CN108648918A - A kind of TiO2(B)NWs/TiO2NP dye-sensitized solar cell anodes and preparation method - Google Patents
A kind of TiO2(B)NWs/TiO2NP dye-sensitized solar cell anodes and preparation method Download PDFInfo
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- CN108648918A CN108648918A CN201810440305.2A CN201810440305A CN108648918A CN 108648918 A CN108648918 A CN 108648918A CN 201810440305 A CN201810440305 A CN 201810440305A CN 108648918 A CN108648918 A CN 108648918A
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- 229910010251 TiO2(B) Inorganic materials 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 113
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 26
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010276 construction Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002070 nanowire Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 8
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000003837 high-temperature calcination Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 235000013339 cereals Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000007790 scraping Methods 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000149 argon plasma sintering Methods 0.000 abstract 1
- 230000031700 light absorption Effects 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 8
- 206010070834 Sensitisation Diseases 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 230000008313 sensitization Effects 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 230000009365 direct transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- -1 NWs) Substances 0.000 description 1
- 229910010455 TiO2 (B) Inorganic materials 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Hybrid Cells (AREA)
Abstract
The present invention relates to a kind of TiO2(B)NWs/TiO2NP dye-sensitized solar cell anodes and preparation method are about 40 μm and flexible TiO using stirring hydro-thermal method and heat treatment process preparation2(B) NWs, then TiO is prepared using mechanical mixing method2(B)NWs/TiO2NP composite constructions.There is TiO by the dye-sensitized solar cells that the composite construction forms2(B) excellent NWs electronic transmission performance and TiO2Specific surface area larger NP can meet sufficient Dye Adsorption amount while improving light induced electron transmission rate.In addition, TiO2(B) light scattering effect of NWs can effectively increase light absorption, final to realize the purpose for improving dye-sensitized solar cells photoelectric conversion efficiency.
Description
Technical field
The invention belongs to technical field of solar cell manufacturing, are related to a kind of TiO2(B)NWs/TiO2The NP dye sensitization sun
It can battery light anode and preparation method.
Background technology
Since 1991, O ' Regan andSince developing dye-sensitized solar cells (DSSC), rely on
At low cost, the simple and higher photoelectric conversion efficiency potentiality of preparation method receive extensive attention.Titania nanoparticles
(TiO2NP) due to large specific surface area, prepare the advantages that simple as the excellent light anode material of dye-sensitized solar cells.
But labyrinth-like meso-hole structure extends the transmission path of electronics, increase electronic interface is compound and by the several of defect capture
Rate；Meanwhile lower electron diffusion coefficient limits further increasing for cell photoelectric transfer efficiency.Research finds one-dimensional TiO2
Nanostructure (nano wire (Nanowires, NWs), nanotube (Nanotube, NT), nanometer rods (Nanorod, NR)) can be improved
The transmission rate and collection efficiency of light induced electron, but its relatively small specific surface area reduces the Dye Adsorption of light anode, leads
It causes the yield of light induced electron to reduce, limits the raising of DSSC photoelectric conversion efficiencies.Therefore by one-dimensional TiO2Nanostructure and TiO2NP
The composite construction of composition becomes the new direction of research.Wherein one-dimensional B phases TiO2(TiO2(B)) nano structural material is due to phase
To open pore structure, along [010] direction there are special parallel channels, higher charge-discharge velocity, high capacitance, excellent is shown
Different photocatalytic activity and chemical property, therefore can be applied to lithium, the electrode material of sode cell, catalyst, humidity sensor material
Material and sensitization solar battery etc..
