CN110729135A - Preparation method of molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material - Google Patents
Preparation method of molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material Download PDFInfo
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- CN110729135A CN110729135A CN201910859213.2A CN201910859213A CN110729135A CN 110729135 A CN110729135 A CN 110729135A CN 201910859213 A CN201910859213 A CN 201910859213A CN 110729135 A CN110729135 A CN 110729135A
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 100
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000007772 electrode material Substances 0.000 title claims abstract description 34
- 229920002627 poly(phosphazenes) Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 40
- 239000008367 deionised water Substances 0.000 claims abstract description 36
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001035 drying Methods 0.000 claims abstract description 31
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 24
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 16
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 16
- 238000001291 vacuum drying Methods 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 11
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910016002 MoS2a Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000002033 PVDF binder Substances 0.000 claims description 5
- 239000006230 acetylene black Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003990 capacitor Substances 0.000 abstract description 6
- WVSZBAHKLHXQFN-UHFFFAOYSA-N tetrahydrate;dihydrochloride Chemical compound O.O.O.O.Cl.Cl WVSZBAHKLHXQFN-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 239000012265 solid product Substances 0.000 abstract 2
- 238000000746 purification Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- LTGQWIGRJSKNBP-UHFFFAOYSA-N hexahydrate;trihydrochloride Chemical compound O.O.O.O.O.O.Cl.Cl.Cl LTGQWIGRJSKNBP-UHFFFAOYSA-N 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention relates to the field of electrode materials of super capacitors, in particular to a preparation method of a molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material. Firstly, preparing molybdenum disulfide; ultrasonically dispersing molybdenum disulfide in a specific solvent, adding hexachlorocyclotriphosphazene, 4' -dihydroxydiphenylsulfone and triethylamine, and carrying out ultrasonic polymerization reaction for a certain time to obtain a molybdenum disulfide/polyphosphazene compound; then the MoS2/PZS compound is dispersed in deionized water by ultrasound, ferrous dichloride-tetrahydrate (FeCl) is added2·4H2O) and FeCl-hexahydrate (FeCl)3·6H2O), performing ultrasonic reaction for 2 hours under an alkaline condition, and performing centrifugal separation, purification and drying to obtain a solid product; finally, the solid product is put intoCalcining at high temperature to obtain MoS2/PZS/Fe3O4A composite electrode material. MoS2/PZS/Fe prepared by the invention3O4The electrode material is suitable for being applied to the field of super capacitors as the electrode material.
Description
Technical Field
The invention relates to the field of super capacitor electrode materials, in particular to a method for preparing a molybdenum disulfide/polyphosphazene/ferroferric oxide super capacitor electrode material through in-situ polymerization and application thereof.
Background
At present, the ever-increasing global energy demand and the severe environmental problems have greatly stimulated research on clean energy and energy storage devices, such as lithium ion batteries, solar cells, supercapacitors, etc., by researchers. Among them, the super capacitor has unique advantages such as high power density and energy density, rapid charge and discharge rate, and long cycle life, and thus, has attracted much attention.
Molybdenum disulfide (MoS)2) Is a representative metal disulfide that has been used as an electrode material in electrochemical energy storage. The molybdenum disulfide has physical properties similar to those of graphene, including high charge carrier transport, high wear resistance and the like, and certain properties are superior to those of graphene, such as low cost, adjustable band gap, good visible light absorption capacity and the like. In adjacent molybdenum disulfide crystal structures, an atomic layer of Mo is sandwiched between two closely packed layers of S atoms, forming a layered structure in the form of S-Mo-S. Mo-S are strong covalent bonds, and the interaction between S layers is Van der Waals force. The structure is mainly applied to the fields of solid lubricants, catalysts, supercapacitors, lithium ion battery anode materials and the like. Moreover, the structure may allow intercalation of electrolyte alkali metal ions (M ═ Li, Na, and K) between S-Mo-S layers without significant volume expansion upon cycling. Polyphosphazene (PZS) is a representative organic-inorganic hybrid material, phosphorus atoms and nitrogen atoms are alternately arranged in a main chain, so that the polyphosphazene has excellent performance, and a product obtained after high-temperature carbonization is similar to a carbon tube structure, has excellent conductivity and is porous, and is favorable for the transmission of current carriers. Ferroferric oxide (Fe)3O4) The method has the advantages of no toxicity, high theoretical capacitance, easy synthesis and the like, but has high interface resistance, poor agglomeration phenomenon and poor electrolyte stability, thereby limiting the application of the method.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a molybdenum disulfide/polyphosphazene/ferroferric oxide supercapacitor electrode material, which is characterized in that a hydrothermal method is adopted to prepare a molybdenum disulfide nanosheet, the molybdenum disulfide/polyphosphazene nanomaterial is prepared by taking the molybdenum disulfide nanosheet as a substrate through ultrasonic in-situ polymerization, ferroferric oxide nanoparticles are generated on the surface of the molybdenum disulfide/polyphosphazene in situ, and finally the molybdenum disulfide/polyphosphazene/ferroferric oxide supercapacitor electrode material is obtained through high-temperature calcination.
