CN105244171A - In-situ synthesized ZnO nanometer sheet photoanode film and preparation method - Google Patents
In-situ synthesized ZnO nanometer sheet photoanode film and preparation method Download PDFInfo
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- CN105244171A CN105244171A CN201510700819.3A CN201510700819A CN105244171A CN 105244171 A CN105244171 A CN 105244171A CN 201510700819 A CN201510700819 A CN 201510700819A CN 105244171 A CN105244171 A CN 105244171A
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Abstract
The invention discloses an in-situ synthesized ZnO nanometer sheet photoanode film and a preparation method. The preparation method disclosed by the invention comprises steps of adopting a high concentration zinc nitrate hexahydrate solution and a hexamethylenetetramine water solution, prolonging reaction time of hydro-thermal synthesis and adopting the hydro-thermal synthesis method to prepare a ZnO nanometer sheet dye sensitization solar energy battery photoanode film having a multi-stage structure through in-situ synthesis. The ZnO nanometer sheet prepared by the invention is characterized in that: the prepared two dimension ZnO nanometer shortens the transmission path of the photoproduction electron; the prepared ZnO nanometer sheet film has the micro holes which benefit the diffusion of the electrolyte in the nanometer sheet film; and the prepared ZnO nanometer sheet film has numerous mesoporous which increases the specific surface area of the ZnO nanometer sheet film and benefits the increase of the absorbing capacity of dye so as to increase the short circuit current of a battery. The dye sensitization solar energy battery prepared by the photoanode film prepared by the invention has high photoelectric conversion efficiency. Besides, the in-situ synthesized ZnO nanometer sheet photoanode film disclosed by the invention also has advantages of low reaction temperature, simple technology, simple device and low cost.
Description
Technical field
The present invention relates to technical field of solar batteries, particularly a kind of fabricated in situ ZnO nano sheet photo-anode film and preparation method thereof.
Background technology
Current, investigation and application is solar cell mainly silicon system solar cell the most widely, but to problems such as environments, thus can limit its extensive use because its cost is high, in large, the production process of complex process, energy consumption.1991,
reach the DSSC (DyeSensitizedSolarCell is called for short DSSC) of 7.9% etc. reported first photoelectric conversion efficiency, start the uncharted field of solar cell research and development.DSSC is by light anode, form a few parts such as electrode, dye sensitizing agent, conductive substrates, electrolyte, and wherein light anode is the core component of DSSC.Nano ZnO material is a kind of important DSSC light anode material, and current obtaining answers general research.The ZnO of existing multiple different-shape is applied in DSSC, as ZnO nanorod, multilevel hierarchy ZnO microsphere, ZnO nano grain, ZnO nano-wire and ZnO composite construction etc.The ZnO nano sheet with multilevel hierarchy, owing to having larger specific area and good pore channel, is conducive to increasing the transmission of Dye Adsorption amount, electrolytical diffusion and electronics, is therefore conducive to the raising of efficiency of dye-sensitized solar battery.
Current making ZnO nanometer sheet photo-anode film main method has electrochemical deposition method and chemical bath deposition method, and wherein the film of electrochemical deposition method acquisition is thinner.Chemical bath deposition method mainly adopts two water zinc acetate/methyl alcohol, zinc nitrate hexahydrate/urea is initial action system, and these two kinds of reaction systems can prepare the porous ZnO nanometer sheet of vertical conduction substrate.Zinc nitrate hexahydrate/hexamethylenetetramine water solution system is widely used in the growth of ZnO nanorod, because ZnO is polar crystal, during liquid phase method synthesis ZnO, and growth unit [Zn (OH)
4]
2-be easy to assemble on positive polarity face, promote ZnO crystal and grow fast along c-axis direction, thus it is bar-shaped that ZnO crystal is easily presented.But the specific area of ZnO nanorod light anode is less, and absorbing dye amount is low, thus limits the photoelectric conversion rate of ZnO nanorod DSSC.
