CN107799314A - Molybdenum disulfide/titanium carbide/carbon composite nano-fiber film and its preparation method and application - Google Patents
Molybdenum disulfide/titanium carbide/carbon composite nano-fiber film and its preparation method and application Download PDFInfo
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- CN107799314A CN107799314A CN201710936876.0A CN201710936876A CN107799314A CN 107799314 A CN107799314 A CN 107799314A CN 201710936876 A CN201710936876 A CN 201710936876A CN 107799314 A CN107799314 A CN 107799314A
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- molybdenum disulfide
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 105
- 239000002131 composite material Substances 0.000 title claims abstract description 103
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 93
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 68
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000012528 membrane Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 19
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 19
- TVWWSIKTCILRBF-UHFFFAOYSA-N molybdenum trisulfide Chemical compound S=[Mo](=S)=S TVWWSIKTCILRBF-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 2
- 239000000969 carrier Substances 0.000 claims description 2
- 238000010041 electrostatic spinning Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 229910052961 molybdenite Inorganic materials 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 17
- 229920002239 polyacrylonitrile Polymers 0.000 description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 15
- 239000011521 glass Substances 0.000 description 14
- 238000007747 plating Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 238000010792 warming Methods 0.000 description 9
- 239000002134 carbon nanofiber Substances 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 7
- 238000009987 spinning Methods 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000013019 agitation Methods 0.000 description 6
- 239000012300 argon atmosphere Substances 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 229920003944 DuPont™ Surlyn® 1702 Polymers 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000007784 solid electrolyte Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 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
- DYAHQFWOVKZOOW-UHFFFAOYSA-N Sarin Chemical compound CC(C)OP(C)(F)=O DYAHQFWOVKZOOW-UHFFFAOYSA-N 0.000 description 3
- 206010070834 Sensitisation Diseases 0.000 description 3
- 235000011054 acetic acid Nutrition 0.000 description 3
- 150000001243 acetic acids Chemical class 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000520 microinjection Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000008313 sensitization Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 235000015393 sodium molybdate Nutrition 0.000 description 3
- 239000011684 sodium molybdate Substances 0.000 description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000005030 aluminium foil Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 241000549556 Nanos Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002238 carbon nanotube film Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
-
- 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
-
- 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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Hybrid Cells (AREA)
Abstract
The present invention relates to a kind of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film and its preparation method and application, belong to flexible solar battery technical field.The composite nano-fiber membrane is used as to electrode, using titanium carbide/carbon composite nano-fiber film as carrier, is made after loading molybdenum disulfide on titanium carbide/carbon composite nano-fiber membrane carrier by sintering process.The present invention realizes MoS using simple sintering process2And the combination of TiC/C flexible compound nano fibrous membranes, and MoS2Nanofiber surface is evenly distributed in, composite nano-fiber membrane is flexible while greatly improve its electrocatalysis characteristic not destroying.Realize high flexibility, high catalytic activity composite nano-fiber membrane electrode preparation.Based on this to electrode assembling efficient high flexibility DSSC, it is possessed the potentiality combined with textile, DSSC application will have been widened significantly and promoted the development of photovoltaic intelligent textile.
Description
Technical field
The present invention relates to a kind of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film and its preparation method and application, belong to
Flexible solar battery technical field.
Background technology
With the development of science and technology, intelligent textile has been occurred gradually in our visual field, this emerging industry rises abruptly
The progress of human society certainly will will be carried forward vigorously by rising.And the intelligent textile based on battery is one important directions of textile,
It is the key factor for restricting wearable electronic product.Inexhaustible solar energy is converted into the solar cell of electric energy
The favor of numerous researchers is obtained.However, conventional solar cell relative stiffness, meeting how solar cell can
The requirement of wearing turns into the focus of research.
In numerous solar cells, DSSC (Dye-Sensitized Solar Cells, DSSC)
Possess the advantages such as making is simple, material is easy to get, cost is low.Such battery is proposed by professor M.Gratzel since 1991, using tool
There is the nanoporous TiO of high-specific surface area2Instead of traditional plate electrode, about 10 microns of thick optical clear films are formed, then
Dipping dyestuff obtains, and its photoelectric transformation efficiency is up to 7.1%.However, traditional DSSC, due to light anode and to the substrate of electrode all
It is glass, causes battery quality weight, it is frangible, seriously limit its practical application.If it can be made on the high flexibility substrate of lightweight
Standby DSSC, you can obtain high flexibility DSSCs, will be provided with the potentiality being combined with textile, will also be greatly promoted answering for DSSC
With.And the core of high flexibility substrate design is light anode and to electrode, at present, the research of high flexibility light anode is more, and obtains
Certain progress, still, research of the high flexibility to electrode needs further to be strengthened.