So far, the researcher of various countries has carried out a large amount of research work to 1-dimention nano composite construction, including
TiO2NWs/TiO2NP, TiO2NT/TiO2NP, TiO2NR/TiO2The composite constructions such as NP.By being found to the retrieval of the prior art,
In " a kind of Anatase and TiO2(B) composite nanostructure titanium dioxide optical catalyst and preparation method thereof " (number of patent application：
201611157665.9) in, inventor is prepared for by anatase phase titanium dioxide quantum dot and TiO2(B) what nanometer sheet was formed answers
Close nanostructure photochemical catalyst.The structure utilizes Anatase and TiO2(B) superior band arrangement realizes high catalytic activity.So
And the TiO of above-mentioned synthesis2(B) if nanometer leaf length is 50nm or so, is applied to the light sun of dye-sensitized solar cells
In extremely, the performance of electronic transmission performance advantage is influenced to a certain extent.Therefore, by a simple method composition length,
The one-dimensional TiO of the controllable high length-diameter ratio of radius2Nanostructure, and construct TiO2(B)NWs/TiO2NP complex light anodes, to improve
The electronic transmission performance of DSSC improves photoelectric conversion efficiency and provides possibility.
Invention content
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of TiO2(B)NWs/TiO2The NP dye sensitization sun
Energy battery light anode and preparation method, overcome using the shorter defect of the nanowire length of prior art preparation, can prepare high length
Diameter than TiO2(B)NWs；Obtain the complex light anode structure with excellent electronic transmission performance and larger specific surface area.
Technical solution
A kind of TiO2(B)NWs/TiO2NP dye-sensitized solar cell anodes, it is characterised in that：By TiO2(B)NWs
And TiO2NP is compounded to form, wherein TiO2(B) mass percent of NWs is less than 70%；The TiO2NWs is that crystalline structure is B phases
TiO2, regular appearance, flexible linear structure, length is about 40 μm；The TiO2NP is Anatase TiO2, received to be spherical
Rice grain structure.
It is a kind of to prepare the TiO2(B)NWs/TiO2The method of NP dye-sensitized solar cell anodes, it is characterised in that
Steps are as follows：
Step 1, TiO2(B) preparation of NWs：It is carried out with the proportioning of the P25 powder of 0.4g and 24g NaOH and 60ml water
It is mixed to form alkaline mixed solution, is then transferred in the stainless steel autoclave with polytetrafluoroethyllining lining, then will reaction
Kettle is placed in the constant-temperature heating magnetic stirring apparatus for filling silicone oil bath, and setting hydrothermal temperature is 120 DEG C~150 DEG C, stirring speed
Rate is 200r min-1~800r min-1, heat preservation 18h~for 24 hours；Reaction kettle is taken out simultaneously from silicone oil bath after the completion of hydro-thermal reaction
It is cooled to room temperature；
Then subsequent processing is carried out：
Collecting reaction product is rinsed using deionized water, is filtered several times until pH=9~10, obtain sodium titanate product；
By the HNO of obtained sodium titanate product and a concentration of 0.1M3Solution is mixed and stirred for 2h~4h, carries out H+Replace Na+
Ion exchange process；It repeatedly rinsed with deionized water again, filter operation up to pH=7, obtain metatitanic acid nano wire, it finally will be anti-
Answer product dry 12h~for 24 hours in 55 DEG C~65 DEG C of air dry oven；
High-temperature calcination is handled again：It is placed in 400 DEG C of calcining 2h~4h in Muffle furnace and obtains TiO2(B) NWs, heating rate, drop
Warm rate is 1~3 DEG C of min-1；
Step 2, TiO2(B)NWs/TiO2The preparation of NP composite constructions：By TiO2(B)NWs、TiO2NP slurries and alcohol are mixed
Conjunction obtains composite mortar, the wherein TiO2(B) mass range of NWs is 0.02g~0.07g, TiO2NP stock qualities are ranging from
0.08g~0.03g, alcohol quality ranging from 0.1g~0.3g；
Scraper method is reused to scratch the composite mortar of preparation on clean FTO.
When the alkaline mixed solution mixing, first ultrasonic disperse 15min~30min, then closed stirring 1h~2h make mixing
Uniformly.
The TiO2(B)NWs、TiO2After NP slurries and alcohol mixing, first ultrasonic disperse 10min~20min is stirred for 2h
Then~3h is further continued for ultrasonic 15min~30min to get to uniformly mixed composite mortar.