Summary of the invention
The object of the invention is the deficiency that will solve prior art problem, a kind of fabricated in situ ZnO nano sheet photo-anode film and preparation method thereof is provided, adopt the zinc nitrate hexahydrate/hexamethylenetetramine aqueous solution of high concentration, and by extending the hydrothermal synthesis reaction time, the ZnO rod of growth being dissolved again and then synthesizes ZnO nano sheet.
For achieving the above object, the present invention implements according to following technical scheme:
A kind of fabricated in situ ZnO nano sheet photo-anode film, comprises FTO electro-conductive glass, also comprise be positioned at FTO electro-conductive glass conductive layer on to be staggeredly stacked the ZnO nano lamella formed by ZnO nano sheet, interlaced, stacking formation micropore between described ZnO nano sheet.
Further, described ZnO nano sheet is made up of ZnO nano particle, and the diameter of ZnO particle is 20 ~ 25nm, is furnished with mesoporous between the ZnO nano particle on described ZnO nano sheet.
A preparation method for fabricated in situ ZnO nano sheet photo-anode film, comprises the following steps:
1) preparation of growth-promoting media: zinc nitrate hexahydrate and hexamethylenetetramine are dissolved in the deionized water of 25 DEG C, and solution is stirred, obtain growth-promoting media, in growth-promoting media, zinc nitrate hexahydrate and hexamethylenetetramine concentration is in aqueous identical;
2) preparation of ZnO nano sheet film: by the conducting surface of FTO electro-conductive glass cleaned up down slant setting in hydrothermal reaction kettle, the growth-promoting media prepared is moved in hydrothermal reaction kettle, and the liquid level of growth-promoting media is higher than FTO electro-conductive glass peak; Hydrothermal reaction kettle is placed in the baking oven being heated to 90 ~ 120 DEG C and carries out hydro-thermal reaction 72 ~ 144h, after reaction terminates, reactor is taken out, and take out the growth in situ FTO electro-conductive glass of film, with deionized water rinsing film surface, to remove responseless growth-promoting media, then film is dry, more dried film is calcined, namely obtain ZnO nano sheet photo-anode film after calcining.
As present invention further optimization scheme, described step 2) in film is carried out baking temperature is 100 ~ 120 DEG C.
As present invention further optimization scheme, described step 2) in film is carried out calcining heat is 250 ~ 450 DEG C.
As present invention further optimization scheme, described step 2) in calcining time heating rate be 8 DEG C/min.
As present invention further optimization scheme, described step 2) in film is calcined after be incubated, temperature retention time is 30 ~ 120min
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention only uses zinc nitrate hexahydrate and hexamethylenetetramine as reaction raw materials, and adopt low-temperature hydrothermal synthetic method, reaction temperature is low, technical process is simple, equipment is simple, and cost is low;
(2) photo-anode film that obtains of the present invention is by having unordered stacking the formed film of multilevel hierarchy ZnO nano sheet, and this ZnO nano sheet film exists two kinds of pore structures simultaneously: a kind of is the micropore of interlaced between nanometer sheet and nanometer sheet, stacking formation; Another kind is that it is mesoporous to be clouded in nanometer sheet, and micropore is conducive to the diffusion of electrolyte in nanometer sheet film; The mesoporous specific area adding ZnO nano sheet film, is conducive to increasing Dye Adsorption amount, thus increases the short circuit current of battery.This structure of ZnO nano sheet film of the present invention is as the advantage of DSSC work electrode: a. is relative to the complete light anode be made up of ZnO nano particle, in ZnO meso-porous nano chip architecture, light induced electron directly can transmit along two-dimensional nano sheet, improves the collection efficiency of light induced electron; The mesoporous specific area substantially increasing nanometer sheet of b. gathering, thus increase Dye Adsorption amount and photogenerated current; C. between nanometer sheet, electrolyte infiltration is convenient in micron-sized space.Therefore, the ZnO nano sheet of double pores system of the present invention is conducive to the transmission at light anode/dyestuff/electrolyte interface of the absorption of dyestuff, the infiltration of electrolyte and electronics, thus obtains higher photoelectric conversion efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation of ZnO nano sheet film of the present invention;
Fig. 2 is the vertical view of ZnO nano sheet film of the present invention;
Fig. 3 is the sectional drawing of the field emission scanning electron microscope (FESEM) of ZnO nano sheet film of the present invention;
Fig. 4 is the exterior view of the field emission scanning electron microscope (FESEM) of ZnO nano sheet film of the present invention;
Fig. 5 is the I-V curve tested after the present invention is assembled into battery.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, is used for explaining the present invention in this illustrative examples of inventing and explanation, but not as a limitation of the invention.
