CN107221641A - A kind of lignin is the MoS of carbon source2The preparation method of@C combination electrode materials - Google Patents
A kind of lignin is the MoS of carbon source2The preparation method of@C combination electrode materials Download PDFInfo
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- 229920005610 lignin Polymers 0.000 title claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 239000007772 electrode material Substances 0.000 title claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 25
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims abstract description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- 239000002105 nanoparticle Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 229910052961 molybdenite Inorganic materials 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 239000004005 microsphere Substances 0.000 claims description 4
- 239000011684 sodium molybdate Substances 0.000 claims description 4
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 13
- 239000003575 carbonaceous material Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000002525 ultrasonication Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000000197 pyrolysis Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- -1 oxo phenylpropanol Chemical compound 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229950009195 phenylpropanol Drugs 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
-
- 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
-
- 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
-
- 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 invention provides a kind of preparation method of lithium battery composite carbon electrode material.The present invention is used as carbon source using sodium lignin sulfonate, sample is set to be in microballoon using suitable solvent and ultrasonication, the direct synthesis of carbon/molybdenum disulfide of hydro-thermal method is recycled, it is grown in lignin surface, the modified porous microballoon carbon material of molybdenum disulfide that we need then is made by high temperature pyrolysis.Finally, test analysis is carried out to the chemical property of sample.The beneficial effects are mainly as follows：The MoS being made2The features such as@C composites have high-specific surface area, good circulation and large current density electrical stability, high specific capacitance.
Description
(1) technical field
The present invention relates to the MoS that a kind of lignin is carbon source2The preparation method of@C combination electrode materials.
(2) background technology
In recent years, for the research of lithium ion battery negative material, raising efficiency for charge-discharge is concentrated mainly on, electricity is improved
In terms of pond service life and the specific surface area of raising material.Research now, is mainly modified and negative on the surface of carbon material
Pole material surface attachment nanometer phase, surface form nanometer micropore and the application of some other nanometer technology.The research of the direction
Achievement it is a lot of, the development prospect that also show lithium ion battery is very considerable.
Molybdenum disulfide (MoS2) be used as lithium ion battery negative material theoretical capacity it is very big, be a kind of electricity of great prospect
Pole material selection；Lignin is to contain oxo phenylpropanol in a kind of unbodied, molecular structure being widely present in plant
Or derivatives thereof construction unit armaticity high polymer, its simultaneously contain various active functional group, such as hydroxyl, carbonyl, carboxyl, first
Base and side-chain structure, are a kind of carbon sources of the porous carbon materials of great prospect.
So far, also there is the MoS synthesized using hydro-thermal method2Nanometer sheet be made electrode report [《Materials
Research Bulletin》,2009,44(9):1811-1815], specific capacitance is up to 748mAh/g.But the electrode remains unchanged and deposited
Trigger MoS in the embedding de- process of lithium ion2The problem of change of volume, it is not stabilization to cause its actual chemical property.It is porous
Carbon material lignin micro Nano material is a kind of good and with the electrode material of actual use value, steady with good structure
It is qualitative, by itself and MoS2It is compound to be expected to have both advantages concurrently.
(3) content of the invention
It is an object of the present invention to provide a kind of Stability Analysis of Structures, specific surface area is big, using lignin as the MoS of carbon source2@C composite woods
The preparation method of material.
The technical solution adopted by the present invention is：
A kind of lignin is the MoS of carbon source2The preparation method of@C combination electrode materials, methods described includes：
(1) sodium lignin sulfonate is dissolved in deionized water, ultrasonic dissolution；
(2) take isopropanol to be placed in ultrasonic water bath, the solution that step (1) is obtained by auto injection machine with 10~
In 20ml/h speed injection isopropanol, the suspension of lignin microballoon is obtained；
(3) weigh thiocarbamide and sodium molybdate is placed in the suspension that step (2) is obtained, mixed liquor is placed in autoclave
In, reactor is placed in high temperature oven, 180~220 DEG C are reacted 8~10h, after cooling, reactant centrifuge washing is long
There is the lignin microsphere powder of molybdenum disulfide, vacuum drying obtains drying MoS2@lignin nanoparticle powder；
(4) the drying MoS for obtaining step (3)2@lignin nanoparticle powder is placed in N2Calcined in atmosphere through tube furnace,
Obtain MoS2@C combination electrode materials.
