CN106024396B - It is a kind of for dye-sensitized solar cells to electrode and preparation method thereof - Google Patents
It is a kind of for dye-sensitized solar cells to electrode and preparation method thereof Download PDFInfo
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- CN106024396B CN106024396B CN201610550243.1A CN201610550243A CN106024396B CN 106024396 B CN106024396 B CN 106024396B CN 201610550243 A CN201610550243 A CN 201610550243A CN 106024396 B CN106024396 B CN 106024396B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
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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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a kind of for dye-sensitized solar cells to electrode and preparation method thereof, this is to electrode by conductive substrates and the LiFePO being adhered in conductive substrates4Catalytic active layer forms.Preparation method is：1) LiFePO is prepared4Base is to electrode slurry：By LiFePO4, nano-titanium dioxide, ethyl cellulose ethanol solution, terpinol mixing after through high speed ball mill grind 1~2 hour, obtain LiFePO4Base is to electrode slurry；2) it prepares to electrode：Electrode slurry will uniformly be scratched or is spun in conductive substrates; low-temperature prewarming is first carried out at 60~80 DEG C; drying to be coated is placed in the tube furnace of logical protection gas; programmed temperature method is warming up to 450~500 DEG C; heat preservation 30~60 minutes; LiFePO4 catalytic active layers are formed, cooled to room temperature, stop logical protection gas.The electrode has preferable catalytic effect to iodine electrolyte, can obtain and short-circuit current density and open-circuit voltage similar in platinum electrode.The preparation method technical process is simple, easy to operate, easy to control, safe.
Description
Technical field
The present invention relates to technical field of solar batteries, and in particular to it is a kind of for dye-sensitized solar cells to electricity
Pole and preparation method thereof.
Background technology
Dye-sensitized solar cells is due to the advantages such as at low cost, assembling is simple, receiving more and more attention.And
Be mainly noble metal platinum to the material of electrode currently used for dye-sensitized solar cells, platinum base electrode to iodine electrolyte have compared with
Good intrinsic catalytic performance and good electric conductivity can obtain higher transformation efficiency after being assembled into battery device, but due to
The rarity and expensive price of platinum, and it is weaker to the resistance to corrosion of iodo electrolyte, it is limited as dyestuff
Large-scale application of the sensitization solar battery to electrode material.
A large amount of phase has been done in order to seek the new material that can substitute platinum electrode or the usage amount for reducing platinum, researcher
Work is closed, attempts various types of materials being used as to electrode, such as porous carbon, transient metal sulfide, selenides, nitride and carbide
Deng these researchs obtain electricity conversion close to platinum electrode.But material mentioned above is all to test mostly
Room synthesis, synthesis process is complex, and cost is higher, and distance, which produces counter electrode of dye sensitization battery in enormous quantities, still one
Fixed distance.So if a kind of material of heavy industrialization can be used to be prepared for electrode, production will be greatly reduced
Cost certainly will push the functionization of dye-sensitized solar cells.
Invention content
To solve the above-mentioned problems of the prior art, the present invention provides a kind of for dye-sensitized solar cells
To electrode and preparation method thereof, this not only has preferable catalytic effect to iodine electrolyte to electrode, can obtain and pure platinum electrode
Similar short-circuit current density and open-circuit voltage.
The preparation method technical process is simple, easy to operate, easy to control, safe.
Realize that technical solution used in above-mentioned purpose of the present invention is：
It is a kind of for dye-sensitized solar cells to electrode, by conductive substrates and be adhered in conductive substrates
LiFePO4Catalytic active layer forms.
Preferably, the conductive substrates are FTO electro-conductive glass, ITO conductive films, AZO electro-conductive glass or metal titanium sheet.
A kind of preparation method to electrode for dye-sensitized solar cells includes the following steps：
1) LiFePO is prepared4Base is to electrode slurry：
By LiFePO4, nano-titanium dioxide, ethyl cellulose ethanol solution, carry out ball milling after terpinol mixing, ethyl is fine
The mass fraction of the plain ethanol solution of dimension is 5~15%, LiFePO4Mass ratio with nano-titanium dioxide is 10~15：1, ethyl
Cellulosic ethanol solution and LiFePO4Mass ratio with both nano-titanium dioxides is 1：1~3, the quality of terpinol is ethyl
2~4 times of cellulosic ethanol solution quality, mixed material are ground 1~2 hour through high speed ball mill, obtain uniform sticky shape
LiFePO4Base is to electrode slurry；
2) it prepares to electrode：
By LiFePO4Base is uniformly scratched or is spun in conductive substrates to electrode slurry, first by conductive substrates 60~80
Low-temperature prewarming is carried out at DEG C, waits for the LiFePO in conductive substrates4After base is to electrode slurry coated and dried, conductive substrates are placed in logical
In the tube furnace for protecting gas, while 450~500 DEG C being warming up to using the method for temperature programming, heating rate is 2~4 DEG C/min,
Heat preservation 30~60 minutes, LiFePO4 catalytic active layers are formed, cooled to room temperature, and stopping is passed through protection gas, obtains and is used for
Dye-sensitized solar cells to electrode.