The invention relates to a preparation method of a molybdenum disulfide/polyphosphazene/ferroferric oxide supercapacitor electrode material, which comprises the following steps:
(1) molybdenum disulfide (MoS)2) The preparation of (1): weighing molybdenum trioxide (MoO)3) Thioacetamide (TAA) and urea are dispersed in deionized water, are transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining after being magnetically stirred, are sealed and are placed into a blast drying box for reaction; cooling to room temperature after the reaction is finished, washing the prepared product with deionized water and absolute ethyl alcohol respectively, and finally drying in vacuum at 50 ℃ to obtain MoS2。
(2)MoS2Preparation of the/PZS complex: weighing molybdenum disulfide, ultrasonically dispersing the molybdenum disulfide in a mixed solution of tetrahydrofuran and ethanol, then adding hexachlorocyclotriphosphazene and 4, 4' -dihydroxydiphenylsulfone, adding triethylamine, after ultrasonic reaction for a period of time, respectively washing the mixed solution with deionized water and absolute ethyl alcohol, and drying the washed mixed solution in a vacuum drying oven at 50 ℃ to obtain MoS2a/PZS complex.
(3)MoS2/PZS/Fe3O4Preparation of the complex: weighing MoS2the/PZS compound is completely dispersed in deionized water, and ferrous dichloride tetrahydrate (FeCl) is weighed2·4H2O) and ferric trichloride hexahydrate (FeCl)3·6H2O), introducing nitrogen for protection, adding sodium hydroxide (NaOH), carrying out ultrasonic reaction for 2h, washing the reaction solution by deionized water and absolute ethyl alcohol, finally drying in a vacuum drying oven at 50 ℃, and finally calcining at high temperature to obtain MoS2/PZS/Fe3O4And (c) a complex.
(4)MoS2/PZS/Fe3O4Preparing an electrode: mixing MoS2/PZS/Fe3O4Mixing and grinding the composite, the acetylene black and the polyvinylidene fluoride according to a certain mass ratio, adding N-methyl pyrrolidone (NMP) in the grinding process, coating the uniformly ground mixture on foamed nickel, drying the foamed nickel in a 60 ℃ oven, and tabletting by using a tabletting machine with the pressure of 10 MPa to obtain the supercapacitor electrode.
In the step (1), the mass ratio of the molybdenum trioxide, the thioacetamide and the urea is 1:1-1.5: 6-10.
In the step (1), the reaction temperature in the oven is 200-240 ℃, and the reaction time is 18-24 h.
In the step (2), the mass ratio of the molybdenum disulfide, the hexachlorocyclotriphosphazene and the 4, 4' -dihydroxydiphenylsulfone is 1:1-10: 0.5-2.
In the step (2), the ultrasonic reaction time is 5-10 h.
In step (3), the MoS2PZS complex, FeCl2·4H2O and FeCl3·6H2The mass ratio of O is 1: 5-10: 0.5-10.
The ultrasonic temperature in the step (3) is controlled to be 40-50 ℃.
The heating rate of the calcination in the step (3) is 1-5 ℃/min, the temperature is controlled at 900 ℃ and the calcination time is 2-4 hours.
MoS described in step (4)2/PZS/Fe3O4The mass ratio of the composite, the acetylene black and the polyvinylidene fluoride is 7:2: 1.
