CN106449099A - Photo-anode film based on ZnO nano powder and preparation method thereof - Google Patents
Photo-anode film based on ZnO nano powder and preparation method thereof Download PDFInfo
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- CN106449099A CN106449099A CN201610980589.5A CN201610980589A CN106449099A CN 106449099 A CN106449099 A CN 106449099A CN 201610980589 A CN201610980589 A CN 201610980589A CN 106449099 A CN106449099 A CN 106449099A
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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
- H01G9/0029—Processes of manufacture
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- 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
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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 preparation method of a photo-anode film based on ZnO nano powder. The preparation method includes: calcining a metal organic frame ZIF-8 to obtain the ZnO nano powder, preparing ZnO slurry, and coating the surface of conductive glass with the ZnO slurry to prepare the photo-anode film. In addition, the invention further discloses the photo-anode film prepared by the preparation method. The preparation method is simple in preparation process, controllable in film thickness, adjustable in powder diameter, low in cost, capable of preparing a large-area film, mild in reaction condition, high in controllability and repeatability, suitable for preparing the large-area photo-anode film, beneficial to popularization, application and industrialization, and the like.
Description
Technical field
The present invention relates to technical field of energy material, more particularly, to a kind of zno-based dye-sensitized solar cell anode
The preparation method of film and its prepared photo-anode film.
Background technology
DSSC have the advantages that cheap, environmental friendliness, make simple, it has also become the third generation is too
The representative of sun energy battery.DSSC is by dye sensitization photo-anode film, to electrode and three part groups of electrolyte
Become, wherein photo-anode film is the core component in battery.
At present, photo-anode film is mainly nanocrystalline TiO2Film.Because ZnO has and TiO2Similar energy gap and electricity
Sub- affinity, and the electron diffusion coefficient of ZnO is better than TiO2, therefore ZnO is as the photo-anode film material one contaminating quick battery
Directly placed high hopes by people.Further, since the growth of ZnO crystal has anisotropy and the method for synthesis ZnO crystal is multiple
Various, therefore with respect to TiO2For, ZnO is easier to synthesize the nanostructured of multiple different-shapes, such as wire, lamellar,
Bar-shaped etc..And ZnO nano powder, because it has big specific surface area and preferable light scattering property, more dyestuffs can be adsorbed,
The absorbance of light can be increased, therefore its electricity conversion of battery based on ZnO nano powder photo-anode film is higher simultaneously.So
And, prior art is based on the preparation of ZnO nano powder and contaminates quick battery light anode film, and generally existing complex process, high cost, controllability
With it is difficult to prepare large-area photo-anode film the problems such as poor repeatability, popularization and application are difficult.Therefore, it is badly in need of research and development new
ZnO nano powder photo-anode film preparation method, be beneficial to popularization and application and industrialized realization.
Content of the invention
It is an object of the invention to overcoming the deficiencies in the prior art, provide a kind of system based on ZnO nano powder photo-anode film
Preparation Method, by metal organic frame ZIF-8 calcining is obtained ZnO nano powder, and then produces ZnO slurry and is scratched in leading
Electric substrate surface prepares photo-anode film, thus obtaining big face with process is simple, controllability and repeated strong preparation method
Long-pending photo-anode film, is beneficial to popularization and application and industrialized realization.Another object of the present invention is to provide utilizing above-mentioned system
The photo-anode film that Preparation Method is obtained.
The purpose of the present invention is achieved by the following technical programs：
A kind of preparation method based on ZnO nano powder photo-anode film that the present invention provides, comprises the following steps：
(1) metal organic frame ZIF-8 is calcined and obtain ZnO nano powder；
(2) described ZnO nano powder is dispersed in the mixed solution being made up of ethyl cellulose, terpineol and alcohol solvent
In, rotary evaporation after vibrating and be ultrasonic, obtain ZnO slurry；
(3) described ZnO slurry is coated in conductive substrates surface, after heating through calcining, that is, be obtained be attached in conductive substrates,
The photo-anode film being made up of ZnO nano powder.
