CN104992838A - Preparation method of zinc oxide absorption film - Google Patents
Preparation method of zinc oxide absorption film Download PDFInfo
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- CN104992838A CN104992838A CN201510407915.9A CN201510407915A CN104992838A CN 104992838 A CN104992838 A CN 104992838A CN 201510407915 A CN201510407915 A CN 201510407915A CN 104992838 A CN104992838 A CN 104992838A
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- conductive substrates
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- absorbing membrane
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- Y02E10/542—Dye sensitized solar cells
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Abstract
Provided is a preparation method of a zinc oxide absorption film. The method has the following specific steps: carrying out ultrasonic cleaning on a conductive substrate and drying the substrate with N2 to obtain a cleaned conductive substrate; immersing the cleaned conductive substrate into a first mixed solution to obtain a first conductive substrate, wherein the ingredients of the first mixed solution are SnCl2 and HCl; immersing the first conductive substrate in an AgNO3 solution and then, immersing the substrate into a second mixed solution to obtain a second conductive substrate, wherein the ingredients of the second mixed solution are PdCl2 and HCl; immersing the second conductive substrate into a third mixed solution to obtain a third conductive substrate, wherein the ingredients of the third mixed solution are Zn(NO3)2, dimethylamino borane and dye; and after drying the third conductive substrate, obtaining the zinc oxide absorption film. The preparation method does not need vacuum and high-temperature environment; the process is simple; the device is easily available and low in energy consumption; and the method is suitable for large-scale industrial production and can be widely applied to the field of a dye-sensitized solar cell.
Description
Technical field
The invention belongs to technical field of solar batteries, be specifically related to a kind of preparation method of zinc oxide absorbing membrane.
Background technology
Along with the develop rapidly of science and technology and the swift and violent increase of world population, global energy requirements amount is increasing year by year, and greatly developing solar cell will be solve one of of paramount importance approach of future world energy crisis.DSSC is as a kind of novel solar cell, and its abundant raw material source, with low cost, production technology are simple and energy consumption is low, has now become the focus of various countries' research.And zinc oxide is a kind of broad-band gap (3.3eV) semi-conducting material, it has, and good in optical property, electron mobility are high, abundance and the advantage such as thermal stability is good, are extremely suitable as the light anode of DSSC.
The zinc oxide absorbing membrane of traditional Zinc oxide-base DSSC first on electro-conductive glass, deposits one deck zinc oxide nanocrystalline film by the method such as hydro thermal method or sol-gel process, then the zinc-oxide film prepared is immersed in a few hours in dye solution, final drying gained.This preparation method's process is loaded down with trivial details, length consuming time and dyestuff are not easy to fully be adsorbed on zinc oxide nanocrystalline, make photo-generated carrier less, the short circuit current that result in DSSC is lower, and the photoelectric conversion efficiency of the solar cell of final gained is less.
Summary of the invention
The present invention is directed to prior art above shortcomings, propose a kind of preparation method of zinc oxide absorbing membrane.
To achieve these goals, present invention employs following technical scheme:
A preparation method for zinc oxide absorbing membrane, concrete steps are as follows:
(1) conductive substrates is placed in successively acetone, ethanol and deionized water and carries out ultrasonic cleaning, then use N
2dry up, obtain clean conductive substrates;
(2) at room temperature, clean conductive substrates immersed in the first mixed solution, obtain the first conductive substrates after then embathing in deionized water, composition and the concentration of described first mixed solution are as follows: 1 ~ 10g/l SnCl
2with 0.01 ~ 0.03mol/l HCl;
(3) at room temperature, the first conductive substrates is first immersed 1 ~ 5g/l AgNO
3in, then immerse in the second mixed solution, obtain the second conductive substrates after then embathing in deionized water, composition and the concentration of described second mixed solution are as follows: 0.1 ~ 0.5g/lPdCl
2with 0.01 ~ 0.03mol/l HCl;
(4) at constant temperature 60 ~ 80 DEG C, the second conductive substrates immersed in the 3rd mixed solution, after washed with de-ionized water, obtain the 3rd conductive substrates, composition and the concentration of described 3rd mixed solution are as follows: 0.01 ~ 0.1mol/l Zn (NO
3)
2, 0.01 ~ 0.1mol/l dimethylamino Borane solution and 10 ~ 200 μm of ol/l dyestuffs;
(5) the 3rd conductive substrates is first dry at 70 ~ 80 DEG C, drier at 120 ~ 150 DEG C, obtain described zinc oxide absorbing membrane.
In step (2), the clean conductive substrates time of immersing in the first mixed solution is 1 ~ 5min.