The method has the advantages of simple preparation process, low equipment requirement and strong operability. And respectively growing polyphosphazene and ferroferric oxide on the molybdenum disulfide with the lamellar structure in situ by taking the molybdenum disulfide as a substrate to obtain the molybdenum disulfide/polyphosphazene/ferroferric oxide supercapacitor electrode material. The advantages are mainly that: (1) the molybdenum disulfide substrate is prepared first, and then the polymer and the metal oxide are coated, so that the damage of the molybdenum disulfide structure can be reduced, and the excellent properties of the molybdenum disulfide can be fully utilized. (2) The performance of the electrode material can be effectively improved by combining polyphosphazene with a large number of active groups (such as-P-, -OH) and ferroferric oxide with high theoretical specific capacitance coated on the surface of the molybdenum disulfide. (3) The product after high-temperature carbonization has excellent conductivity and more internal pores, and is beneficial to the transmission of current carriers.
Compared with the prior art, the invention has the following remarkable advantages:
the uniqueness of the polyphosphazene structure is utilized to grow the polyphosphazene on the surface of the molybdenum disulfide in situ, so that the surface functionalization of the molybdenum disulfide is realized, the electrochemical performance of the molybdenum disulfide is effectively improved, and Fe with high theoretical capacitance is coated on the surface of the molybdenum disulfide3O4To obtain a target product MoS2/PZS/Fe3O4So that the electrode material has the advantages of excellent electrochemical performance and high specific capacitance. And the reaction operation and the process conditions are simple, green and environment-friendly, and suitable for large-scale production. (2) MoS prepared by applying the invention2/PZS/Fe3O4The electrode material combines the excellent properties of molybdenum disulfide, polyphosphazene and ferroferric oxide, and is very suitable for being applied to the field of super capacitors as the electrode material.
Drawings
FIG. 1 shows the MoS obtained in example 12/PZS/Fe3O4Fourier transform infrared spectrogram of electrode material;
FIG. 2 shows the MoS obtained in example 12/PZS/Fe3O4Transmission electron microscope photographs of the electrode materials;
FIG. 3 shows the MoS obtained in example 12/PZS/Fe3O4Constant current charge-discharge diagram of electrode material.
The specific implementation mode is as follows:
example 1
(1) Molybdenum disulfide (MoS)2) The preparation of (1): weighing 24mg of molybdenum trioxide (MoO)3) 28mg of Thioacetamide (TAA) and 200mg of urea are dispersed in 20mL of deionized water, are transferred to the inner liner of a stainless steel reaction kettle to be sealed after being magnetically stirred, and are placed into a blast drying oven at 200 ℃ to carry out reaction for 18 hours; cooling to room temperature after the reaction is finished, washing the prepared product with deionized water and absolute ethyl alcohol respectively, and finally drying in vacuum at 50 ℃ to obtain MoS2。
(2)MoS2Preparation of the/PZS complex: weighing 0.1g of molybdenum disulfide, ultrasonically dispersing the molybdenum disulfide in 150mL of mixed solution of tetrahydrofuran and ethanol, then adding 0.1g of hexachlorocyclotriphosphazene and 0.25g of 4, 4' -dihydroxydiphenylsulfone which are precursors of Polyphosphazene (PZS), adding 3mL of triethylamine, after carrying out ultrasonic reaction for 5 hours, respectively washing the mixed solution with deionized water and absolute ethyl alcohol, and drying the mixed solution in a 50 ℃ vacuum drying oven to obtain MoS2a/PZS complex.
(3)MoS2/PZS/Fe3O4Preparation of the complex: 0.05g of MoS was weighed2the/PZS compound, completely dispersed in deionized water, then 0.25g ferrous dichloride-tetrahydrate (FeCl) was weighed2·4H2O) and 0.06g of ferrous trichloride hexahydrate (FeCl)3·6H2O), introducing nitrogen for protection, adding 0.03g of sodium hydroxide (NaOH), carrying out ultrasonic reaction for 2h, washing the reaction solution by deionized water and absolute ethyl alcohol, finally putting the reaction solution into a vacuum drying oven at 50 ℃ for drying, and finally calcining to obtain MoS2/PZS/Fe3O4And (c) a complex.