Further, in step (1) of the present invention, calcining heat is 450～750 DEG C；The particle diameter of described ZnO nano powder
For 30～100nm.
Further, in step (2) of the present invention, ethyl cellulose is 10cp ethyl cellulose and 46cp ethyl cellulose
Element；Described 10cp ethyl cellulose, 46cp ethyl cellulose, mass-volume concentration in alcohol solvent for the terpineol are respectively
0.1～0.5g/cm3；The shared mass percent concentration in mixed solution of described ZnO nano powder is 1～10wt%.Described step
Suddenly in (2), the time of vibration is 5～10min；The ultrasonic time is 20～40min；Vibration and ultrasonic cycle-index are 3～5
Secondary；The temperature of described rotary evaporation is 70～80 DEG C, and the time is 25～60min.
Further, in step (3) of the present invention ZnO slurry be coated in conductive substrates surface thickness be 7～35 μm；
Heating-up temperature is 80～120 DEG C；Calcining heat is 350～450 DEG C.
In such scheme, metal organic frame ZIF-8 of the present invention is prepared as：By zinc nitrate hexahydrate and 2- methyl miaow
Azoles is dissolved separately in methanol solvate and stirs, and respectively obtains zinc nitrate hexahydrate methanol solution and 2-methylimidazole methanol is molten
Liquid；Then described zinc nitrate hexahydrate methanol solution is poured in 2-methylimidazole methanol solution, carry out after stirring reaction under room temperature
It is centrifuged, washs, is dried, obtain metal organic frame ZIF-8.
Further, in zinc nitrate hexahydrate methanol solution of the present invention, the molar concentration of zinc nitrate hexahydrate is 9～30mM,
In 2-methylimidazole methanol solution, the molar concentration of 2-methylimidazole is 72～240mM.The time of described reaction is 1～3h；Dry
Dry temperature is 50～70 DEG C.
Another object of the present invention is achieved by the following technical programs：
The photo-anode film being obtained using above-mentioned preparation method, the thickness of described photo-anode film is 7～35 μm, and described ZnO receives
The particle diameter of rice flour is 30～100nm.
The invention has the advantages that：
(1) present invention have preparation process is simple, thickness is controlled, powder diameter is adjustable, low cost, can the spy such as large area masking
Point, controllability and repeatability, by force it is adaptable to prepare large-area photo-anode film, are conducive to popularization and application and industrialized realization.
(2) present invention, with zinc nitrate hexahydrate and 2-methylimidazole as raw material, obtains metal organic frame ZIF-8 under room temperature,
Reaction condition is gentle, and the ZnO nano powder obtaining after calcining is used for the preparation of dye-sensitized solar cell anode film, gained
The photo-anode film specific surface area arriving is big, has higher photoelectric transformation efficiency.
Brief description
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail：
Fig. 1 is the field emission scanning electron microscope surface picture of ZnO photo-anode film obtained by the embodiment of the present invention one；
Fig. 2 is the field emission scanning electron microscope cross-section photographs of ZnO photo-anode film obtained by the embodiment of the present invention one；
Fig. 3 be the DSSC that is assembled into of ZnO photo-anode film that the embodiment of the present invention is obtained photoelectric current-
Voltage curve.
Specific embodiment
A kind of preparation method based on ZnO nano powder photo-anode film of the embodiment of the present invention, using the fin oxide condutire of fluorine doped
Glass (FTO) or indium tin oxide-coated glass (ITO) are as conductive substrates.