It is the important component of DSSC to electrode, it is the electronics for collecting external circuit that it, which is acted on, and
By the I in electrolyte3 -It is reduced to I-.Traditional is typically made up of to electrode platinum plating electro-conductive glass, but alloy platinum material cost is high, long
Phase is using easily by electrolytic corrosion.In recent years, carbon material had good electric conductivity, thermal conductivity, catalytic activity and corrosion resistance
The characteristics of, there is vast potential for future development in the application field to electrode.Therefore, graphene film is thin to electrode, CNT
Film is widely studied to electrode, carbon black film to carbon materials such as electrodes to electrode etc..Although these carbon materials can be effective to electrode
Reduce DSSCs cost, but themselves preparation technology is more complicated, and Yield comparison is low, and with the knot to electrode base board
Close relatively difficult, the stability of battery is also to be improved, thus its practical application is somewhat limited.
In recent years, increasing concern is attracted electrode by the use of the standby carbon nano-fiber of electro-spinning as DSSCs.Such as
Qiao et al. and Lee et al. is respectively by carbon nano-fiber and hollow carbon nanofibres deposit on conducting glass substrate, as right
Application of electrode is in DSCSs.Then, Qiao et al. is by TiO2Nano particle and carbon nano-fiber mixed deposit are in conducting glass substrate
It is upper to be applied to DSSCs.However, because the pure carbon nanofiber membrane low intensity of Static Spinning, fragility are big, it is difficult to combined with flexible substrate,
It is typically only capable to the DSSCs applied to glass substrate.High flexibility how is obtained efficiently to ask electrode as high flexibility DSSC key
One of topic.
The content of the invention
The purpose of the present invention is to be directed to the above-mentioned problems in the prior art, it is proposed that a kind of to have good electro-catalysis
High flexibility molybdenum disulfide/titanium carbide/carbon composite nano-fiber film of activity and charge transport ability.
The purpose of the present invention can be realized by following technical proposal:Molybdenum disulfide/titanium carbide/carbon composite nano-fiber
Film, for the composite nano-fiber membrane using titanium carbide/carbon composite nano-fiber film as carrier, the molybdenum disulfide is carried on the carbon
Change on titanium/carbon composite nano-fiber membrane carrier.
Although titanium carbide is added in carbon nanofiber membrane can significantly improve the pliability of carbon nanofiber membrane and certain
Its electro catalytic activity is improved in degree, but its electro catalytic activity is still difficult to match in excellence or beauty with platinum electrode.And molybdenum disulfide is a kind of high
Catalytic activity to electrode material.Therefore, the present invention is by molybdenum disulfide and flexible titanium carbide/carbon composite nano-fiber film combination,
The electro catalytic activity of flexible nano fiber membrane electrode is significantly improved, and then improves flexible DSSCs electricity conversion.
Second purpose of the invention is the preparation side for providing above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film
Method, the preparation method are:Using titanium carbide/carbon composite nano-fiber film as carrier, received by sintering process titanium carbide/carbon is compound
Rice tunica fibrosa supported on carriers molybdenum disulfide.
In the preparation method of above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, the titanium carbide/carbon is multiple
The preparation method for closing nano fibrous membrane comprises the following steps:
A. configuration contains PVP (polyvinylpyrrolidone), PAN (polyacrylonitrile), PMMA (polymethyls in organic solvent
Sour methyl esters) mixed polymer mixed solution;
B. catalyst and TiP (isopropyl titanate) are added in the mixed solution of above-mentioned preparation, prepared through method of electrostatic spinning
Obtain TiP/PVP/PAN/PMMA composite nano-fiber membranes;
C. the above-mentioned TiP/PVP/PAN/PMMA composite nano-fiber membranes being prepared are pre-oxidized into 1-4 hours, Ran Hou
It is carbonized under inert gas shielding 0.5-2 hours, obtains titanium carbide/carbon composite nano-fiber film.