The ratio between sodium lignin sulfonate, thiocarbamide and sodium molybdate quality consumption are：500~1000：150~160：230~250,
Preferably 500：151：237.
Calcine technology is preferably in step (4)：300 DEG C are warming up to 5 DEG C/min speed, then with 2 DEG C/min speed
It is warming up to after 500 DEG C, insulation 1h, is warming up to 900 DEG C with 5 DEG C/min, 300 are cooled to 6 DEG C/min speed after being incubated through 1h
DEG C, then cool to the furnace after 100 DEG C and take out.
Step (3) centrifugation is set to 6000r/min, 5min/ times.
Step (2) high temperature oven reaction temperature is 180 DEG C.
In the present invention, described lignin sulfonic acid sodium water solution is dispersed in isopropanol under ultrasonication, forms stable
Nanoparticle.Through hydro-thermal reaction in the long molybdenum disulfide of lignin nano-particle surface, MoS is obtained2@lignin nanoparticle powder
End.
The MoS using lignin as carbon source that the present invention is provided2@C composites have coreshell type structure, and the molybdenum disulfide changes
The specific surface area of property porous microsphere carbon material is higher, it is to avoid the Volume Changes of molybdenum disulfide charge and discharge process.
The invention provides the MoS using lignin as carbon source2@C composites are used as lithium ion battery negative material
Application, as a result show, the features such as it has good circulation and large current density electrical stability, high specific capacitance.
The beneficial effects are mainly as follows：
1、MoS2Lignin microballoon has successfully been coated, has been core shell structure, specific surface area is big, is 14.93m2/ g or so.
2nd, selection isopropanol is solvent, and lignin forms good spherical template.Lignin microballoon is obtained through high temperature cabonization
Carbon material still keeps spherical, a diameter of 1 μm or so, and particle is uniform, and because the distillation of lignin small molecular is escaped into many
Pass, aperture is 100~160nm, and these ducts can realize MoS2Contacted with the lithium ion in electrolyte, and further improve material
The contact area of material and electrolyte.
3、MoS2@C composites have higher specific capacitance (748mAh/g or so), and still have good under multiple circulation
Retention (91.3%), show the chemical property of good and stable circulation.
(4) illustrate
Fig. 1 is MoS prepared by embodiment 12The SEM figures of@C composites；
Fig. 2 is MoS prepared by embodiment 12The desorption absorption figure and size distribution figure of the nitrogen of@C composites；
Fig. 3 is the MoS of the not be the same as Example prepared using the present invention2The cyclic voltammogram of@C composite electrode materials,
Lines correspond to 0.1~0.005V respectively from top to bottom in figure；A~d is corresponding in turn to the MoS of the preparation of embodiment 1~42@C are answered
Condensation material electrode material.
Fig. 4 is the MoS prepared using the present invention2The constant current charge-discharge diagram and specific capacitance figure of@C composite electrode materials；
Wherein a and c is the constant current charge-discharge diagram and specific capacitance figure of embodiment 1, b and constant current charge-discharge diagram and specific capacitance that d is embodiment 3
Figure.