Embodiment one：
A kind of preparation method of the photo-anode film based on ZnO nano powder of the present embodiment, its step is as follows：
(1) metal organic frame ZIF-8 is calcined and obtain ZnO nano powder
(1-1) preparation of metal organic frame ZIF-8：Weigh 2.93g zinc nitrate hexahydrate and 6.49g 2-methylimidazole divides
It is not placed in two beakers, is separately added into 200mL methanol, magnetic agitation dissolves, and obtaining zinc nitrate hexahydrate molar concentration is
The zinc nitrate hexahydrate methanol solution of 9.85mM, 2-methylimidazole molar concentration are the 2-methylimidazole methanol solution of 79.05mM；So
Afterwards zinc nitrate hexahydrate methanol solution is poured into rapidly in 2-methylimidazole methanol solution, at ambient temperature magnetic agitation reaction
1h, after reaction terminates, centrifugal treating is simultaneously washed 3 times, is dried at a temperature of 50 DEG C with methanol, obtains metal organic frame ZIF-8；
(1-2) in 500 DEG C of temperature lower calcinations after metal organic frame ZIF-8 milling, heating rate is 8 DEG C/min, protects
The warm time is 5h, obtains ZnO nano powder；
(2) preparation of ZnO slurry
2.8g ethyl cellulose (46cp), 2.2g ethyl cellulose (10cp) and 3g terpineol are completely dissolved in 10mL second
Form mixed solution in alcohol；Weigh 1g ZnO nano powder and pour in above-mentioned mixed solution, ultrasonic 20min after vibration 5min,
Repeating this process makes for 4 times ZnO nano powder be uniformly dispersed in mixed solution；Then after rotary evaporation 30min at a temperature of 75 DEG C
Obtain ZnO slurry；
(3) preparation of ZnO photo-anode film
The ZnO slurry of 4 layers of tape thickness is scratched to FTO substrate surface using doctor blade method, 120 DEG C of heating plates heat
Put into calcining in electric furnace after 5min, first rise to 350 DEG C with the heating rate of 8 DEG C/min, with the intensification speed of 8 DEG C/min after insulation 1h
Rate rises to 450 DEG C, Temperature fall after insulation 30min, that is, be obtained and be attached to the light sun forming in conductive substrates, by ZnO nano powder
Pole film.
As shown in figure 1, the size of the present embodiment ZnO nano powder is 50nm.As shown in Fig. 2 the present embodiment light anode
The thickness of film is 30 μm, and thickness can increase with the increase of the adhesive tape number of plies；And photo-anode film is to be made up of ZnO nano powder.
Embodiment two：
A kind of preparation method of the photo-anode film based on ZnO nano powder of the present embodiment, its step is as follows：
(1) metal organic frame ZIF-8 is calcined and obtain ZnO nano powder
(1-1) preparation of metal organic frame ZIF-8：Weigh 5.86g zinc nitrate hexahydrate and 12.98g 2-methylimidazole divides
It is not placed in two beakers, is separately added into 200mL methanol, magnetic agitation dissolves, and obtaining zinc nitrate hexahydrate molar concentration is
The zinc nitrate hexahydrate methanol solution of 19.70mM, 2-methylimidazole molar concentration are the 2-methylimidazole methanol solution of 158.10mM；
Then zinc nitrate hexahydrate methanol solution is poured into rapidly in 2-methylimidazole methanol solution, at ambient temperature magnetic agitation reaction
1h, after reaction terminates, centrifugal treating is simultaneously washed 3 times, is dried at a temperature of 60 DEG C with methanol, obtains metal organic frame ZIF-8；
(1-2) in 550 DEG C of temperature lower calcinations after metal organic frame ZIF-8 milling, heating rate is 8 DEG C/min, protects
The warm time is 5h, obtains ZnO nano powder；
(2) preparation of ZnO slurry
2.8g ethyl cellulose (46cp), 2.2g ethyl cellulose (10cp) and 3.5g terpineol are completely dissolved in 10mL
Form mixed solution in alcohol solvent；Weigh 1.2g ZnO nano powder and pour in above-mentioned mixed solution, super after vibration 5min
Sound 20min, repeating this process makes for 4 times ZnO nano powder be uniformly dispersed in mixed solution；Then rotary evaporation at a temperature of 70 DEG C
ZnO slurry is obtained after 50min；
(3) preparation of ZnO photo-anode film
The ZnO slurry of 4 layers of tape thickness is scratched to FTO substrate surface using doctor blade method, 100 DEG C of heating plates heat
Put into calcining in electric furnace after 5min, first rise to 350 DEG C with the heating rate of 8 DEG C/min, with the intensification speed of 8 DEG C/min after insulation 1h
Rate rises to 450 DEG C, Temperature fall after insulation 30min, that is, be obtained and be attached to the light sun forming in conductive substrates, by ZnO nano powder
Pole film.