It is mixed described in step a in the preparation method of above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film
The mass fraction for closing PVP, PAN, PMMA mixed polymer in solution is 9-22%.
In the preparation method of above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, urging described in step b
The dosage of agent is the 3-10% of mixed liquor volume, and catalyst is preferably glacial acetic acid.
In the preparation method of above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, the TiP described in step b
Dosage be 0.2-1.5 times of quality of mixed polymer of PVP, PAN, PMMA.
It is pre- described in step c in the preparation method of above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film
The temperature of oxidation is 200-300, and the temperature of the carbonization described in DEG C is 900-1200.℃
In the preparation method of above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, the sintering process it is specific
Process is:By titanium carbide/carbon composite nano-fiber film and molybdenum trisulfide under inert gas shielding, the constant temperature at 400-800 DEG C
Sinter 3-10 hours.The amount ratio of molybdenum trisulfide and titanium carbide/carbon composite nano-fiber film is any ratio, so manufactured two sulphur
The mass ratio for changing molybdenum and titanium carbide/carbon composite nano-fiber membrane carrier is also any ratio.
3rd purpose of the invention is the application for providing above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, institute
Molybdenum disulfide/titanium carbide/carbon composite nano-fiber film is stated to be used as to electrode.
In the application of above-mentioned molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, the molybdenum disulfide/titanium carbide/
Carbon composite nano-fiber film be used as DSSC to electrode.
Compared with prior art, the present invention realizes MoS using simple sintering process2With TiC/C flexible compound Nanowires
Tie up the combination of film, and MoS2Nanofiber surface is evenly distributed in, it is flexible simultaneously not destroying composite nano-fiber membrane
Greatly improve its electrocatalysis characteristic.Realize high flexibility, high catalytic activity composite nano-fiber membrane electrode preparation.
Based on this to electrode assembling efficient high flexibility DSSC, it is possessed the potentiality combined with textile, DSSC will have been widened significantly
Application and promote photovoltaic intelligent textile development.
Brief description of the drawings
Fig. 1 is the FESEM photos of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from embodiment 1, the upper right corner
For the enlarged drawing of nanofiber;
Fig. 2 is TEM (a) and the HRTEM (b- of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from embodiment 1
C) photo;
Fig. 3 is the XRD spectrum of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from embodiment 1;
Fig. 4 is the XPS full figures (a) of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, Mo 3d made from embodiment 1
And S2p collection of illustrative plates (c) (b).
Fig. 5 is the pliability schematic diagram of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from embodiment 1;
Fig. 6 be molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from embodiment 1 to the CV curves (a) of electrode,
EIS collection of illustrative plates (b), Tafel curves (c);
Fig. 7 is molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from embodiment 1 to the flexibility of electrode assembling
DSSC digital photographs (a) and I-V characteristic curves (b).
Embodiment
It is below the specific embodiment of the present invention, and is described with reference to the drawings and technical scheme is made further to retouch
State, but the present invention is not limited to these embodiments.
Embodiment 1:
It is 1 that 0.28g PAN, 0.28g PVP and 0.56g PMMA, which are added in 6mL DMF solvents, and form mass ratio:1:
2:20 solution, after magnetic agitation 4h, 0.3mL glacial acetic acids and 0.7mL isopropyl titanates are added in the solution, through magnetic agitation
Spinning liquid as precursor is obtained after 12h.Spinning liquid as precursor is fitted into syringe, by micro-injection pump control syringe with
0.8mL/h rate of extrusion, injection thread is formed under the effect of 15kV voltages, shape on receiver board is directly collected with disordered state
Into TiP/PVP/PAN/PMMA composite nano-fiber membranes.The TiP/PVP/PAN/PMMA composite nano-fiber membranes of collection are put into pipe
It is sintered in formula stove, is warming up to 5 DEG C/min speed after 250 DEG C and is incubated 1h, then with 5 DEG C/min's under argon atmosphere
Speed is incubated 0.5h after being warming up to 1000 DEG C, and titanium carbide/carbon composite nano-fiber film of high flexibility is obtained after being cooled to normal temperature.
Prepare sodium molybdate:Vulcanized sodium:Absolute ethyl alcohol:Deionized water quality ratio is 1:5:5:21 mixed solution simultaneously stirs equal
It is even, then volume ratio is slowly added in the solution that stirs for the dilute sulfuric acid (3.6mol/L) of 1.875 times of absolute ethyl alcohols, stood
Brown paste precipitation is produced, precipitates through filtering, washing, brown molybdenum trisulfide powder is obtained after drying.
