing for preparing, press 1 with anhydrous sodium sulfate:10 quality than mixed grinding, in Ar
Under gas atmosphere, under the conditions of 600 DEG C or 700 DEG C or 800 DEG C, with the heating gradient roasting 3h of 10 DEG C/min, naturally cool to room
Temperature, obtains the presoma of molybdenum bisuphide/carbon nano-composite material, standby;
(4)By step(3)In the presoma water that obtains and each centrifuge washing of dehydrated alcohol five times, be finally stored in dehydrated alcohol
In;Product is dried to obtain at 50 DEG C the powder body of molybdenum bisuphide/carbon nano-composite material.
2. the method that coprecipitation according to claim 1 prepares molybdenum bisuphide/carbon nano-composite material, its feature exists
In:Described potassium humate is bought from Xinjiang Shuan Long humic acidss company.
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CN111370675A (en) * | 2020-03-24 | 2020-07-03 | 合肥工业大学 | Carbon nanosheet sodium-ion battery cathode material inlaid with metal phosphide and preparation method thereof |
CN113981489A (en) * | 2021-10-28 | 2022-01-28 | 济南大学 | Molybdenum carbide/carbon composite material, preparation method based on molten salt method and application |
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