In step (3), the first conductive substrates first immerses AgNO
3in time be 1 ~ 3min, the time of immersing in the second mixed solution is 1 ~ 3min.
In step (4), the time that the second conductive substrates immerses in the 3rd mixed solution is 2 ~ 6h.
In step (5), the 3rd conductive substrates first time dry at 70 ~ 80 DEG C is 30 ~ 60min, and the time dry at 120 ~ 150 DEG C is 30 ~ 60min.
Described conductive substrates is ITO electro-conductive glass, FTO electro-conductive glass, Al paper tinsel or stainless steel foil.
Described dyestuff is rose-red, eosin W or W S, bromophenol blue, methylene blue, anthocyanidin, cumarin, N719, Z719 or N3.
Compared with prior art, the present invention has the following advantages:
(1) the present invention's dye sensitization zinc oxide absorbing membrane of adopting one-step method to prepare on conductive substrates, compared with customary preparation methods, eliminate the step of the independent sensitization of dyestuff, the sensitization of dyestuff is carried out while short and growth of zinc oxide nano consuming time is brilliant, most zinc oxide grain ambient absorption dyestuff can be made, improve the short-circuit current density of DSSC, thus greatly improve the photoelectric conversion efficiency of solar cell.
(2) preparation method of the present invention is without the need to the environment of vacuum and high temperature, and technique is simple, and equipment is easy to get and consumes energy low, is applicable to large-scale industrial production, can be widely used in field of dye-sensitized solar cells.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 is prepared and the electron scanning micrograph of the zinc oxide absorbing membrane obtained.
Fig. 2 is that embodiment 2 is prepared and the electron scanning micrograph of the zinc oxide absorbing membrane obtained.
Fig. 3 is the absorbance curve of the zinc oxide absorbing membrane that embodiment 1 and embodiment 2 are prepared and obtained.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
A preparation method for zinc oxide absorbing membrane, concrete steps are as follows:
The present embodiment for conductive substrates, take eosin W or W S as dyestuff with ITO electro-conductive glass,
(1) conductive substrates is placed in successively acetone, ethanol and deionized water and carries out ultrasonic cleaning, then use N
2dry up, obtain clean conductive substrates;
(2) at room temperature, clean conductive substrates immersed in the first mixed solution, obtain the first conductive substrates after then embathing in deionized water, composition and the concentration of described first mixed solution are as follows: 1g/l SnCl
2with 0.01mol/l HCl;
(3) at room temperature, the first conductive substrates is first immersed 1g/lAgNO
3in, then immerse in the second mixed solution, finally make the Pd particle of the flexible substrate adsorption q.s without conductivity, obtain the second conductive substrates after then embathing in deionized water, composition and the concentration of described second mixed solution are as follows: 0.1g/l PdCl
2with 0.01mol/l HCl;
(4) at constant temperature 60 DEG C, the second conductive substrates immersed in the 3rd mixed solution, after washed with de-ionized water, obtain the 3rd conductive substrates, composition and the concentration of described 3rd mixed solution are as follows: 0.01mol/l Zn (NO
3)
2, 0.01mol/l dimethylamino Borane solution and 10 μm of ol/l dyestuffs;
(5) the 3rd conductive substrates is first dry at 70 DEG C, drier at 120 DEG C, obtain described zinc oxide absorbing membrane.
In step (2), the clean conductive substrates time of immersing in the first mixed solution is 1min.
In step (3), the first conductive substrates first immerses AgNO
3in time be 1min, the time of immersing in the second mixed solution is 1min.
In step (4), the time that the second conductive substrates immerses in the 3rd mixed solution is 2h.
In step (5), the 3rd conductive substrates first time dry at 70 DEG C is 60min, and the time dry at 120 DEG C is 60min.
Embodiment 2
A preparation method for zinc oxide absorbing membrane, concrete steps are as follows:
The present embodiment for conductive substrates, is dyestuff with FTO electro-conductive glass with rose-red,
(1) conductive substrates is placed in successively acetone, ethanol and deionized water and carries out ultrasonic cleaning, then use N
2dry up, obtain clean conductive substrates;
(2) at room temperature, clean conductive substrates immersed in the first mixed solution, obtain the first conductive substrates after then embathing in deionized water, composition and the concentration of described first mixed solution are as follows: 10g/l SnCl
2with 0.03mol/l HCl;
(3) at room temperature, the first conductive substrates is first immersed 5g/l AgNO
3in, then immerse in the second mixed solution, obtain the second conductive substrates after then embathing in deionized water, composition and the concentration of described second mixed solution are as follows: 0.5g/l PdCl
2with 0.03mol/l HCl;
(4) at constant temperature 80 DEG C, the second conductive substrates immersed in the 3rd mixed solution, after washed with de-ionized water, obtain the 3rd conductive substrates, composition and the concentration of described 3rd mixed solution are as follows: 0.1mol/l Zn (NO
3)
2, 0.1mol/l dimethylamino Borane solution and 200 μm of ol/l dyestuffs;
(5) the 3rd conductive substrates is first dry at 80 DEG C, drier at 150 DEG C, obtain described zinc oxide absorbing membrane.