Embodiment one
The preparation process of a kind of ZnO nano of the present embodiment sheet dye-sensitized solar cell anode film is as follows:
(1) preparation of growth-promoting media
The deionized water measuring 140ml with graduated cylinder is poured in beaker, adds 8.32g zinc nitrate hexahydrate and 3.92g hexamethylenetetramine successively under magnetic stirring in beaker, stirs, stirred by solution and obtain growth-promoting media at 25 DEG C; Zinc nitrate hexahydrate and hexamethylenetetramine concentration is in aqueous 0.2M;
(2) preparation of multistage ZnO nano sheet film
The hydrothermal reaction kettle that volume is 200ml is put into by downward-sloping for the electro-conductive glass conducting surface cleaned up, then 140ml growth-promoting media is poured in hydrothermal reaction kettle, the volume filling rate of hydrothermal reaction kettle is 70%, then hydrothermal reaction kettle is put into the baking oven being heated to 90 DEG C and carries out hydro-thermal reaction.The hydro-thermal reaction time is 144h.After hydro-thermal reaction terminates, taken out by reactor, question response still temperature is down to room temperature 25 DEG C, is taken out by film, uses deionized water rinsing film.Dried at 120 DEG C by film, then calcine in Muffle furnace, calcining heat is 350 DEG C, and temperature retention time is 30min, and calcining heating rate is 8 DEG C/min; Thus obtain ZnO nano sheet photo-anode film.
Embodiment two
The preparation process of a kind of ZnO nano of the present embodiment sheet dye-sensitized solar cell anode film is as follows:
(1) preparation of growth-promoting media
The deionized water measuring 140ml with graduated cylinder is poured in beaker, adds 8.32g zinc nitrate hexahydrate and 3.92g hexamethylenetetramine successively under magnetic stirring in beaker, stirs, stirred by solution and obtain growth-promoting media at 25 DEG C; Zinc nitrate hexahydrate and hexamethylenetetramine concentration is in aqueous 0.2M;
(2) preparation of multistage ZnO nano sheet film
The hydrothermal reaction kettle that volume is 200ml is put into by downward-sloping for the electro-conductive glass conducting surface cleaned up, then 140ml growth-promoting media is poured in hydrothermal reaction kettle, the volume filling rate of hydrothermal reaction kettle is 70%, then hydrothermal reaction kettle is put into the baking oven being heated to 90 DEG C and carries out hydro-thermal reaction.The hydro-thermal reaction time is 72h.After hydro-thermal reaction terminates, taken out by reactor, question response still temperature is down to room temperature 25 DEG C, has the electro-conductive glass of film to take out growth, uses deionized water rinsing film.Dried at 120 DEG C by film, then calcine in Muffle furnace, calcining heat is 350 DEG C, and temperature retention time is 30min, and calcining heating rate is 8 DEG C/min; Thus obtain ZnO nano sheet photo-anode film.