It is described scrape the light anode coated and carry out interim heating on heating platform be dried and subsequent heat treatment, at heat
Science and engineering skill is：450 DEG C of 2~4h of heat preservation, heating rate and rate of temperature fall are 1~3 DEG C of min-1。
Advantageous effect
A kind of TiO proposed by the present invention2(B)NWs/TiO2NP dye-sensitized solar cell anodes and preparation method, are adopted
With the composite construction of titanium dioxide nano thread and nano particle.First, the TiO that length is 40 microns is prepared2(B) NWs is utilized
TiO2(B) electron-transporting excellent NWs promotes the quick transmission of light induced electron；Meanwhile the scattering effect of nano wire enhances light
It absorbs.Use mechanical mixing method by TiO again2(B) NWs and TiO2NP is mixed, TiO2Specific surface area larger NP can guarantee foot
Enough Dye Adsorption amounts, generate more light induced electron, improve the photoelectric conversion efficiency of DSSC.Light prepared by the embodiment of the present invention
Anode and routine TiO2NP light anodes are compared, and the short-circuit current density of DSSC is from 10.46mAcm-2It is increased to 14.03mA cm-2, light
Photoelectric transformation efficiency is increased to 5.84% from 4.28%, improves 36.4%.
Compared with prior art, advantages of the present invention is as follows：
(1)TiO2(B)NWs/TiO2NP composite constructions have excellent electron-transporting and larger specific surface area two excellent
Point, not only increases the transmission rate of light induced electron, and ensure that sufficient Dye Adsorption, and DSSC photoelectricity is improved to reach
The purpose of transfer efficiency.
(2)TiO2(B) NWs has more excellent electronic transmission performance relative to anatase phase titanium dioxide nano wire.
Description of the drawings
Fig. 1 is TiO of the present invention2(B)NWs/TiO2NP composite construction radical dye sensitization solar battery light anode structural representations
Figure；
Fig. 2 (a) is TiO prepared by the present invention2(B) X-ray diffractogram of NWs (b) is the TiO of the invention prepared2(B)
The scanning electron microscope (SEM) photograph of NWs；
Fig. 3 is composite construction TiO prepared by the present invention2(B)NWs/TiO2NP light anode base DSSC and refer to TiO2NP light sun
Short circuit currents and open circuit voltage curve of the pole base DSSC in the case where simulating 1.5G sunlights.Wherein 1 is the TiO obtained with example 12
(B)NWs/TiO2DSSC prepared by NP light anodes, 2 be the TiO obtained with example 52DSSC prepared by NP light anodes.
Specific implementation mode
In conjunction with embodiment, attached drawing, the invention will be further described：
TiO2(B)NWs/TiO2NP dye-sensitized solar cell anodes, by TiO2(B) NWs and TiO2NP complexs
At.TiO2(B) NWs can provide direct transmission channel for light induced electron, reduce electronics and compound probability occurs, and promote photoproduction electricity
Effective collection of son；TiO2The adsorbable enough dyestuffs of specific surface area larger NP ensure higher smooth capture rate.
The light anode is by TiO2(B) NWs and TiO2NP is uniformly distributed composition, TiO2NWs is that crystalline structure is B phases
TiO2, TiO2NP is Anatase TiO2, TiO2(B) mass percent of NWs is less than 70%.Wherein TiO2NWs be regular appearance,
Flexible linear structure, length are about 40 μm；TiO2NP is spherical nanoparticles structure.
The TiO2(B) NWs is prepared by stirring hydro-thermal method and heat treatment process, the TiO2(B)NWs/TiO2NP is compound
Structure is prepared by mechanical mixing method.
Include the following steps：
Step 1, TiO2(B) preparation of NWs：Alkaline mixed solution is prepared, mixed solution, which is then transferred to volume, is
In the stainless steel autoclave with polytetrafluoroethyllining lining of 100ml, then reaction kettle is placed in the constant temperature for filling silicone oil bath
It heats in magnetic stirring apparatus, setting hydrothermal temperature is 120 DEG C~150 DEG C, stir speed (S.S.) 200rmin-1~800r min-1, heat preservation 18h~for 24 hours；Reaction kettle is taken out and is cooled to room temperature from silicone oil bath after the completion of hydro-thermal reaction, collecting reaction product
Carry out subsequent processing and high-temperature calcination processing.
