CN107424845A - A kind of preparation method of used by dye sensitization solar battery to electrode material - Google Patents
A kind of preparation method of used by dye sensitization solar battery to electrode material Download PDFInfo
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- CN107424845A CN107424845A CN201710599827.2A CN201710599827A CN107424845A CN 107424845 A CN107424845 A CN 107424845A CN 201710599827 A CN201710599827 A CN 201710599827A CN 107424845 A CN107424845 A CN 107424845A
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- electrode material
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007772 electrode material Substances 0.000 title claims abstract description 15
- 206010070834 Sensitisation Diseases 0.000 title claims abstract description 12
- 230000008313 sensitization Effects 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 239000002134 carbon nanofiber Substances 0.000 claims abstract description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920000767 polyaniline Polymers 0.000 claims abstract description 17
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 14
- 238000011282 treatment Methods 0.000 claims abstract description 14
- 239000002121 nanofiber Substances 0.000 claims abstract description 12
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003763 carbonization Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical class CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 235000018417 cysteine Nutrition 0.000 claims description 3
- 150000001945 cysteines Chemical class 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001523 electrospinning Methods 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000009388 chemical precipitation Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 238000006479 redox reaction Methods 0.000 abstract description 3
- 238000005868 electrolysis reaction Methods 0.000 abstract description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000000975 dye Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000002023 wood Substances 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
-
- 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)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Hybrid Cells (AREA)
Abstract
A kind of preparation method the invention discloses used by dye sensitization solar battery to electrode material, the present invention prepares polyaniline/polyacrylonitrile composite nano fiber by electrostatic spinning technique, nitrogen-doped carbon nano-fiber is obtained after carbonization treatment, big with draw ratio, low cost and other advantages, the specific surface area of carbon nano-fiber is improved by reducing carbon nano-fiber diameter, it can increase the electric conductivity and stability of composite additionally by nitrogen-atoms is introduced, substrate as composite, more avtive spots can be provided for cobaltosic sulfide catalytic electrolysis matter redox reaction, reduce electronics transfer resistance, and then improve the energy conversion efficiency of battery.
Description
Technical field
The present invention relates to a kind of combination electrode material field, and in particular to a kind of used by dye sensitization solar battery is to electrode
The preparation method of material.
Background technology
As third generation solar cell, DSSC has many good qualities, such as environment-friendly, plasticity
By force, cost is low, energy conversion efficiency is high etc., therefore enjoys the concern of researcher.Typical DSSC
It is made up of the light anode of absorption dyestuff, the electrolyte to electrode and containing oxidation-reduction pair, wherein, as the dye sensitization sun
Can battery important component, play a part of collecting external circuit electronics and catalytic oxidation-reduction electricity to electrode to circular regeneration,
Therefore, the photoelectric properties of DSSC are largely affected to electrode material performance.
To in electrode material, precious metals pt relies on its excellent catalytic performance, high conductance and good chemically stable
Property, it is most widely used, but Pt is high to electrode cost, reserves are limited, has had a strong impact on that it is applied, therefore find a kind of price
It is cheap, rich reserves, and catalytic activity is high particularly significant to electrode material.
Carrying transition metal oxide forms combination electrode material on carbon-based material, electrode can be made to have both above two
The characteristic of electric capacity, greatly improve the chemical property of material.In addition, the chemical property of carbon-based electrode mainly has benefited from material
Specific surface area, and the pore passage structure of carbon-based material itself can accelerate electric transmission.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of preparation of used by dye sensitization solar battery to electrode material
Method, the specific surface area of carbon nano-fiber can be effectively increased, while specific capacitance is obtained significantly by introducing fake capacitance mechanism
Lifting.