(4)MoS2/PZS/Fe3O4Preparing an electrode: and mixing and grinding the composite, the acetylene black and the polyvinylidene fluoride according to the mass ratio of 7:2:1, adding N-methyl pyrrolidone (NMP) in the grinding process, coating the uniformly ground mixture on foamed nickel, drying the foamed nickel in an oven at 60 ℃, and tabletting by using a tabletting machine with the pressure of 10 MPa to obtain the supercapacitor electrode.
FIG. 1 shows the MoS obtained in example 12/PZS/Fe3O4Fourier transform infrared spectrogram of electrode material, and MoS has been successfully synthesized from the chart2/PZS/Fe3O4An electrode material.
FIG. 2 shows the MoS obtained in example 12/PZS/Fe3O4As can be seen from the transmission electron microscope photograph of the electrode material, the surface of the molybdenum disulfide is coated by polyphosphazene and ferroferric oxide to form MoS with a lamellar structure2/PZS/Fe3O4A composite material.
FIG. 3 shows the MoS obtained in example 12/PZS/Fe3O4Constant current charge-discharge diagram of electrode material, when the current density is 2A/gThe specific capacitance reaches 405F/g, and the stability is higher.
Example 2
(1) Molybdenum disulfide (MoS)2) The preparation of (1): weighing 24mg of molybdenum trioxide (MoO)3) 28mg of Thioacetamide (TAA) and 200mg of urea are dispersed in 20mL of deionized water, are transferred to the inner liner of a stainless steel reaction kettle to be sealed after being magnetically stirred, and are placed into a blast drying oven at 200 ℃ to carry out reaction for 24 hours; cooling to room temperature after the reaction is finished, washing the prepared product with deionized water and absolute ethyl alcohol respectively, and finally drying in vacuum at 50 ℃ to obtain MoS2。
(2)MoS2Preparation of the/PZS complex: weighing 0.1g of molybdenum disulfide, ultrasonically dispersing the molybdenum disulfide in 150mL of mixed solution of tetrahydrofuran and ethanol, then adding 0.1g of hexachlorocyclotriphosphazene and 0.25g of 4, 4' -dihydroxydiphenylsulfone which are precursors of Polyphosphazene (PZS), adding 3mL of triethylamine, after carrying out ultrasonic reaction for 5 hours, respectively washing the mixed solution with deionized water and absolute ethyl alcohol, and drying the mixed solution in a 50 ℃ vacuum drying oven to obtain MoS2a/PZS complex.
(3)MoS2/PZS/Fe3O4Preparation of the complex: 0.05g of MoS was weighed2the/PZS compound, completely dispersed in deionized water, then 0.25g ferrous dichloride-tetrahydrate (FeCl) was weighed2·4H2O) and 0.05g of ferrous trichloride hexahydrate (FeCl)3·6H2O), introducing nitrogen for protection, adding 0.03g of sodium hydroxide (NaOH), carrying out ultrasonic reaction for 2h, washing the reaction solution by deionized water and absolute ethyl alcohol, finally putting the reaction solution into a vacuum drying oven at 50 ℃ for drying, and finally calcining to obtain MoS2/PZS/Fe3O4And (c) a complex.
Example 3
(1) Molybdenum disulfide (MoS)2) The preparation of (1): weighing 24mg of molybdenum trioxide (MoO)3) 28mg of Thioacetamide (TAA) and 200mg of urea are dispersed in 20mL of deionized water, are transferred to the inner liner of a stainless steel reaction kettle to be sealed after being magnetically stirred, and are placed into a blast drying oven at 200 ℃ to carry out reaction for 18 hours; cooling to room temperature after the reaction is finished, washing the prepared product with deionized water and absolute ethyl alcohol respectively, and finally drying in vacuum at 50 ℃ to obtain MoS2。
(2)MoS2Preparation of the/PZS complex: weighing 0.1g of molybdenum disulfide, ultrasonically dispersing the molybdenum disulfide in 150mL of mixed solution of tetrahydrofuran and ethanol, then adding 0.05g of precursor of Polyphosphazene (PZS), 0.1g of hexachlorocyclotriphosphazene and 0.1g of 4, 4' -dihydroxy diphenyl sulfone, adding 2mL of triethylamine, after carrying out ultrasonic reaction for 5 hours, respectively washing the mixed solution with deionized water and absolute ethyl alcohol, and drying the mixed solution in a 50 ℃ vacuum drying oven to obtain MoS2a/PZS complex.