Titanium carbide/carbon composite nano-fiber film and molybdenum trisulfide powder are inserted into high temperature process furnances, protected in argon atmosphere
Under be warming up to 650 DEG C with 5 DEG C/min speed after be incubated 4h, obtain flexible molybdenum disulfide/titanium carbide/carbon composite nano-fiber
Film.
Fig. 1 is the FESEM photos of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film prepared by the example, by can in figure
There are some classes on molybdenum disulfide/titanium carbide/carbon composite nano-fiber in addition to being uniform-distribution with some nano particles to find out
Like the material of burr shape.Fig. 2 be the example prepare molybdenum disulfide/titanium carbide/carbon composite nano-fiber TEM (a) photos and
HRTEM (b and c) photo, as seen from the figure, the nano particle being distributed on molybdenum disulfide/titanium carbide/carbon nanofiber membrane have TiC and
MoS2, and that burr shape is MoS2.Fig. 3 is molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from the embodiment
XRD, in figure 3, compareed with JCPDS No.75-1539 cards and JCPDS No.32-1383 cards, typical MoS be present2's
The peak crystallization at peak and TiC, so as to confirm MoS2With TiC presence.Fig. 4 XPS collection of illustrative plates (a-c) further demonstrates MoS2's
In the presence of.Fig. 5 is the pliability schematic diagram of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film made from the embodiment, can be seen
Going out tunica fibrosa can significantly bend, and show preferable pliability.
Molybdenum disulfide/titanium carbide/carbon composite nano-fiber film of preparation can be directly as to the flexibility after electrode, with sensitization
Light anode, quasi-solid electrolyte and the heat-seal films of Surlyn 1702 assemble flexible DSSC.Equally, it is multiple based on flexible titanium carbide/carbon
Nano fibrous membrane (prepared by the embodiment preparation method) and plating Pt electro-conductive glass are closed to electrode assembling DSSC.
To molybdenum disulfide/titanium carbide/carbon composite nano-fiber film to electrode, titanium carbide/carbon composite nano-fiber film to electricity
Pole and plating Pt electro-conductive glass carry out test analysis to the chemical property of electrode.Fig. 6 be the embodiment obtained molybdenum disulfide/
Cyclic voltammetric (CV) curve (a) of titanium carbide/carbon composite nano-fiber film, electrochemical impedance spectroscopy (EIS) (b) Ta Feier polarization
(Tafel) curve (c).The negative electrode electricity in molybdenum disulfide/titanium carbide/carbon composite nano-fiber film CV curves can be drawn from figure
Current density IPCFor 23.38mA cm-2, to the series resistance R of electrodesFor 92.71 Ω cm2, charge-transfer resistance RctFor 5.23 Ω
cm2, exchange current density (J0) it is 3.05mA cm-2.The electricity of this explanation molybdenum disulfide/titanium carbide/carbon composite nano-fiber film is urged
Change activity and be better than titanium carbide/carbon composite nano-fiber film to electrode and plating Pt electro-conductive glass to electrode.But charge transport capability
It is weaker than titanium carbide/carbon composite nano-fiber film to electrode and plating Pt electro-conductive glass to electrode.
Respectively with molybdenum disulfide/titanium carbide/carbon composite nano-fiber film of preparation, titanium carbide/carbon composite nano-fiber film
And plating Pt electro-conductive glass is to the flexible TiO after electrode, with sensitization2Light anode, quasi-solid electrolyte and sarin heat-seal film
(Surlyn 1702) heat-seal film is assembled into flexible DSSC, is tested, and compares the performance difference between three class batteries.Fig. 7 is
Flexible DSSC digital photograph and I-V characteristic curves.Flexible DSSC can significantly be bent.It can be drawn from I-V curves, based on two
The flexible DSSC of molybdenum sulfide/titanium carbide/carbon composite nano-fiber film photoelectric transformation efficiency is 5.5%, with titanium carbide/carbon nanometer
Tunica fibrosa is compared to the battery (4.5%) of electrode, improves about 22%;Efficiency higher than Pt/FTO to electrode battery
(4.60%).