Preferably, the LiFePO4For the LITHIUM BATTERY product having been commercialized, the mass fraction of wherein carbon is less than
0.2%.
Preferably, the protection gas is nitrogen or argon gas.
Preferably, the grain size of the nano-titanium dioxide is 25nm.
Compared with prior art, the advantages of the present invention are：
1) present invention's has preferable catalytic effect to electrode to iodine electrolyte.
2) LiFePO to electrode of the invention4Adhesiveness of the catalytic active layer on electro-conductive glass is preferable, not easily to fall off.
3) preparation method of the invention is simple to operation, safe, and used raw material sources are extensive, cheap, prepares
Low to process conditions, equipment requirement in the process, therefore, the preparation method production cost is low, is suitble to industrialized production.
Description of the drawings
Fig. 1 is that the X to electrode (being indicated with LFPO in figure) for dye-sensitized solar cells prepared by embodiment 1 is penetrated
Ray diffraction diagram.
Fig. 2 is the SEM figures (scanning electron microscope (SEM) photograph) for dye-sensitized solar cells to electrode prepared by embodiment 1.
Fig. 3 is the LiFePO based on the present invention4Dye-sensitized solar cells (test cell) that base prepares electrode and
I~V curve graphs based on dye-sensitized solar cells (control cell) prepared by platinum electrode.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
1, LiFePO is prepared4Base is to electrode slurry：
By 2g commercial batteries grades LiFePO4(mass fraction of carbon is less than 0.2%), the nanometer that 0.2g grain sizes are 25nm
Titanium dioxide, 1g ethyl celluloses ethanol solution and 4ml terpinols are mixed evenly, and mixed material is through QM-3B type clipping the balls
Grinding machine grinds 2h with 1200 revs/min of speed, obtains uniformly sticky LiFePO4Base is to electrode slurry.
2, it prepares to electrode：
3M adhesive tapes are sticked at clean FTO (the SnO2 transparent conducting glass of doping fluorine) both ends, are fixed on platform, film
Thickness is controlled by the number of plies of 3M adhesive tapes, is single layer 3M adhesive tapes in the present invention.The LiFePO first prepared by step 14Base is to electrode
Slurry drops on the conducting surface of FTO, and slurry is scratched back and forth using the method for blade coating, until uniformly neat film coating is formed,
Then FTO is subjected to low-temperature prewarming on 70 DEG C of heated at constant temperature platform, waits for the LiFePO on FTO4Base dries electrode slurry coating
It after dry, is then transferred in the tube furnace of logical nitrogen, while 450 DEG C is warming up to using the method for temperature programming, heating rate 2
DEG C/min, keep the temperature 30min, LiFePO4Catalytic active layer is formed, cooled to room temperature (20-30 DEG C), and stopping is passed through nitrogen,
It obtains for dye-sensitized solar cells to electrode.
X-ray diffraction analysis, XRD are carried out to electrode for dye-sensitized solar cells by manufactured in the present embodiment
Figure is as shown in Figure 1, as shown in Figure 1, prepare LiFePO4During catalytic active layer, after high-temperature process, the structure of LiFePO4
Do not change, it is almost the same with standard spectrogram.
Electronic Speculum morphology analysis is scanned to electrode for dye-sensitized solar cells by manufactured in the present embodiment,
SEM schemes as shown in Fig. 2, as shown in Figure 2, preparation it is larger to electrode surface roughness, and micropore not of uniform size is distributed with,
These shape characteristics show that this has larger specific surface area to electrode, can be provided for the quick reduction of iodide ion in electrolyte
More active sites are the major reasons that the electrode can obtain preferable electricity conversion.
Embodiment 2
1, LiFePO is prepared4Base is to electrode slurry：
By 4g commercial batteries grades LiFePO4(mass fraction of carbon is less than 0.2%), the nanometer that 0.3g grain sizes are 25nm
Titanium dioxide, 1.5g ethyl celluloses ethanol solution and 6ml terpinols are mixed evenly, and are placed in ball milling 1.5h in ball grinder,
Obtain uniform LiFePO4Base is to electrode slurry.