(5) embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Embodiment 1：
0.5g sodium lignin sulfonates are dissolved in 20ml deionized waters, ultrasonic dissolution.Take 40ml isopropanols to be placed in 150w to surpass
In sound water-bath, by lignin sulfonic acid sodium water solution 30ml syringes, isopropyl is injected with 20ml/h speed by auto injection machine
In alcohol.Obtain the suspension of lignin microballoon.Weigh 0.151g thiocarbamides and 0.237g sodium molybdates are placed in suspension, by mixed liquor
It is placed in autoclave.Reactor is placed in 180 DEG C of high temperature ovens, 8h is reacted.After cooling, reactant centrifuge washing is obtained
To the lignin microsphere powder with molybdenum disulfide.Powder product is dried 24 hours for 60 DEG C in vacuum drying oven, drying is obtained
Product MoS2@lignin nanoparticle powder.MoS will be dried2@lignin nanoparticle powder is placed in N2Through tube furnace in atmosphere
Calcining (be warming up to 300 DEG C with 5 DEG C/min speed, then be warming up to 2 DEG C/min speed after 500 DEG C, insulation 1h, with 5 DEG C/
Min is warming up to 900 DEG C, and 300 DEG C are cooled to 6 DEG C/min speed after being incubated through 1h, is taken after then cooling to 100 DEG C with the furnace
Go out), obtain MoS2@C composites.Its SEM figure is referring to Fig. 1, and the desorption absorption figure and size distribution figure of nitrogen are referring to figure
2, as seen from the figure, the carbon material that lignin microballoon is obtained through high temperature cabonization still keeps spherical, a diameter of 1 μm or so, and its surface can
See obvious molybdenum disulfide nano fold lamella, illustrate that molybdenum disulfide lamellar structure has preferably coated matrix.
Embodiment 2：
Other are same as Example 1, and difference is that reaction temperature is 200 DEG C.Gained MoS2@C composite particulates
Dispersed preferable, its particle diameter is 1 μm or so.But molybdenum disulfide cladding situation is general.
Embodiment 3：
Other are same as Example 2, and difference is that the consumption of sodium lignin sulfonate is 1g.Gained MoS2@C composite woods
It is 1 μm or so to expect mean particle dia.Molybdenum disulfide also preferably realizes the constant current charge-discharge that b and d in cladding, Fig. 4 is embodiment 3
Figure and specific capacitance figure.As seen from the figure, the specific capacity retention rate of embodiment 3 is not high, with the increase of discharge and recharge number of times, its specific capacity
Decay is fast.
Embodiment 4：
Other are same as Example 1, and difference is that reaction temperature is 220 DEG C.Gained MoS2@C composite particulates
It is dispersed preferable, a diameter of 1 μm or so.Its molybdenum disulfide covering amount increases, but electric property is not directly proportional to covering amount.
Embodiment 5：Application Example 1
By obtained MoS2@C composites press 8 with conductive agent (acetylene black), polytetrafluoroethylene PTFE (binding agent)：1：1
Ratio mixing, be equably coated in the nickel foam of precise, working electrode be made, reference electrode is made with Ag/AgCl electrodes,
It is that electrolyte constitutes three-electrode system that platinized platinum, which is used as auxiliary electrode and potassium hydroxide solution, for testing chemical property.
The not MoS of be the same as Example2The cyclic voltammogram of@C composite electrode materials is referring to Fig. 3, MoS2@C composites electricity
The constant current charge-discharge diagram and specific capacitance figure of pole material are referring to Fig. 4.As seen from the figure, being continuously increased with sweep speed, material ratio
Electric capacity is slowly decayed, and each embodiment of Integrated comparative can be found that the electrical property of embodiment 1 preferably, and it has higher specific capacitance
(748mAh/g or so), and (50 times) still have good retention (91.3%) under multiple circulation.Show good and circulation
Stable chemical property.
Claims (5)
1. a kind of lignin is the MoS of carbon source2The preparation method of@C combination electrode materials, methods described includes：
(1) sodium lignin sulfonate is dissolved in deionized water, ultrasonic dissolution；
(2) isopropanol is taken to be placed in ultrasonic water bath, the solution that step (1) is obtained is by auto injection machine with 10~20ml/h's
In speed injection isopropanol, the suspension of lignin microballoon is obtained；
(3) weigh thiocarbamide and sodium molybdate is placed in the suspension that step (2) is obtained, mixed liquor is placed in autoclave, will
Reactor is placed in high temperature oven, 180~220 DEG C of 8~10h of reaction, and after cooling, reactant centrifuge washing is obtained with two sulphur
Change the lignin microsphere powder of molybdenum, vacuum drying obtains drying MoS2@lignin nanoparticle powder；
(4) the drying MoS for obtaining step (3)2@lignin nanoparticle powder is placed in N2Calcine, obtain through tube furnace in atmosphere
MoS2@C combination electrode materials.