Embodiment 2:
0.48g PAN, 0.24g PVP and 0.18g PMMA are added in 6mL DMF solvents, after magnetic agitation 4h,
0.3mL glacial acetic acids and 0.8mL isopropyl titanates are added in the solution, spinning liquid as precursor is obtained after magnetic agitation 12h.By before
Drive body spinning solution to be fitted into syringe, control syringe to make with 0.8mL/h rate of extrusion in 15kV voltages by micro-injection pump
With lower formation injection thread, it is directly collected with disordered state on the aluminium foil of receiver board and forms that TiP/PVP/PAN/PMMA is compound to be received
Rice tunica fibrosa.It is put into tube furnace and is sintered after the TiP/PVP/PAN/PMMA composite nano-fiber membranes of collection are dried, with 1
DEG C/min speed is incubated 2h after being warming up to 210 DEG C, after being then warming up to 900 DEG C under argon atmosphere with 5 DEG C/min speed
2h is incubated, titanium carbide/carbon composite nano-fiber film of high flexibility is obtained after being cooled to normal temperature.
Prepare sodium molybdate:Vulcanized sodium:Absolute ethyl alcohol:Deionized water quality ratio is 1:5:5:21 mixed solution simultaneously stirs equal
It is even, then volume ratio is slowly added in the solution that stirs for the dilute sulfuric acid (3.6mol/L) of 1.875 times of absolute ethyl alcohols, stood
Brown paste precipitation is produced, precipitates through filtering, washing, brown molybdenum trisulfide powder is obtained after drying.
Titanium carbide/carbon composite nano-fiber film and molybdenum trisulfide powder are inserted into high temperature process furnances, protected in argon atmosphere
Under be warming up to 400 DEG C with 5 DEG C/min speed after insulation 8h obtain flexible molybdenum disulfide/titanium carbide/carbon composite nano-fiber film.
To molybdenum disulfide/titanium carbide/carbon composite nano-fiber film to electrode, titanium carbide/carbon composite nano-fiber film to electricity
Pole and plating Pt electro-conductive glass carry out test analysis to the chemical property of electrode.Respectively with molybdenum disulfide/titanium carbide/carbon of preparation
Composite nano-fiber membrane, titanium carbide/carbon composite nano-fiber film and plating Pt electro-conductive glass are to the flexibility after electrode, with sensitization
TiO2Light anode, quasi-solid electrolyte and sarin heat-seal film (Surlyn 1702) heat-seal film are assembled into flexible DSSC, carry out
Test, and compare the performance difference between three class batteries.Sign is similar in embodiment 1 to the process and result of performance test,
Wherein, the photoelectric transformation efficiency of most critical is 4.8%, and this efficiency is slightly above titanium carbide/carbon composite nano-fiber film to electrode
Battery and Pt/FTO are to electrode battery.
Embodiment 3:
0.16g PAN, 0.24g PVP and 0.8g PMMA are added in 6mL DMF solvents, after magnetic agitation 4h, at this
0.3mL glacial acetic acids and 1.0mL isopropyl titanates are added in solution, spinning liquid as precursor is obtained after magnetic agitation 12h.By forerunner
Body spinning solution is fitted into syringe, controls syringe to be acted on 0.8mL/h rate of extrusion in 15kV voltages by micro-injection pump
Lower formation injection thread, formation TiP/PVP/PAN/PMMA composite Nanos on the aluminium foil of receiver board are directly collected with disordered state
Tunica fibrosa.It is put into tube furnace and is sintered after the TiP/PVP/PAN/PMMA composite nano-fiber membranes of collection are dried, with 2
DEG C/min speed is incubated 1h after being warming up to 300 DEG C, after being then warming up to 1200 DEG C under argon atmosphere with 5 DEG C/min speed
0.5h is incubated, titanium carbide/carbon composite nano-fiber film of high flexibility is obtained after being cooled to normal temperature.
Prepare sodium molybdate:Vulcanized sodium:Absolute ethyl alcohol:Deionized water quality ratio is 1:5:5:21 mixed solution simultaneously stirs equal
It is even, then volume ratio is slowly added in the solution that stirs for the dilute sulfuric acid (3.6mol/L) of 1.875 times of absolute ethyl alcohols, stood
Brown paste precipitation is produced, precipitates through filtering, washing, brown molybdenum trisulfide powder is obtained after drying.