Step 2, TiO2(B)NWs/TiO2The preparation of NP composite constructions：Weigh the TiO of certain mass2(B)NWs、TiO2NP
Three is uniformly mixed, wherein TiO by slurry and alcohol2(B) mass range of NWs is 0.02g~0.07g, TiO2NP is starched
Material mass range is 0.08g~0.03g, alcohol quality ranging from 0.1g~0.3g.Reuse composite pulp of the scraper method by preparation
Material blade coating is on clean FTO.
The P25 powder that alkaline mixed solution in the step 1 is 0.4g is mixed with 24g NaOH and 60ml water,
First ultrasonic disperse 15min~30min, then closed stirring 1h~2h make to be uniformly mixed.
The subsequent processing is to be rinsed, filtered several times until pH=9~10 with a large amount of deionized waters；It will obtain again
The HNO of sodium titanate product and a concentration of 0.1M3Solution is mixed and stirred for 2h~4h, carries out ion exchange process (H+Replace Na+)；
Obtained suspension is repeatedly rinsed with deionized water again, filters operation until pH=7, has obtained metatitanic acid nano wire, most at this time
Afterwards by reaction product in 55 DEG C~65 DEG C of air dry oven dry 12h~for 24 hours.
The high-temperature calcination processing obtains TiO for the sample after drying is placed in 400 DEG C of calcining 2h~4h in Muffle furnace2
(B) NWs, heating rate, rate of temperature fall are 1~3 DEG C of min-1。
TiO in the step 22(B)NWs/TiO2The specific preparation flow of NP is：First ultrasonic disperse 10min~20min, then
2h~3h is stirred, is then further continued for ultrasonic 15min~30min, you can obtain uniformly mixed slurry.
After the step 2, the light anode coated will be scraped and carry out interim heating drying process on heating platform with after
Continuous heat treatment.Heat treatment process is：(heating rate, rate of temperature fall are 1~3 DEG C of min to 450 DEG C of 2~4h of heat preservation-1)。
Pass through 7 example detailed description of the present invention technical solutions.
Embodiment 1
The TiO2(B)NWs/TiO2NP composite construction radical dye sensitization solar battery light anodes are by TiO2(B)NWs
And TiO2NP is compounded to form.TiO2(B) NWs can provide direct transmission channel for light induced electron, reduce electronics by defect capture,
Compound probability occurs, promotes effective collection of light induced electron；TiO2The adsorbable enough dyestuffs of specific surface area larger NP,
Ensure higher smooth capture rate.
The TiO2NWs is regular appearance, flexible linear structure, and length is about 40 μm, and crystalline structure is B phases
TiO2；TiO2NP globular nanostructures, average diameter 20nm are Anatase TiO2.By TiO2(B) NWs and TiO2NP is distributed
Uniform composite construction, wherein TiO2(B) mass percent of NWs：0%~70%.The TiO2(B) NWs is by stirring hydro-thermal
Prepared by method and heat treatment process, the TiO2(B)NWs/TiO2NP composite constructions are prepared by mechanical mixing method.
The TiO2(B) mass percent of NWs is 20%.
In 6 embodiments of the present invention, the TiO2(B)NWs/TiO2NP composite construction dye-sensitized solar cells light
The TiO of anode2(B) NWs contents and TiO2(B) NWs appearance structures are different, are specifically shown in Table 1
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| TiO2(B) NWs hydro-thermals stir speed (S.S.) (r min-1) | 800 | 0 | 200 | 400 | 800 | 800 | 800 |
| TiO2(B) NWs contents (wt%) | 50 | 50 | 50 | 50 | 0 | 20 | 70 |
It is proposed by the present invention to prepare the TiO2(B)NWs/TiO2NP composite construction dye-sensitized solar cell anodes
Detailed process be：
The TiO2(B) NWs is prepared by stirring hydro-thermal method and heat treatment process, the TiO2(B)NWs/TiO2NP is compound
Structure is prepared by mechanical mixing method.
The TiO2(B) appearance structure of NWs by hydro-thermal reaction stir speed (S.S.) control, wherein stir speed (S.S.) be 0~
800r min-1；TiO2(B) NWs contents are 0g~0.07g.