In step (2), the clean conductive substrates time of immersing in the first mixed solution is 5min.
In step (3), the first conductive substrates first immerses AgNO
3in time be 3min, the time of immersing in the second mixed solution is 3min.
In step (4), the time that the second conductive substrates immerses in the 3rd mixed solution is 6h.
In step (5), the 3rd conductive substrates first time dry at 80 DEG C is 30min, and the time dry at 150 DEG C is 60min.
Embodiment 3
A preparation method for zinc oxide absorbing membrane, concrete steps are as follows:
The present embodiment for conductive substrates, take bromophenol blue as dyestuff with stainless steel foil electro-conductive glass,
(1) conductive substrates is placed in successively acetone, ethanol and deionized water and carries out ultrasonic cleaning, then use N
2dry up, obtain clean conductive substrates;
(2) at room temperature, clean conductive substrates immersed in the first mixed solution, obtain the first conductive substrates after then embathing in deionized water, composition and the concentration of described first mixed solution are as follows: 5g/l SnCl
2with 0.02mol/l HCl;
(3) at room temperature, the first conductive substrates is first immersed 3g/l AgNO
3in, then immerse in the second mixed solution, obtain the second conductive substrates after then embathing in deionized water, composition and the concentration of described second mixed solution are as follows: 0.3g/l PdCl
2with 0.02mol/l HCl;
(4) at constant temperature 70 DEG C, the second conductive substrates immersed in the 3rd mixed solution, after washed with de-ionized water, obtain the 3rd conductive substrates, composition and the concentration of described 3rd mixed solution are as follows: 0.05mol/l Zn (NO
3)
2, 0.05mol/l dimethylamino Borane solution and 100 μm of ol/l dyestuffs;
(5) the 3rd conductive substrates is first dry at 75 DEG C, drier at 135 DEG C, obtain described zinc oxide absorbing membrane.
In step (2), the clean conductive substrates time of immersing in the first mixed solution is 2min.
In step (3), the first conductive substrates first immerses AgNO
3in time be 2min, the time of immersing in the second mixed solution is 2min.
In step (4), the time that the second conductive substrates immerses in the 3rd mixed solution is 4h.
In step (5), the 3rd conductive substrates first time dry at 75 DEG C is 45min, and the time dry at 135 DEG C is 45min.
Embodiment 4
A preparation method for zinc oxide absorbing membrane, concrete steps are as follows:
The present embodiment for conductive substrates, take methylene blue as dyestuff with Al paper tinsel electro-conductive glass,
(1) conductive substrates is placed in successively acetone, ethanol and deionized water and carries out ultrasonic cleaning, then use N
2dry up, obtain clean conductive substrates;
(2) at room temperature, clean conductive substrates immersed in the first mixed solution, obtain the first conductive substrates after then embathing in deionized water, composition and the concentration of described first mixed solution are as follows: 8g/l SnCl
2with 0.015mol/l HCl;
(3) at room temperature, the first conductive substrates is first immersed 2g/l AgNO
3in, then immerse in the second mixed solution, obtain the second conductive substrates after then embathing in deionized water, composition and the concentration of described second mixed solution are as follows: 0.4g/l PdCl
2with 0.025mol/l HCl;
(4) at constant temperature 75 DEG C, the second conductive substrates immersed in the 3rd mixed solution, after washed with de-ionized water, obtain the 3rd conductive substrates, composition and the concentration of described 3rd mixed solution are as follows: 0.08mol/l Zn (NO
3)
2, 0.03mol/l dimethylamino Borane solution and 150 μm of ol/l dyestuffs;
(5) the 3rd conductive substrates is first dry at 75 DEG C, drier at 130 DEG C, obtain described zinc oxide absorbing membrane.
In step (2), the clean conductive substrates time of immersing in the first mixed solution is 3min.
In step (3), the first conductive substrates first immerses AgNO
3in time be 2.5min, the time of immersing in the second mixed solution is 2.5min.
In step (4), the time that the second conductive substrates immerses in the 3rd mixed solution is 3h.
In step (5), the 3rd conductive substrates first time dry at 75 DEG C is 45min, and the time dry at 130 DEG C is 45min.