The present invention is achieved by the following technical solutions：
A kind of used by dye sensitization solar battery is to the preparation method of electrode material, including step in detail below：
（1）Polyaniline/polyacrylonitrile composite nano fiber：
Weigh 18-26 parts by weight polyanilines to be dissolved in the mixed solution of acetone and DMF, uniform stirring 40-70
Minute, then weigh 38-65 part polyacrylonitrile and be dissolved in above-mentioned polyaniline mixed solution, it is uniform with magnetic stirring apparatus after to be dissolved
15-20 hours are stirred, are configured to polyaniline/polyacrylonitrile electrospun solution, 2-4 hours is stood to remove bubble removing, is transferred to afterwards
In syringe, electrostatic spinning is carried out using syringe pump, obtains polyaniline/polyacrylonitrile composite nano fiber；
（2）Carbonization treatment：
Above-mentioned composite nano fiber is placed in reactor, 230-260 DEG C is warming up to 1-3 DEG C/min speed, is incubated 50-70
Minute, pre-oxidation treatment is carried out, 800-900 DEG C of progress carbonization treatment is warming up to 4-6 DEG C/min speed afterwards, protected in nitrogen
Shield lower insulation 2-3 hours, obtain nitrogen-doped carbon nano-fiber；
（3）Chemical precipitation cobaltosic sulfide：
The nitrogen-doped carbon nano-fiber of above-mentioned preparation and 26-45 parts cobalt nitrate, 4-16 part cysteines are dissolved in 80-140 parts
In ionized water, it is placed in autoclave, in 150-170 DEG C of hydro-thermal reaction 10-14 hour, reaction centrifuges after terminating and removes supernatant,
It is in respectively neutrality with absolute ethyl alcohol and deionized water centrifuge washing to solution by precipitation, black precipitate is placed in drying box and dried
It is dry, obtain nitrogen-doped carbon nano-fiber load cobaltosic sulfide powder；
（4）Preparation to electrode：
Take step（3）Composite granule is placed in agate pot with a certain amount of pick pearl, 60-150 part isopropanols, is sealed, with planetary ball
Grinding machine ball milling 3-5 hours, nitrogen-doped carbon nano-fiber load cobaltosic sulfide slurry is obtained, then using ultrasonic spraying equipment,
Slurry is subjected to ultrasonic atomizatio, is sprayed on and accomplished fluently in advance on the electro-conductive glass of aperture, afterwards by it in nitrogen environmental protection
Under, 25-35 minutes are sintered under the conditions of 480-520 DEG C, are produced to electrode.
Wherein, both volume ratios are 1 in the mixed solution of described acetone and DMF:1.
Wherein, electrospinning conditions are：It is 10-20cm to receive distance, and application voltage is 12-15kV, flow velocity 1ml/h.
Wherein, step（4）The mass ratio of pick pearl and composite granule is 8 during middle ball-milling treatment:1.
Compared with prior art, the present invention has advantages below：
（1）The present invention prepares polyaniline/polyacrylonitrile composite nano fiber by electrostatic spinning technique, is obtained after carbonization treatment
Nitrogen-doped carbon nano-fiber, have draw ratio it is big, low cost and other advantages, improve nano-sized carbon by reducing carbon nano-fiber diameter
The specific surface area of fiber, the electric conductivity and stability of composite can be increased additionally by nitrogen-atoms is introduced, as composite wood
The substrate of material, more avtive spots can be provided for cobaltosic sulfide catalytic electrolysis matter redox reaction, reduce electronics and turn
Resistance is moved, and then improves the energy conversion efficiency of battery.
（2）The present invention uses ultrasonic spraying technology, by ul-trasonic irradiation, makes the vulcanization of nitrogen-doped carbon nano-fiber load four
Three cobalt dust high degree of dispersion, reduce its agglomeration, can be coated uniformly on electro-conductive glass, are provided for redox reaction higher
Catalytic performance, and ultrasonic spraying process can effectively save slurry, improve the utilization rate of slurry, reduce cost.