Embodiment three：
A kind of preparation method of the photo-anode film based on ZnO nano powder of the present embodiment, its step is as follows：
(1) metal organic frame ZIF-8 is calcined and obtain ZnO nano powder
(1-1) preparation of metal organic frame ZIF-8：Weigh 8.80g zinc nitrate hexahydrate and 12.98g 2-methylimidazole divides
It is not placed in two beakers, is separately added into 200mL methanol, magnetic agitation dissolves, and obtaining zinc nitrate hexahydrate molar concentration is
The zinc nitrate hexahydrate methanol solution of 29.58mM, 2-methylimidazole molar concentration are the 2-methylimidazole methanol solution of 237.15mM；
Then zinc nitrate hexahydrate methanol solution is poured into rapidly in 2-methylimidazole methanol solution, at ambient temperature magnetic agitation reaction
1h, after reaction terminates, centrifugal treating is simultaneously washed 3 times, is dried at a temperature of 70 DEG C with methanol, obtains metal organic frame ZIF-8；
(1-2) in 600 DEG C of temperature lower calcinations after metal organic frame ZIF-8 milling, heating rate is 8 DEG C/min, protects
The warm time is 5h, obtains ZnO nano powder；
(2) preparation of ZnO slurry
2.8g ethyl cellulose (46cp), 2.2g ethyl cellulose (10cp) and 4g terpineol are completely dissolved in 10mL second
Form mixed solution in alcoholic solvent；Weigh 1.5g ZnO nano powder and pour in above-mentioned mixed solution, ultrasonic after vibration 5min
20min, repeating this process makes for 4 times ZnO nano powder be uniformly dispersed in mixed solution；Then rotary evaporation at a temperature of 80 DEG C
ZnO slurry is obtained after 25min；
(3) preparation of ZnO photo-anode film
The ZnO slurry of 4 layers of tape thickness is scratched to FTO substrate surface using doctor blade method, 80 DEG C of heating plates heat
Put into calcining in electric furnace after 5min, first rise to 350 DEG C with the heating rate of 8 DEG C/min, with the intensification speed of 8 DEG C/min after insulation 1h
Rate rises to 450 DEG C, Temperature fall after insulation 30min, that is, be obtained and be attached to the light sun forming in conductive substrates, by ZnO nano powder
Pole film.
Using the photo-anode film obtained by the embodiment of the present invention, make DSSC in accordance with the following methods：
The ZnO photo-anode film of room temperature, room temperature immersion 2h in 0.05mM N719 dyestuff will be cooled to after calcining, take out light
Anode film rinses the N719 dyestuff on surface with dehydrated alcohol, has adsorbed photo-anode film and the pyrolysis of N719 dyestuff after then drying
The FTO of the platinum sandwich structure battery open to electrode composition.Deca electrolyte between in photo-anode film with to electrode, electrolysis
Liquid consist of 0.6M 1- butyl -3- Methylimidazole. iodine salt, 0.06M LiI, 0.03M I2,0.5M 4- tert .-butylpyridine and
The acetonitrile solution of 0.1M guanidinium isothiocyanate.The J-V curve obtaining after test as shown in Figure 3, obtains the photoelectricity of battery after calculating
Conversion efficiency is 2.85%, shows that the ZnO photo-anode film of embodiment of the present invention preparation is applied to DSSC.