2. the method as described in claim 1, it is characterised in that：The sodium lignin sulfonate, thiocarbamide and sodium molybdate quality consumption
The ratio between be：500~1000：150~160：230~250.
3. the method as described in claim 1, it is characterised in that：Calcine technology is in the step (4)：With 5 DEG C/min speed
Degree is warming up to 300 DEG C, then is warming up to 2 DEG C/min speed after 500 DEG C, insulation 1h, 900 DEG C is warming up to 5 DEG C/min, through 1h
300 DEG C are cooled to 6 DEG C/min speed after insulation, then cools to the furnace after 100 DEG C and takes out.
4. the method as described in claim 1, it is characterised in that step (3) centrifugation is set to 6000r/min, 5min/ times.
5. the method as described in claim 1, it is characterised in that step (2) the high temperature oven reaction temperature is 180 DEG C.
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| CN108231426A (en) * | 2017-12-29 | 2018-06-29 | 北京化工大学 | A kind of molybdenum disulfide/porous Nano carbon balls composite material and preparation method thereof |
| CN108996485A (en) * | 2018-08-06 | 2018-12-14 | 浙江工业大学 | It is a kind of using lignin as the classification mesoporous carbon preparation method of nano material of carbon source |
| CN109137144A (en) * | 2018-08-06 | 2019-01-04 | 浙江工业大学 | The preparation method of molybdenum disulfide composite hollow carbon nano-fiber materials |
| CN109161023A (en) * | 2018-08-06 | 2019-01-08 | 浙江工业大学 | Polyphosphazene microspheres are the preparation method of the molybdenum disulfide composite material of carbon source |
| CN109742368A (en) * | 2019-01-08 | 2019-05-10 | 福建师范大学 | A kind of preparation for lacking the compound anode material of lithium-ion battery of layer with the long-life |
| CN110357161A (en) * | 2019-07-03 | 2019-10-22 | 山东省分析测试中心 | A kind of MCHS@molybdenum disulfide nano-composite material and its preparation method and application based on core-shell structure |
| CN113097466A (en) * | 2021-04-02 | 2021-07-09 | 宁波润锦环保科技有限公司 | Lithium ion battery negative electrode material MoS2Preparation method of @ CFs |
| CN114149844A (en) * | 2021-12-07 | 2022-03-08 | 上海海事大学 | Preparation method of multifunctional modified molybdenum disulfide nano additive |
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| CN114149844A (en) * | 2021-12-07 | 2022-03-08 | 上海海事大学 | Preparation method of multifunctional modified molybdenum disulfide nano additive |
| CN114864928A (en) * | 2022-05-31 | 2022-08-05 | 河北坤天新能源科技有限公司 | Carbon material with enlarged accessible subsurface layer and preparation method thereof |
| CN114864928B (en) * | 2022-05-31 | 2024-02-20 | 河北坤天新能源股份有限公司 | Carbon material with enlarged accessible subsurface layer and preparation method thereof |
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Application publication date: 20170929 Assignee: ZHEJIANG ACHEN NEW MATERIAL TECHNOLOGY Co.,Ltd. Assignor: JIANG University OF TECHNOLOGY Contract record no.: X2023980045591 Denomination of invention: Preparation method of MoS2@ C composite electrode material with lignin as carbon source Granted publication date: 20191203 License type: Common License Record date: 20231103 Application publication date: 20170929 Assignee: HUZHOU KAIJIN NEW ENERGY TECHNOLOGY Co.,Ltd. Assignor: JIANG University OF TECHNOLOGY Contract record no.: X2023980045565 Denomination of invention: Preparation method of MoS2@ C composite electrode material with lignin as carbon source Granted publication date: 20191203 License type: Common License Record date: 20231102 |