2, it prepares to electrode：
By LiFePO4Base scratches on clean ITO (indium tin oxide transparent conductive semiconductor glass) electrode slurry,
Subsequent step is the same as embodiment one.
Embodiment 3
1, LiFePO is prepared4Base is to electrode slurry：
By 6g commercial batteries grades LiFePO4(mass fraction of carbon is less than 0.2%), the nanometer that 0.4g grain sizes are 25nm
Titanium dioxide, 2g ethyl celluloses ethanol solution and 8ml terpinols are mixed evenly, and are placed in ball milling 1.5h in ball grinder, obtain
To uniform LiFePO4Base is to electrode slurry.
2, it prepares to electrode：
By LiFePO4Base scratches in clean AZO (zinc oxide (ZnO) transparent conducting glass of aluminium doping) electrode slurry
On, subsequent step is the same as embodiment one.
Embodiment 4
1, LiFePO is prepared4Base is to electrode slurry：
By 3g commercial batteries grades LiFePO4(mass fraction of carbon is less than 0.2%), 0.25g grain sizes are receiving for 25nm
Rice titanium dioxide, the ethanol solution of 2g ethyl celluloses and 5ml terpinols are mixed evenly, and are placed in ball milling h in ball grinder, obtain
To uniform LiFePO4Base is to electrode slurry.
2, it prepares to electrode：
By LiFePO4Base scratches in clean metal titanium sheet electrode slurry, and subsequent step is the same as embodiment one.
Embodiment 5
1, LiFePO is prepared4Base is to electrode slurry：
By 2g commercial batteries grades LiFePO4(mass fraction of carbon is less than 0.2%), the nanometer that 0.2g grain sizes are 25nm
Titanium dioxide, 1g ethyl celluloses ethanol solution and 8ml terpinols are mixed evenly, and mixed material is through QM-3B type clipping the balls
Grinding machine grinds 2h with 1200 revs/min of speed, has obtained uniform LiFePO4To electrode slurry, the LiFePO with embodiment 14Base
Electrode slurry is compared, concentration is relatively dilute.
2, it prepares to electrode：
It is prepared to electrode using the method for spin coating, film thickness is controlled by spin speed and spin-coating time.It prepared by step 1
LiFePO4 bases electrode slurry is dropped on FTO, using KW-4A type spin coaters by 700rpm/s rate spin coating 18s after, shape
At neat uniform film coating, then places it on 60 DEG C of heated at constant temperature platform and carry out low-temperature prewarming, wait and be adhered to FTO
On LiFePO4 bases electrode slurry coating is slowly dried, when becoming curdled appearance, be then transferred in the tube furnace of logical argon gas,
500 DEG C are warming up to using the method for temperature programming simultaneously, heating rate is 4 DEG C/min, keeps the temperature 60min, LiFePO4Catalytic activity
Layer is formed, cooled to room temperature (20-30 DEG C), and stopping is passed through nitrogen, obtains pair for dye-sensitized solar cells
Electrode.
Comparative example 1
First by the aqueous isopropanol drop coating of 1/50g/ml chloroplatinic acids on the FTO conducting surfaces that size is 2.5cm × 1.5cm,
FTO is placed in Muffle furnace again, is sintered 30 minutes at 390 DEG C, with stove cooled to room temperature (20-30 DEG C), platinum pair is made
Electrode.
Experiment one prepares dye-sensitized solar cells to electrode using the present invention and measures its electricity conversion
Experimental method：
1, the LiFePO based on the present invention is prepared4Dye-sensitized solar cells (test cell) of the base to electrode：
1) FTO electro-conductive glass is cleaned with water, ethyl alcohol and acetone successively, titania slurry is passed through into screen printing technique
It is printed on FTO electro-conductive glass, then at 500 DEG C of heat treatment 2h, obtains light anode.
2) by light anode in bis- (isothiocyanos) bis- (2,2 '-bipyridyl -4,4'- dicarboxyls) rutheniums of 60 DEG C of 0.5mM
(II) 12h is impregnated in the ethanol solution of (N3) dyestuff, completes dye sensitization process.
3) 3M adhesive tapes are affixed on the both ends to electrode prepared by embodiment 1, prevent short circuit, using clip by its be sensitized
Light anode be fixed together, then by iodo electrolyte inject crack between, be just simply completed dye sensitization too in this way
Positive energy battery.
2, it prepares based on platinum to the dye-sensitized solar cells (control cell) of electrode
The manufacturing process of the dye-sensitized solar cells of electrode is same as above based on platinum, pair that embodiment 1 need to be only prepared
Electrode changes platinum into electrode.