(3)MoS2/PZS/Fe3O4Preparation of the complex: 0.05g of MoS was weighed2the/PZS compound, completely dispersed in deionized water, then 0.25g ferrous dichloride-tetrahydrate (FeCl) was weighed2·4H2O) and 0.06g of ferrous trichloride hexahydrate (FeCl)3·6H2O), introducing nitrogen for protection, adding 0.03g of sodium hydroxide (NaOH), carrying out ultrasonic reaction for 2h, washing the reaction solution by deionized water and absolute ethyl alcohol, finally putting the reaction solution into a vacuum drying oven at 50 ℃ for drying, and finally calcining to obtain MoS2/PZS/Fe3O4And (c) a complex.
Example 4
(1) Molybdenum disulfide (MoS)2) The preparation of (1): weighing 24mg of molybdenum trioxide (MoO)3) 28mg of Thioacetamide (TAA) and 200mg of urea are dispersed in 20mL of deionized water, are transferred to the inner liner of a stainless steel reaction kettle to be sealed after being magnetically stirred, and are placed into a blast drying oven at 200 ℃ to carry out reaction for 18 hours; cooling to room temperature after the reaction is finished, washing the prepared product with deionized water and absolute ethyl alcohol respectively, and finally drying in vacuum at 50 ℃ to obtain MoS2。
(2)MoS2Preparation of the/PZS complex: weighing 0.1g of molybdenum disulfide, ultrasonically dispersing the molybdenum disulfide in 150mL of mixed solution of tetrahydrofuran and ethanol, then adding 0.1g of hexachlorocyclotriphosphazene and 0.25g of 4, 4' -dihydroxydiphenylsulfone which are precursors of Polyphosphazene (PZS), adding 3mL of triethylamine, after carrying out ultrasonic reaction for 10 hours, respectively washing the mixed solution with deionized water and absolute ethyl alcohol, and drying the mixed solution in a 50 ℃ vacuum drying oven to obtain MoS2a/PZS complex.
(3)MoS2/PZS/Fe3O4Preparation of the complex: 0.05g of MoS was weighed2PZS complexThe composition was completely dispersed in deionized water, and then 0.25g ferrous dichloride-tetrahydrate (FeCl) was weighed out2·4H2O) and 0.05g of ferrous trichloride hexahydrate (FeCl)3·6H2O), introducing nitrogen for protection, adding 0.03g of sodium hydroxide (NaOH), carrying out ultrasonic reaction for 2h, washing the reaction solution by deionized water and absolute ethyl alcohol, finally putting the reaction solution into a vacuum drying oven at 50 ℃ for drying, and finally calcining to obtain MoS2/PZS/Fe3O4And (c) a complex.
Example 5
(1) Molybdenum disulfide (MoS)2) The preparation of (1): weighing 24mg of molybdenum trioxide (MoO)3) 28mg of Thioacetamide (TAA) and 200mg of urea are dispersed in 20mL of deionized water, are transferred to the inner liner of a stainless steel reaction kettle to be sealed after being magnetically stirred, and are placed into a blast drying oven at 200 ℃ to carry out reaction for 18 hours; cooling to room temperature after the reaction is finished, washing the prepared product with deionized water and absolute ethyl alcohol respectively, and finally drying in vacuum at 50 ℃ to obtain MoS2。
(2)MoS2Preparation of the/PZS complex: weighing 0.1g of molybdenum disulfide, ultrasonically dispersing the molybdenum disulfide in 150mL of mixed solution of tetrahydrofuran and ethanol, then adding 0.05g of precursor of Polyphosphazene (PZS), 0.1g of hexachlorocyclotriphosphazene and 0.1g of 4, 4' -dihydroxy diphenyl sulfone, adding 2mL of triethylamine, after carrying out ultrasonic reaction for 10 hours, respectively washing the mixed solution with deionized water and absolute ethyl alcohol, and drying the mixed solution in a 50 ℃ vacuum drying oven to obtain MoS2a/PZS complex.