What the present embodiment proposed prepares the TiO2(B)NWs/TiO2NP composite construction dye-sensitized solar cells light sun
Pole detailed process is：
Step 1, TiO2(B) preparation of NWs：Alkaline mixed solution is prepared, mixed solution, which is then transferred to volume, is
In the stainless steel autoclave with polytetrafluoroethyllining lining of 100ml, then reaction kettle is placed in the constant temperature for filling silicone oil bath
It heats in magnetic stirring apparatus, setting hydrothermal temperature is 150 DEG C, and stir speed (S.S.) is 0~800r min-1, heat preservation is for 24 hours.
The alkaline mixed solution is the mixing of the P25 powder and 24g NaOH and 60ml water of 0.4g, first ultrasound point
15min is dissipated, then closed stirring 1h makes to be uniformly mixed.
Step 2, reaction kettle is taken out and is cooled to room temperature from silicone oil bath after the completion of hydro-thermal reaction, collecting reaction product,
It rinsed, filtered several times until pH=9 with a large amount of deionized waters；Again by the HNO of obtained sodium titanate product and a concentration of 0.1M3
Solution is mixed and stirred for 4h, carries out ion exchange process (H+Replace Na+)；Obtained suspension is repeatedly rushed with deionized water again
It washes, filter operation until pH=7, has obtained metatitanic acid nano wire, finally by reaction product in 60 DEG C of air dry oven at this time
Drying is for 24 hours.
Step 3, high-temperature calcination is handled：The sample made is placed in heat preservation 2h in 400 DEG C of Muffle furnace and can be obtained TiO2
(B)NWs.Wherein, heating rate, rate of temperature fall are 1 DEG C of min-1。
Step 4, TiO2(B)NWs/TiO2The preparation of NP composite constructions：Weigh the TiO of certain mass2(B)NWs、TiO2NP
Three is uniformly mixed, wherein TiO by slurry and alcohol2(B) quality of NWs is：0g~0.07g, TiO2The quality of NP is
1g~0.03g, alcohol quality are 0g~0.3g.The composite mortar of preparation is scratched on clean FTO using scraper method.
The TiO2(B)NWs/TiO2The specific preparation flow of NP composite constructions is：First ultrasonic disperse 10min, is stirred for
Then 2h is further continued for ultrasonic 15min, you can obtain uniformly mixed slurry.
Step 5, it is dried and is heat-treated the method for taking interim heating treatment.Concrete technology is：It will scrape and coat
Light anode is on heating platform in 30 DEG C of dry 2h, 70 DEG C of dry 2h, 100 DEG C of dry 2h；It is heat-treated after the completion of dry, work
Skill is：(heating rate, rate of temperature fall are 1 DEG C of min to 450 DEG C of heat preservation 2h-1)。
Step 6, preparations of the Pt to electrode：Isopropyl alcohol solution of chloroplatinic acid and the dropwise addition of appropriate a concentration of 5mM are drawn with dropper
Onto electro-conductive glass, 3M adhesive tapes are torn after spontaneously drying, and is put in 380 DEG C of Muffle furnace and keeps the temperature 30min, are then dropped
Can be obtained Pt to room temperature, (wherein, heating rate is 1 DEG C of min to electrode-1, rate of temperature fall is 3 DEG C of min-1)。
Step 7, DSSC assemblings and performance test：50%TiO prepared by embodiment 12(B) NWs/50%TiO2NP is compound
Light anode is placed in N719 dyestuffs, and immersion is protected from light in 60 DEG C for 24 hours, alcohol washes is used after taking-up 2 times, removes unadsorbed dyestuff,
Then drying.Again using heat-sealing film as diaphragm, by the light anode of sensitization and Pt to electrode relative makeup to together, and made using capillary
Clamp is used with by rear between electrolyte two electrodes of instillation, typical sandwich structure DSSC is assembled into, can then test
The photoelectric conversion efficiency of battery.
