CN104701019A - Preparation method of composite counter electrode for quantum dot-sensitized solar cell - Google Patents
Preparation method of composite counter electrode for quantum dot-sensitized solar cell Download PDFInfo
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Abstract
The invention belongs to the technical field of solar cells and particularly discloses a preparation method of composite counter electrode for a quantum dot-sensitized solar cell. The composite counter electrode comprises multi-walled carbon nano-tubes, a metal sulfide and a conductive substrate. During preparation, a layer of multi-walled carbon nano-tubes deposits on the conductive substrate by means of an electrophoresis method, the metal sulfide synthesized in a liquid phase mode deposits on the multi-walled carbon nano-tubes by means of the electrophoresis method to prepare the composite counter electrode, and a photo-anode and electrolyte form the quantum dot-sensitized solar cell. The preparation method has the advantages that operation is simple, special devices and solvents are not needed, cost is low, the photoelectric converting efficiency and stability of the quantum dot-sensitized solar cell are improved, and the method is suitable for manufacture of various quantum dot-sensitized solar cells.
Description
Technical field
The invention belongs to area of solar cell, further belong to the technical field to electrode in solar cell, be specifically related to a kind of preparation method of the metal sulfide combined counter electrode for quantum dot sensitized solar cell.
Background technology
Along with the continuous consumption of fossil energy and the day by day serious of the environmental problem that causes thereof, add the sustainable growth of the mankind to energy demand, research solar cell is significant, imperative.
DSSC is considered to the solar cell of new generation having prospect, and compared with DSSC, quantum dot sensitized solar cell has higher theoretical conversion efficiency.Relative dye sensitizing agent, quantum dot sensitizer has many advantages, and as higher extinction coefficient, energy gap is adjustable, and has the potential of many exciton effects.Therefore, quantum dot sensitized solar cell gets more and more people's extensive concerning in recent years.
For quantum dot sensitized solar cell, noble metal (platinum, gold), carbon, metal sulfide three major types are mainly contained to electrode material.Wherein the noble metal such as platinum, gold is to electrode catalyst activity is not high and cost is higher.Carbon is cheap but catalytic activity is not best to electrode.Metal sulfide because cost is lower to electrode, has excellent catalytic performance and is expected.At present, the preparation of metal sulfide to electrode mainly contains and utilizes sheet metal etch, hot vapour deposition method on electro-conductive glass, the ion layer adsorption of original position and reaction method on electro-conductive glass.It is unstable to electrode that sheet metal etch obtains, and hot vapour deposition method is strict to equipment requirement, and the ion layer adsorption of original position and reaction method are difficult to obtain uniform sulfide film in smooth substrate of glass.Therefore, in this technical field, need a kind of metal sulfide that improves to the preparation of the electrode also further method to electrode improving the catalytic effect of metal sulfide.
Summary of the invention
The object of the invention is to overcome the defect existed in prior art, a kind of low cost is provided, and effectively can improve the preparation method of the electricity conversion of quantum dot sensitization solar battery and the metal sulfide combined counter electrode of stability.This is to deposit one deck multi-walled carbon nano-tubes with electrophoresis in conductive substrates to the feature of electrode, again the metal sulfide electrophoresis of liquid phase synthesis is deposited in above-mentioned multi-wall carbon nano-tube tube layer, improve photoelectric conversion efficiency and the stability of quantum dot sensitized solar cell.
In order to realize object of the present invention, the technical scheme of employing is:
For the preparation method of the combined counter electrode of quantum dot sensitized solar cell, it is characterized in that, comprise the following steps:
(1) dispersion of carboxylated multi-walled carbon nano-tubes is made into suspension in organic solvent;
(2) with electrophoresis, multi-walled carbon nano-tubes is deposited in conductive substrates;
(3) metal sulfide of liquid phase synthesis is separated from synthetic, dry;
(4) by dried metal sulfide dispersion in organic solvent;
(5) with electrophoresis, metal sulfide is deposited in the conductive substrates of multi-walled carbon nano-tubes;
(6) combined counter electrode is heat-treated.
Preferably, disperse the organic solvent of described multi-walled carbon nano-tubes to be toluene or chloroform, and the concentration of multi-walled carbon nano-tubes is 0.5-6mg/ml.
Preferably, described metal sulfide is Cu
xany one in S (x=1-2), CoS, PbS or NiS, and described metal sulfide liquid phase synthesis in water-soluble or oil-soluble solvent.
Preferably, described metal sulfide synthesizes in water miscible solvent, and is added with the oleyl amine of the promotion dispersion of 2-5mg/ml in described water miscible solvent.
Preferably, what the electrophoretic deposition of described multi-walled carbon nano-tubes adopted is constant voltage method, and voltage is 100-120V, and sedimentation time is 3-5min.
Preferably, described conductive substrates is any one in electro-conductive glass, stainless steel substrates, metal titanium sheet or conductive plastic film.
Preferably, the concentration of described metal sulfide is 0.2-3mg/ml, and disperses the organic solvent of described metal sulfide to be volume ratio to be the chloroform of 3:2-3:4.5 and the mixed solvent of acetonitrile or volume ratio to be the toluene of 3:2-3:4.5 and the mixed solvent of acetonitrile.
Preferably, what the electrophoretic deposition of described metal sulfide adopted is constant voltage method, and voltage is 40-60V, and sedimentation time is 10-30s.
Preferably, the heat treatment temperature of described combined counter electrode is no more than 150 DEG C.