Embodiment
A kind of used by dye sensitization solar battery is to the preparation method of electrode material, including step in detail below：
（1）Polyaniline/polyacrylonitrile composite nano fiber：
Weigh 18 parts by weight polyanilines to be dissolved in the mixed solution of acetone and DMF, uniform stirring 60 minutes,
52 parts of polyacrylonitrile are weighed again to be dissolved in above-mentioned polyaniline mixed solution, it is small with magnetic stirring apparatus uniform stirring 16 after to be dissolved
When, polyaniline/polyacrylonitrile electrospun solution is configured to, 4 hours is stood to remove bubble removing, is transferred to afterwards in syringe, is utilized
Syringe pump carries out electrostatic spinning, obtains polyaniline/polyacrylonitrile composite nano fiber；
（2）Carbonization treatment：
Above-mentioned composite nano fiber is placed in reactor, 250 DEG C is warming up to 2 DEG C/min speed, is incubated 60 minutes, carry out
Pre-oxidation treatments, 850 DEG C of progress carbonization treatments are warming up to 5 DEG C/min speed afterwards, are incubated 2 hours under nitrogen protection,
Obtain nitrogen-doped carbon nano-fiber；
（3）The nitrogen-doped carbon nano-fiber of above-mentioned preparation and 32 parts of cobalt nitrates, 12 parts of cysteines are dissolved in 120 parts of deionized waters
In, be placed in autoclave, in 160 DEG C of hydro-thermal reactions 12 hours, after reaction terminates centrifugation remove supernatant, use nothing respectively by precipitating
Water-ethanol and deionized water centrifuge washing to solution are in neutrality, and black precipitate is placed in drying box and dried, obtains nitrogen-doped carbon
Nano-fibre supported cobaltosic sulfide powder；
（4）Preparation to electrode：
Take step（3）Composite granule is placed in agate pot with a certain amount of pick pearl, 120 parts of isopropanols, is sealed, with planetary ball mill
Ball milling 4 hours, nitrogen-doped carbon nano-fiber load cobaltosic sulfide slurry is obtained, then using ultrasonic spraying equipment, by slurry
Ultrasonic atomizatio is carried out, is sprayed on and accomplished fluently in advance on the electro-conductive glass of aperture, afterwards by it under nitrogen environmental protection,
Sinter 30 minutes, produced to electrode under the conditions of 500 DEG C.
Wherein, both volume ratios are 1 in the mixed solution of described acetone and DMF:1.
Wherein, electrospinning conditions are：It is 15cm to receive distance, and application voltage is 12kV, flow velocity 1ml/h.
Wherein, step（4）The mass ratio of pick pearl and composite granule is 8 during middle ball-milling treatment:1.
Claims (4)
1. a kind of used by dye sensitization solar battery is to the preparation method of electrode material, it is characterised in that including walking in detail below
Suddenly：
（1）Polyaniline/polyacrylonitrile composite nano fiber：
Weigh 18-26 parts by weight polyanilines to be dissolved in the mixed solution of acetone and DMF, uniform stirring 40-70
Minute, then weigh 38-65 part polyacrylonitrile and be dissolved in above-mentioned polyaniline mixed solution, it is uniform with magnetic stirring apparatus after to be dissolved
15-20 hours are stirred, are configured to polyaniline/polyacrylonitrile electrospun solution, 2-4 hours is stood to remove bubble removing, is transferred to afterwards
In syringe, electrostatic spinning is carried out using syringe pump, obtains polyaniline/polyacrylonitrile composite nano fiber；
（2）Carbonization treatment：
Above-mentioned composite nano fiber is placed in reactor, 230-260 DEG C is warming up to 1-3 DEG C/min speed, is incubated 50-70
Minute, pre-oxidation treatment is carried out, 800-900 DEG C of progress carbonization treatment is warming up to 4-6 DEG C/min speed afterwards, protected in nitrogen
Shield lower insulation 2-3 hours, obtain nitrogen-doped carbon nano-fiber；
（3）Chemical precipitation cobaltosic sulfide：
The nitrogen-doped carbon nano-fiber of above-mentioned preparation and 26-45 parts cobalt nitrate, 4-16 part cysteines are dissolved in 80-140 parts
In ionized water, it is placed in autoclave, in 150-170 DEG C of hydro-thermal reaction 10-14 hour, reaction centrifuges after terminating and removes supernatant,
It is in respectively neutrality with absolute ethyl alcohol and deionized water centrifuge washing to solution by precipitation, black precipitate is placed in drying box and dried
It is dry, obtain nitrogen-doped carbon nano-fiber load cobaltosic sulfide powder；
（4）Preparation to electrode：
Take step（3）Composite granule is placed in agate pot with a certain amount of pick pearl, 60-150 part isopropanols, is sealed, with planetary ball
Grinding machine ball milling 3-5 hours, nitrogen-doped carbon nano-fiber load cobaltosic sulfide slurry is obtained, then using ultrasonic spraying equipment,
Slurry is subjected to ultrasonic atomizatio, is sprayed on and accomplished fluently in advance on the electro-conductive glass of aperture, afterwards by it in nitrogen environmental protection
Under, 25-35 minutes are sintered under the conditions of 480-520 DEG C, are produced to electrode.