Embodiment three
The preparation process of a kind of ZnO nano of the present embodiment sheet dye-sensitized solar cell anode film is as follows:
(1) preparation of growth-promoting media
The deionized water measuring 140ml with graduated cylinder is poured in beaker, adds 8.32g zinc nitrate hexahydrate and 3.92g hexamethylenetetramine successively under magnetic stirring, stirs at 25 DEG C of temperature, stirred by solution and obtain growth-promoting media in beaker; Zinc nitrate hexahydrate and hexamethylenetetramine concentration is in aqueous 0.2M;
(2) preparation of multistage ZnO nano sheet film
The hydrothermal reaction kettle that volume is 200ml is put into by downward-sloping for the electro-conductive glass conducting surface cleaned up, then 140ml growth-promoting media is poured in hydrothermal reaction kettle, the volume filling rate of hydrothermal reaction kettle is 70%, then hydrothermal reaction kettle is put into the baking oven being heated to 120 DEG C and carries out hydro-thermal reaction.The hydro-thermal reaction time is 72h.After hydro-thermal reaction terminates, taken out by reactor, question response still temperature is down to room temperature 25 DEG C, has the electro-conductive glass of film to take out growth, uses deionized water rinsing film.Dried at 120 DEG C by film, then calcine in Muffle furnace, calcining heat is 250 DEG C, and temperature retention time is 30min, and calcining heating rate is 8 DEG C/min; Thus obtain ZnO nano sheet photo-anode film.
Embodiment four
The preparation process of a kind of ZnO nano of the present embodiment sheet dye-sensitized solar cell anode film is as follows:
(1) preparation of growth-promoting media
The deionized water measuring 140ml with graduated cylinder is poured in beaker, adds 16.65g zinc nitrate hexahydrate and 7.85g hexamethylenetetramine successively under magnetic stirring in beaker, stirs, stirred by solution and obtain growth-promoting media at 25 DEG C; Zinc nitrate hexahydrate and hexamethylenetetramine concentration is in aqueous 0.4M;
(2) preparation of multistage ZnO nano sheet film
The hydrothermal reaction kettle that volume is 200ml is put into by downward-sloping for the electro-conductive glass conducting surface cleaned up, then 140ml growth-promoting media is poured in hydrothermal reaction kettle, the volume filling rate of hydrothermal reaction kettle is 70%, then hydrothermal reaction kettle is put into the baking oven being heated to 90 DEG C and carries out hydro-thermal reaction.The hydro-thermal reaction time is 144h.After hydro-thermal reaction terminates, taken out by reactor, question response still temperature is down to room temperature 25 DEG C, has the electro-conductive glass of film to take out growth, uses deionized water rinsing film.Dried at 120 DEG C by film, then calcine in Muffle furnace, calcining heat is 350 DEG C, and temperature retention time is 30min, and calcining heating rate is 8 DEG C/min; Thus obtain ZnO nano sheet photo-anode film.
See the photo-anode film obtained by Fig. 1, Fig. 2, Fig. 3 and Fig. 4 embodiment of the present invention by also comprise be positioned at FTO electro-conductive glass 1 conductive layer on to be staggeredly stacked the ZnO nano lamella 2 formed by ZnO nano sheet, interlaced, stacking formation micropore 3 between described ZnO nano sheet.ZnO nano sheet is made up of ZnO nano particle 4, and the diameter of ZnO particle 4 is 20 ~ 25nm, is furnished with mesoporous 5 between the ZnO nano particle 4 on ZnO nano sheet.
Owing to structure there is micropore and mesoporous in photo-anode film prepared by the present invention, electronics transmits the few feature of fast compound between two-dimensional nano sheet simultaneously, so the performance of battery as shown in Figure 5, ZnO photo-anode film of the present invention makes DSSC concrete steps: will be cooled to the ZnO photo-anode film of 80 DEG C after calcining, under room temperature, 2h is flooded in 0.05mMN719 dyestuff, take out the N719 dyestuff that photo-anode film absolute ethyl alcohol rinses surface, then the photo-anode film of N719 dyestuff has been adsorbed and the FTO of pyrolysis platinum forms open sandwich structure battery to electrode by after oven dry.Light anode and to electrode between drip liquid electrolyte, liquid electrolyte consist of 0.6M1-butyl-3-methylimidazole salt compounded of iodine, 0.06MLiI, 0.03MI
2, 0.5M4-tert .-butylpyridine and 0.1M guanidinium isothiocyanate acetonitrile solution.
Technical scheme of the present invention is not limited to the restriction of above-mentioned specific embodiment, the technology distortion that every technical scheme according to the present invention is made, and all falls within protection scope of the present invention.