(3)MoS2/PZS/Fe3O4Preparation of the complex: 0.025g of MoS was weighed2the/PZS compound, completely dispersed in deionized water, then 0.25g ferrous dichloride-tetrahydrate (FeCl) was weighed2·4H2O) and 0.06g of ferrous trichloride hexahydrate (FeCl)3·6H2O), introducing nitrogen for protection, adding 0.03g of sodium hydroxide (NaOH), carrying out ultrasonic reaction for 2h, washing the reaction solution by deionized water and absolute ethyl alcohol, finally putting the reaction solution into a vacuum drying oven at 50 ℃ for drying, and finally calcining to obtain MoS2/PZS/Fe3O4And (c) a complex.
Claims (9)
1. A preparation method of a molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material is characterized by comprising the following specific steps:
(1) molybdenum disulfide (MoS)2) The preparation of (1): weighing molybdenum trioxide (MoO)3) Thioacetamide (TAA) and urea are dispersed in deionized water, are transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining after being magnetically stirred, are sealed and are placed into a blast drying box for reaction; cooling to room temperature after the reaction is finished, washing the prepared product with deionized water and absolute ethyl alcohol respectively, and finally carrying out vacuum drying to obtain MoS2；
(2)MoS2Preparation of the/PZS complex: weighing molybdenum disulfide, ultrasonically dispersing the molybdenum disulfide in a mixed solution of tetrahydrofuran and ethanol, then adding hexachlorocyclotriphosphazene and 4, 4' -dihydroxydiphenylsulfone, adding triethylamine, after ultrasonic reaction for a period of time, respectively washing the mixed solution with deionized water and absolute ethyl alcohol, putting the washed mixed solution into a vacuum drying oven for drying to obtain MoS2a/PZS complex;
(3)MoS2/PZS/Fe3O4preparation of the complex: weighing MoS2the/PZS compound is completely dispersed in deionized water, and ferrous dichloride tetrahydrate (FeCl) is weighed2·4H2O) and ferric trichloride hexahydrate (FeCl)3·6H2O), introducing nitrogen for protection, adding sodium hydroxide (NaOH), washing reaction liquid by deionized water and absolute ethyl alcohol after ultrasonic reaction, finally putting the reaction liquid into a vacuum drying oven for drying, and finally calcining at high temperature to obtain MoS2/PZS/Fe3O4A complex;
(4)MoS2/PZS/Fe3O4preparing an electrode: mixing MoS2/PZS/Fe3O4And mixing and grinding the composite, the acetylene black and the polyvinylidene fluoride according to a certain mass ratio, adding N-methyl pyrrolidone (NMP) in the grinding process, coating the uniformly ground mixture on foamed nickel, drying the foamed nickel in an oven, and tabletting by using a tabletting machine to obtain the supercapacitor electrode.
2. The preparation method of molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material according to claim 1, wherein in the step (1), the mass ratio of molybdenum trioxide, thioacetamide and urea is 1:1-1.5: 6-10.
3. The method for preparing the molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material as claimed in claim 1, wherein in the step (1), the reaction temperature in the oven is 200-240 ℃ and the reaction time is 18-24 h; the vacuum drying temperature was 50 ℃.
4. The preparation method of molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material according to claim 1, wherein in the step (2), the mass ratio of molybdenum disulfide, hexachlorocyclotriphosphazene to 4, 4' -dihydroxydiphenylsulfone is 1:1-10: 0.5-2.
5. The preparation method of molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material according to claim 1, wherein in the step (2), the ultrasonic reaction time is 5-10 h; the vacuum oven temperature was 50 ℃.
6. The method for preparing the molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material according to claim 1, wherein in the step (3), the MoS is2PZS complex, FeCl2·4H2O and FeCl3·6H2The mass ratio of O is 1: 5-10: 0.5-10.
7. The preparation method of the molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material according to claim 1, wherein in the step (3), the ultrasonic temperature is controlled at 40-50 ℃; the ultrasonic reaction time is 2 h.
8. The method for preparing a molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material as claimed in claim 1, wherein in the step (3), the temperature rise rate of the calcination is 1-5 ℃/min, the temperature is controlled at 700-900 ℃, and the calcination time is 2-4 hours; the vacuum oven temperature was 50 ℃.
9. The method for preparing the molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material according to claim 1, wherein in the step (4), the MoS is2/PZS/Fe3O4The mass ratio of the composite to the acetylene black to the polyvinylidene fluoride is 7:2: 1; the oven temperature was 60 ℃ and the tablet press pressure was 10 MPa.
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