Claims (10)
1. a kind of preparation method based on ZnO nano powder photo-anode film is it is characterised in that comprise the following steps：
(1) metal organic frame ZIF-8 is calcined and obtain ZnO nano powder；
(2) described ZnO nano powder is dispersed in the mixed solution being made up of ethyl cellulose, terpineol and alcohol solvent,
Rotary evaporation after vibrating and be ultrasonic, obtains ZnO slurry；
(3) described ZnO slurry is coated in conductive substrates surface, after heating through calcining, that is, be obtained be attached in conductive substrates, by
The photo-anode film of ZnO nano powder composition.
2. the preparation method based on ZnO nano powder photo-anode film according to claim 1 it is characterised in that：Described step
(1) in, calcining heat is 450～750 DEG C；The particle diameter of described ZnO nano powder is 30～100nm.
3. the preparation method based on ZnO nano powder photo-anode film according to claim 1 it is characterised in that：Described step
(2) in, ethyl cellulose is 10cp ethyl cellulose and 46cp ethyl cellulose；Described 10cp ethyl cellulose, 46cp ethyl are fine
Dimension element, mass-volume concentration in alcohol solvent for the terpineol are respectively 0.1～0.5g/cm3；Described ZnO nano powder is in mixing
In solution, shared mass percent concentration is 1～10wt%.
4. the preparation method based on ZnO nano powder photo-anode film according to claim 1 it is characterised in that：Described step
(2) in, the time of vibration is 5～10min；The ultrasonic time is 20～40min；Vibration and ultrasonic cycle-index are 3～5 times；
The temperature of described rotary evaporation is 70～80 DEG C, and the time is 25～60min.
5. the preparation method based on ZnO nano powder photo-anode film according to claim 1 it is characterised in that：Described step
(3) in ZnO slurry be coated in conductive substrates surface thickness be 7～35 μm；Heating-up temperature is 80～120 DEG C；Calcining heat is
350～450 DEG C.
6. the preparation method based on ZnO nano powder photo-anode film according to claim 1 it is characterised in that：Described metal
Organic frame ZIF-8 is prepared as, and zinc nitrate hexahydrate and 2-methylimidazole is dissolved separately in methanol solvate and stirs, point
Do not obtain zinc nitrate hexahydrate methanol solution and 2-methylimidazole methanol solution；Then described zinc nitrate hexahydrate methanol solution is poured into
In 2-methylimidazole methanol solution, carry out after stirring reaction under room temperature being centrifuged, wash, be dried, obtain metal organic frame ZIF-
8.
7. the preparation method based on ZnO nano powder photo-anode film according to claim 6 it is characterised in that：Described six water
In zinc nitrate methanol solution, the molar concentration of zinc nitrate hexahydrate is 9～30mM, 2-methylimidazole in 2-methylimidazole methanol solution
Molar concentration be 72～240mM.
8. the preparation method based on ZnO nano powder photo-anode film according to claim 6 it is characterised in that：Described reaction
Time be 1～3h；Baking temperature is 50～70 DEG C.
9. utilize the photo-anode film that the described preparation method based on ZnO nano powder photo-anode film of one of claim 1-8 is obtained.
10. according to claim 9 based on ZnO nano powder photo-anode film it is characterised in that：The thickness of described photo-anode film
For 7～35 μm, the particle diameter of described ZnO nano powder is 30～100nm.
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Cited By (2)
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| CN109243829A (en) * | 2018-09-19 | 2019-01-18 | 东莞理工学院 | A kind of application of dye-sensitized cell electrode and preparation method thereof and MIL-47 material |
| CN111185150A (en) * | 2020-01-18 | 2020-05-22 | 温州大学 | Preparation method for preparing ZnO crystal based on ZIF-8 |
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| CN111185150A (en) * | 2020-01-18 | 2020-05-22 | 温州大学 | Preparation method for preparing ZnO crystal based on ZIF-8 |
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