Titanium carbide/carbon composite nano-fiber film and molybdenum trisulfide powder are inserted into high temperature process furnances, protected in argon atmosphere
Under be warming up to 800 DEG C with 5 DEG C/min speed after insulation 3h obtain flexible molybdenum disulfide/titanium carbide/carbon composite nano-fiber film.
To molybdenum disulfide/titanium carbide/carbon composite nano-fiber film to electrode, titanium carbide/carbon composite nano-fiber film to electricity
Pole and plating Pt electro-conductive glass carry out test analysis to the chemical property of electrode.Respectively with molybdenum disulfide/titanium carbide/carbon of preparation
Composite nano-fiber membrane, titanium carbide/carbon composite nano-fiber film and plating Pt electro-conductive glass are to the flexibility after electrode, with sensitization
TiO2Light anode, quasi-solid electrolyte and sarin heat-seal film (Surlyn 1702) heat-seal film are assembled into flexible DSSC, carry out
Test, compares the performance difference between three class batteries.Sign is similar in embodiment 1 to the process and result of performance test, its
In, the photoelectric transformation efficiency of most critical has reached 5.3%.
In view of the present invention program embodiment is numerous, each embodiment experimental data is huge numerous, is not suitable for arranging one by one herein
Act explanation, but the content of checking required for each embodiment approaches with obtained final conclusion.So herein not to each reality
The checking content for applying example is illustrated one by one, only illustrates the excellent part of the present patent application using embodiment 1-3 as representative.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology belonging to the present invention is led
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be substituted using similar mode, but simultaneously
Do not deviate by the spirit of the present invention or surmount scope defined in appended claims.
Claims (10)
1. molybdenum disulfide/titanium carbide/carbon composite nano-fiber film, it is characterised in that the composite nano-fiber membrane with titanium carbide/
Carbon composite nano-fiber film is carrier, and the molybdenum disulfide is carried on the titanium carbide/carbon composite nano-fiber membrane carrier.
2. the preparation method of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film as claimed in claim 1, it is characterised in that
The preparation method is:Using titanium carbide/carbon composite nano-fiber film as carrier, by sintering process in titanium carbide/carbon composite nano
Tunica fibrosa supported on carriers molybdenum disulfide.
3. the preparation method of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film according to claim 2, its feature exist
In the preparation method of the titanium carbide/carbon composite nano-fiber film comprises the following steps:
A. the mixed solution of the mixed polymer containing PVP, PAN, PMMA is configured in organic solvent;
B. catalyst and TiP are added in the mixed solution of above-mentioned preparation, TiP/PVP/PAN/ is prepared through method of electrostatic spinning
PMMA composite nano-fiber membranes;
C. the above-mentioned TiP/PVP/PAN/PMMA composite nano-fiber membranes being prepared are pre-oxidized into 1-4 hours, then in inertia
It is carbonized under gas shield 0.5-2 hours, obtains titanium carbide/carbon composite nano-fiber film.
4. the preparation method of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film according to claim 3, its feature exist
In the total mass fraction of PVP, PAN, PMMA mixed polymer is 9-22% in the mixed solution described in step a.
5. the preparation method of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film according to claim 3, its feature exist
In the dosage of the catalyst described in step b is the 3-10% of mixed liquor volume.
6. the preparation method of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film according to claim 3, its feature exist
In the dosage of the TiP described in step b is 0.2-1.5 times of the quality of PVP, PAN, PMMA mixed polymer.
7. the preparation method of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film according to claim 3, its feature exist
In the temperature of the pre-oxidation described in step c is 200-300 DEG C, and the temperature of described carbonization is 900-1200 DEG C.
8. the preparation method of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film according to claim 2, its feature exist
In the detailed process of the sintering process is:By titanium carbide/carbon composite nano-fiber film and molybdenum trisulfide in inert gas shielding
Under, the Isothermal sinter 3-10 hours at 400-800 DEG C.
9. the application of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film as claimed in claim 1, it is characterised in that described
Molybdenum disulfide/titanium carbide/carbon composite nano-fiber film is used as to electrode.
10. the application of molybdenum disulfide/titanium carbide/carbon composite nano-fiber film according to claim 9, it is characterised in that
Molybdenum disulfide/titanium carbide/carbon composite nano-fiber the film be used as DSSC to electrode.
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