Claims (7)
1. a fabricated in situ ZnO nano sheet photo-anode film, comprise FTO electro-conductive glass (1), it is characterized in that, also comprise be positioned at FTO electro-conductive glass (1) conductive layer on to be staggeredly stacked the ZnO nano lamella (2) formed by ZnO nano sheet, interlaced, stacking formation micropore (3) between described ZnO nano sheet.
2. fabricated in situ ZnO nano sheet photo-anode film according to claim 1, it is characterized in that: described ZnO nano sheet is made up of ZnO nano particle (4), the diameter of ZnO particle (4) is 20 ~ 25nm, is furnished with mesoporous (5) between the ZnO nano particle (4) on described ZnO nano sheet.
3. a preparation method for fabricated in situ ZnO nano sheet photo-anode film as claimed in claim 1 or 2, is characterized in that, comprise the following steps:
1) preparation of growth-promoting media: zinc nitrate hexahydrate and hexamethylenetetramine are dissolved in the deionized water of 25 DEG C, and solution is stirred, obtain growth-promoting media, in growth-promoting media, zinc nitrate hexahydrate and hexamethylenetetramine concentration is in aqueous identical;
2) preparation of ZnO nano sheet film: by the conducting surface of FTO electro-conductive glass cleaned up down slant setting in hydrothermal reaction kettle, the growth-promoting media prepared is moved in hydrothermal reaction kettle, and the liquid level of growth-promoting media is higher than FTO electro-conductive glass peak; Hydrothermal reaction kettle is placed in the baking oven being heated to 90 ~ 120 DEG C and carries out hydro-thermal reaction 72 ~ 144h, after reaction terminates, reactor is taken out, and take out the growth in situ FTO electro-conductive glass of film, with deionized water rinsing film surface, to remove responseless growth-promoting media, then film is dry, more dried film is calcined, namely obtain ZnO nano sheet photo-anode film after calcining.
4. the preparation method of fabricated in situ ZnO nano sheet photo-anode film according to claim 3, is characterized in that: described step 2) in film is carried out baking temperature is 100 ~ 120 DEG C.
5. the preparation method of fabricated in situ ZnO nano sheet photo-anode film according to claim 3, is characterized in that: described step 2) in film is carried out calcining heat is 250 ~ 450 DEG C.
6. the preparation method of fabricated in situ ZnO nano sheet photo-anode film according to claim 3, is characterized in that: described step 2) in calcining time heating rate be 8 DEG C/min.
7. the preparation method of fabricated in situ ZnO nano sheet photo-anode film according to claim 3, is characterized in that: described step 2) in film is calcined after be incubated, temperature retention time is 30 ~ 120min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381513A (en) * | 2016-08-31 | 2017-02-08 | 昆明理工大学 | Preparation method and application of multi-stage nanosheet zinc oxide |
| CN109872877A (en) * | 2019-02-28 | 2019-06-11 | 江苏赛清科技有限公司 | A kind of dye-sensitized solar cells ZnO photo-anode and preparation method thereof |
| CN109879607A (en) * | 2019-03-28 | 2019-06-14 | 中国民航大学 | The preparation method of the modified hydrophobic automatically cleaning film of ZnO/ZnS nano-chip arrays |
-
2015
- 2015-10-26 CN CN201510700819.3A patent/CN105244171B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
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| HU X ET.AL.: "A Facile Template-free Route to Synthesize Porous ZnO Nanosheets with High Surface Area", <JOURNAL OF ALLOYS AND COMPOUNDS> * |
| 王艳香 等: "垂直导电衬底的ZnO纳米片的制备及其染料敏化太阳电池的性能", 《人工晶体学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381513A (en) * | 2016-08-31 | 2017-02-08 | 昆明理工大学 | Preparation method and application of multi-stage nanosheet zinc oxide |
| CN109872877A (en) * | 2019-02-28 | 2019-06-11 | 江苏赛清科技有限公司 | A kind of dye-sensitized solar cells ZnO photo-anode and preparation method thereof |
| CN109879607A (en) * | 2019-03-28 | 2019-06-14 | 中国民航大学 | The preparation method of the modified hydrophobic automatically cleaning film of ZnO/ZnS nano-chip arrays |
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