Except the dyestuff that embodiment 1 ~ 4 uses, anthocyanidin, cumarin, N719, Z719 or N3 are the preferred coloring agent preparing zinc oxide absorbing membrane.
Claims (7)
1. a preparation method for zinc oxide absorbing membrane, is characterized in that, concrete steps are as follows:
(1) conductive substrates is placed in successively acetone, ethanol and deionized water and carries out ultrasonic cleaning, then use N
2dry up, obtain clean conductive substrates;
(2) at room temperature, clean conductive substrates immersed in the first mixed solution, obtain the first conductive substrates after then embathing in deionized water, composition and the concentration of described first mixed solution are as follows: 1 ~ 10g/l SnCl
2with 0.01 ~ 0.03mol/l HCl;
(3) at room temperature, the first conductive substrates is first immersed 1 ~ 5g/l AgNO
3in solution, then immerse in the second mixed solution, obtain the second conductive substrates after then embathing in deionized water, composition and the concentration of described second mixed solution are as follows: 0.1 ~ 0.5g/l PdCl
2with 0.01 ~ 0.03mol/l HCl;
(4) at constant temperature 60 ~ 80 DEG C, the second conductive substrates immersed in the 3rd mixed solution, after washed with de-ionized water, obtain the 3rd conductive substrates, composition and the concentration of described 3rd mixed solution are as follows: 0.01 ~ 0.1mol/l Zn (NO
3)
2, 0.01 ~ 0.1mol/l dimethylamino borine and 10 ~ 200 μm of ol/l dyestuffs;
(5) the 3rd conductive substrates is first dry at 70 ~ 80 DEG C, drier at 120 ~ 150 DEG C, obtain described zinc oxide absorbing membrane.
2. the preparation method of zinc oxide absorbing membrane as claimed in claim 1, it is characterized in that, in step (2), the clean conductive substrates time of immersing in the first mixed solution is 1 ~ 5min.
3. the preparation method of zinc oxide absorbing membrane as claimed in claim 1, it is characterized in that, in step (3), the first conductive substrates first immerses AgNO
3time in solution is 1 ~ 3min, and the time of immersing in the second mixed solution is 1 ~ 3min.
4. the preparation method of zinc oxide absorbing membrane as claimed in claim 1, is characterized in that, in step (4), the time that the second conductive substrates immerses in the 3rd mixed solution is 2 ~ 6h.
5. the preparation method of zinc oxide absorbing membrane as claimed in claim 1, is characterized in that, in step (5), the 3rd conductive substrates first time dry at 70 ~ 80 DEG C is 30 ~ 60min, and the time dry at 120 ~ 150 DEG C is 30 ~ 60min.
6. the preparation method of zinc oxide absorbing membrane as claimed in any one of claims 1 to 5, wherein, it is characterized in that, described conductive substrates is ITO electro-conductive glass, FTO electro-conductive glass, Al paper tinsel or stainless steel foil.
7. the preparation method of as claimed in any one of claims 1 to 5, wherein zinc oxide absorbing membrane, is characterized in that, described dyestuff is rose-red, eosin W or W S, bromophenol blue, methylene blue, anthocyanidin, cumarin, N719, Z719 or N3.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005353588A (en) * | 2004-06-09 | 2005-12-22 | Korea Electronics Telecommun | Flexible dye sensitized solar cell including conductive metal substrate |
| EP1801909A1 (en) * | 2004-10-15 | 2007-06-27 | Bridgestone Corporation | Dye sensitized metal oxide semiconductor electrode and method for manufacturing the same, and dye sensitized solar cell |
| CN104498916A (en) * | 2014-11-24 | 2015-04-08 | 广西大学 | Method used for preparing aluminium-doped zinc oxide thin film via electroless deposition |
-
2015
- 2015-07-13 CN CN201510407915.9A patent/CN104992838B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005353588A (en) * | 2004-06-09 | 2005-12-22 | Korea Electronics Telecommun | Flexible dye sensitized solar cell including conductive metal substrate |
| EP1801909A1 (en) * | 2004-10-15 | 2007-06-27 | Bridgestone Corporation | Dye sensitized metal oxide semiconductor electrode and method for manufacturing the same, and dye sensitized solar cell |
| CN104498916A (en) * | 2014-11-24 | 2015-04-08 | 广西大学 | Method used for preparing aluminium-doped zinc oxide thin film via electroless deposition |
Non-Patent Citations (2)
| Title |
|---|
| SUMAN KUSHWAHA ETC: "Studies of structural and morphological characteristics of flower-like ZnO thin film and its application as photovoltaic material", 《OPTIK》 * |
| 杨静: "金属氧化物半导体纳米材料的制备与性能研究", 《北京化工大学 硕士学位论文》 * |
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