3, the test of dye-sensitized solar cells electrical property
The electricity being connected with test equipment is clipped in the LiFePO based on the present invention4Dye sensitization of solar of the base to electrode
For the light anode of battery on electrode, control intensity of illumination is 100mw/cm2, the work area of battery is 0.25cm2, to be based on
Platinum is control to the dye-sensitized solar cells of electrode.Measure short-circuit photocurrent (Isc), open-circuit photovoltage (Voc), filling because
Sub (ff) and photoelectric conversion efficiency (η), wherein fill factor refer on the point for can get in I~V curves peak power output
Current Voltage product (Iopt × Vopt) and the ratio between Isc × Voc (Isc is short-circuit photocurrent, and Voc is open-circuit photovoltage), electricity
Transfer efficiency is the ratio between Iopt × Vopt and the luminous power Pin of input, and Pin herein is 25mw.
Test result：
LiFePO based on the present invention4Base is to the dye-sensitized solar cells (test cell) of electrode and based on platinum to electricity
The I-V curve figure of the dye-sensitized solar cells (control cell) of pole is as shown in figure 3, from the figure 3, it may be seen that the dyestuff of the present invention is quick
Change solar cell (test cell) short-circuit photocurrent, open-circuit photovoltage, fill factor and photoelectric conversion efficiency be respectively
11.61mAcm-2, 0.72V, 0.506 and 4.24%, the dye-sensitized solar cells (control cell) prepared based on platinum electrode
Short-circuit photocurrent, open-circuit photovoltage, fill factor and photoelectric conversion efficiency are respectively 11.81mAcm-2, 0.74V, 0.622 and
5.47%.The result shows that being based on LiFePO of the present invention4Base is to its open-circuit voltage of the dye-sensitized solar cells of electrode and short circuit
The indexs such as current density have reached platinum to the 98% of electrode, and total transfer efficiency reaches platinum to the 78% of electrode, and is prepared into
This is but well below platinum to electrode.
It can be seen that using commercialization LiFePO4 preparations to electrode, short-circuit current density and open-circuit voltage,
It is essentially identical to existing platinum electrode, shows that the electrode reveals preferable catalytic performance to iodine electrolyte meter, is being greatly reduced into
Under the premise of this, which helps to push dye-sensitized solar cells practical, shows preferable application prospect.
Claims (5)
1. a kind of preparation method to electrode for dye-sensitized solar cells, it is characterised in that include the following steps：
1) LiFePO is prepared4Base is to electrode slurry：
By LiFePO4, nano-titanium dioxide, ethyl cellulose ethanol solution, terpinol mixing after carry out ball milling, ethyl cellulose
The mass fraction of ethanol solution is 5~15%, LiFePO4Mass ratio with nano-titanium dioxide is 10~15：1, ethyl cellulose
Plain ethanol solution and LiFePO4The mass ratio of the two is 1：1~4, the quality of terpinol is ethyl cellulose ethanol solution quality
2~8 times, mixed material is ground 1~2 hour through high speed ball mill, obtains uniform sticky shape LiFePO4Base is to electrode slurry
Material；
2) it prepares to electrode：
By LiFePO4Base is uniformly scratched or is spun in conductive substrates to electrode slurry, first by conductive substrates at 60~80 DEG C into
Row low-temperature prewarming waits for the LiFePO in conductive substrates4After base is to electrode slurry coated and dried, conductive substrates are placed in logical protection gas
Tube furnace in, while being warming up to 450~500 DEG C using the method for temperature programming, heating rate is 2~4 DEG C/min, heat preservation 30
~60 minutes, LiFePO4 catalytic active layers were formed, cooled to room temperature, and stopping is passed through protection gas, obtains quick for dyestuff
Change solar cell to electrode.
2. the preparation method to electrode according to claim 1 for dye-sensitized solar cells, it is characterised in that：
The conductive substrates are FTO electro-conductive glass, ITO conductive films or AZO electro-conductive glass.
3. the preparation method to electrode according to claim 1 for dye-sensitized solar cells, it is characterised in that：
The LiFePO4The mass fraction of middle carbon is less than 0.2%.
4. the preparation method to electrode according to claim 1 for dye-sensitized solar cells, it is characterised in that：
The protection gas is nitrogen or argon gas.
5. the preparation method to electrode according to claim 1 for dye-sensitized solar cells, it is characterised in that：
The grain size of the nano-titanium dioxide is 25nm.
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| CN105551804A (en) * | 2016-01-28 | 2016-05-04 | 常州大学 | Photocathode and quantum dot-sensitized solar cell comprising same |
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| CN102347143A (en) * | 2011-07-11 | 2012-02-08 | 中国科学院上海硅酸盐研究所 | Graphene composite porous counter electrode, preparation method and application thereof |
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