2. for a kind of used by dye sensitization solar battery according to claims 1 to the preparation method of electrode material, it is special
Sign is that both volume ratios are 1 in the mixed solution of described acetone and DMF:1.
3. for a kind of used by dye sensitization solar battery according to claims 1 to the preparation method of electrode material, it is special
Sign is that electrospinning conditions are：It is 10-20cm to receive distance, and application voltage is 12-15kV, flow velocity 1ml/h.
4. for a kind of used by dye sensitization solar battery according to claims 1 to the preparation method of electrode material, it is special
Sign is, step（4）The mass ratio of pick pearl and composite granule is 8 during middle ball-milling treatment:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710599827.2A CN107424845A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of used by dye sensitization solar battery to electrode material |
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| CN201710599827.2A CN107424845A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of used by dye sensitization solar battery to electrode material |
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| CN107424845A true CN107424845A (en) | 2017-12-01 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774810A (en) * | 2018-06-25 | 2018-11-09 | 上海交通大学 | A kind of preparation method of nitrogen, fluorine codope micropore carbon nano-fiber |
| CN113903985A (en) * | 2021-09-17 | 2022-01-07 | 海南大学 | Solid electrolyte buffer layer and preparation method thereof |
| CN114373637A (en) * | 2022-01-12 | 2022-04-19 | 河北大学 | Quantum dot sensitized solar cell counter electrode and preparation method thereof |
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| CN105600745A (en) * | 2016-03-18 | 2016-05-25 | 复旦大学 | Cobalt disulfide/carbon nanofiber composite material and preparation method thereof |
| US20160149211A1 (en) * | 2014-11-21 | 2016-05-26 | General Electric Company | Electrode compositions and related energy storage devices |
| CN106770562A (en) * | 2017-03-21 | 2017-05-31 | 安徽工业大学 | A kind of CoS2/ nitrogen-doped graphene composite builds application of the electrochemical sensor in glucose electrochemical analysis |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774810A (en) * | 2018-06-25 | 2018-11-09 | 上海交通大学 | A kind of preparation method of nitrogen, fluorine codope micropore carbon nano-fiber |
| CN108774810B (en) * | 2018-06-25 | 2021-09-24 | 上海交通大学 | Preparation method of nitrogen and fluorine double-doped microporous carbon nanofiber |
| CN113903985A (en) * | 2021-09-17 | 2022-01-07 | 海南大学 | Solid electrolyte buffer layer and preparation method thereof |
| CN113903985B (en) * | 2021-09-17 | 2024-02-23 | 海南大学 | Solid electrolyte buffer layer and preparation method thereof |
| CN114373637A (en) * | 2022-01-12 | 2022-04-19 | 河北大学 | Quantum dot sensitized solar cell counter electrode and preparation method thereof |
| CN114373637B (en) * | 2022-01-12 | 2023-12-12 | 河北大学 | Quantum dot sensitized solar cell counter electrode and preparation method thereof |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171201 |
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| RJ01 | Rejection of invention patent application after publication |