Subordinate list 1 is the test result of embodiment 1,5
The TiO that subordinate list 1 is prepared using the present invention2(B)NWs/TiO2The dye-sensitized solar cells of NP composite constructions assembling
And routine TiO2The comparison of NP solar cells
Fig. 3 is to be based on TiO2(B)NWs/TiO2NP complex light anode base DSSC and refer to TiO2NP light anode bases DSSC is in mould
Short circuit current under quasi- 1.5G sunlights and open circuit voltage curve.Wherein 1 is the TiO obtained with example 12(B)NWs/TiO2NP light
DSSC prepared by anode, 2 be the TiO obtained with example 52DSSC prepared by NP light anodes.Fig. 3 is confirmed based on TiO2(B)NWs/
TiO2NP complex light anode bases DSSC can increase the short circuit current of battery, to improve the photoelectric conversion efficiency of battery.
Claims (5)
1. a kind of TiO2(B)NWs/TiO2NP dye-sensitized solar cell anodes, it is characterised in that：By TiO2(B) NWs and
TiO2NP is compounded to form, wherein TiO2(B) mass percent of NWs is less than 70%；The TiO2NWs is that crystalline structure is B phases
TiO2, regular appearance, flexible linear structure, length is about 40 μm；The TiO2NP is Anatase TiO2, received to be spherical
Rice grain structure.
2. a kind of preparing TiO described in claim 12(B)NWs/TiO2The method of NP dye-sensitized solar cell anodes,
It is characterized in that steps are as follows：
Step 1, TiO2(B) preparation of NWs：It carries out mixing shape with the proportioning of 24g NaOH and 60ml water with the P25 powder of 0.4g
At alkaline mixed solution, it is then transferred in the stainless steel autoclave with polytetrafluoroethyllining lining, then reaction kettle is placed in
In the constant-temperature heating magnetic stirring apparatus for filling silicone oil bath, setting hydrothermal temperature is 120 DEG C~150 DEG C, and stir speed (S.S.) is
200r min-1~800r min-1, heat preservation 18h~for 24 hours；Reaction kettle is taken out and cooled down from silicone oil bath after the completion of hydro-thermal reaction
To room temperature；
Then subsequent processing is carried out：
Collecting reaction product is rinsed using deionized water, is filtered several times until pH=9~10, obtain sodium titanate product；
By the HNO of obtained sodium titanate product and a concentration of 0.1M3Solution is mixed and stirred for 2h~4h, carries out H+Replace Na+From
Sub- exchange process；It repeatedly rinsed with deionized water again, filter operation until pH=7, obtains metatitanic acid nano wire, finally by reaction production
Object dry 12h~for 24 hours in 55 DEG C~65 DEG C of air dry oven；
High-temperature calcination is handled again：It is placed in 400 DEG C of calcining 2h~4h in Muffle furnace and obtains TiO2(B) NWs, heating rate, rate of temperature fall
It is 1~3 DEG C of min-1；
Step 2, TiO2(B)NWs/TiO2The preparation of NP composite constructions：By TiO2(B)NWs、TiO2NP slurries and alcohol are mixed to get
Composite mortar, the wherein TiO2(B) mass range of NWs is 0.02g~0.07g, TiO2NP stock qualities ranging from 0.08g
~0.03g, alcohol quality ranging from 0.1g~0.3g；
Scraper method is reused to scratch the composite mortar of preparation on clean FTO.
3. according to the method described in claim 2, it is characterized in that：When the alkaline mixed solution mixing, first ultrasonic disperse
15min~30min, then closed stirring 1h~2h make to be uniformly mixed.
4. according to the method described in claim 2, it is characterized in that：The TiO2(B)NWs、TiO2NP slurries and alcohol mixing
Afterwards, first ultrasonic disperse 10min~20min, is stirred for 2h~3h, is then further continued for ultrasonic 15min~30min to get to mixing
Uniform composite mortar.
5. according to the method described in claim 2, it is characterized in that：The light anode coated of scraping is in the enterprising row order of heating platform
Section property heating is dried and subsequent heat treatment, heat treatment process are：450 DEG C of 2~4h of heat preservation, heating rate and rate of temperature fall are equal
For 1~3 DEG C of min-1。
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