The beneficial effect that the present invention has:
(1) simple to operate, the above-mentioned metal sulfide that is suitable for all liquid phase synthesis of the present invention, and the pattern of metal sulfide and size adjustable, do not need special installation and solvent; Simple to operate, cost is low.
(2) according to method of the present invention, the continuous dense uniform of structure of the combined counter electrode film obtained, between adjacent layer, adhesion is strong.
(3) the present invention is applicable to different conductive substrates, can comprise glass, the conductive substrates that metal, plastics etc. are different obtains uniform to electrode film, and does not need high temperature processing step.
(4) the present invention first utilizes electrophoresis to deposit multi-walled carbon nano-tubes, again metal sulfide is deposited on multi-walled carbon nano-tubes, owing to introducing multi-walled carbon nano-tubes, to the catalytic activity of electrode, electric conductivity and electrochemical stability performance improve, and then improve electricity conversion and the stability of quantum dot sensitized solar cell.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention for quantum dot sensitized solar cell metal sulfide combined counter electrode;
Wherein, 1-metal sulfide, 2-multi-walled carbon nano-tubes, 3-conductive substrates;
Fig. 2 is the picture of metal sulfide combined counter electrode prepared by the present invention;
Fig. 3 is the photoelectric current-photovoltage curve of the quantum dot sensitized solar cell adopting metal sulfide combined counter electrode of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not only confined to embodiment.
Experimental group 1
(1) multi-walled carbon nano-tubes carboxylated for 0.04g is dispersed in 20ml toluene, ultrasonic 5min.
(2) two panels is mixed the SnO of F
2electro-conductive glass (FTO) immerses in the suspension of above-mentioned multi-walled carbon nano-tubes, and at a distance of 0.5cm, adopt constant voltage 120V to deposit 3min, multi-walled carbon nano-tubes is deposited on FTO, and negative electrode obtains MWCNT/FTO.
(3) under agitation the aqueous solution of 0.04M thioacetamide is added drop-wise in the aqueous solution of 0.04M copper acetate, stirring at room temperature 10min, centrifugally obtains metallic copper sulfide precipitation, ethanol washing post-drying.
(4) 0.02g metallic copper sulfide is dispersed in the mixed solvent (V chloroform/V acetonitrile=1:1.5) of 20ml chloroform and acetonitrile, adds 2-5 oil dripping amine (0.04-0.10g), ultrasonic 5min.
(5) FTO is connected negative pole, MWCNT/FTO connects positive pole, immerses in the suspension of metallic copper sulfide, and at a distance of 0.5cm, adopt constant voltage 40V to deposit 30s, metallic copper deposition of sulfides, on MWCNT/FTO, obtains Cu
xs/MWCNT/FTO combined counter electrode.
(6) combined counter electrode is heated 10min at 100 DEG C.
Change the concentration of multi-walled carbon nano-tubes or metallic copper sulfide, dispersion solvent, the voltage of electrophoretic deposition and time, keep other steps and parameter constant, prepare a series of combined counter electrode, obtained combined counter electrode is assembled into quantum dot sensitized solar cell and carries out photoelectric conversion efficiency test, wherein light anode is the nano titanium dioxide porous film adopting silk screen print method to prepare.Quantum dot sensitizer is CdS/CdSe prepared by SILAR method (SILAR), and concrete grammar can refer to the method that document " Y.L.Lee, Y.S.Lo, Adv.Funct.Mater.2009,19,604-609 " provides, and seldom repeats at this.Electrolyte is the solution (V of 2M vulcanized sodium and 2M elemental sulfur
methyl alcohol/ V
water=7:3).Battery is numbered 1-12, and respectively as embodiments of the invention 1-embodiment 12, test result is as shown in table 1.As seen from Table 1, higher cell conversion efficiency can be obtained under the Parameter Conditions of battery numbering 8.
Table 1 is based on the Cu of different preparation condition
xthe efficiency of the quantum dot sensitized solar cell of S/MWCNT/FTO combined counter electrode
Experimental group 2
Select the Parameter Conditions of battery numbering 8, with reference to experimental group 1, the copper acetate in step (3) is changed to lead acetate respectively, cobalt acetate and nickel acetate, keep other steps and parameter constant, respectively obtained PbS/MWCNT/FTO, CoS/MWCNT/FTO, NiS/MWCNT/FTO combined counter electrode.
For comparing, empirically organize 1, step (1) and (2) prepare multi-walled carbon nano-tubes to electrode MWCNT/FTO; With reference to experimental group 1, metal sulfide is prepared to electrode Cu in step (3)-(5)
xs/FTO, PbS/FTO, CoS/FTO and NiS/FTO, just use FTO by the both positive and negative polarity in (5).
Become quantum dot sensitized solar cell to carry out photoelectric conversion efficiency test to electrode assembling obtained for experimental group 2, battery is numbered 13-20, and as embodiments of the invention 13-embodiment 20, test result is as shown in table 2.As seen from Table 2, metal sulfide combined counter electrode than single multi-walled carbon nano-tubes to electrode and single metal sulfide obviously good to the catalytic activity of electrode, this is because multi-walled carbon nano-tubes has very large specific area, good electron conductivity, stable chemical property and higher catalytic activity, make the catalytic performance of combined counter electrode be significantly improved.Wherein at Cu
xs/MWCNT/FTO combined counter electrode can obtain higher cell conversion efficiency.
Table 2 is based on different metal sulfide combined counter electrode, and multi-walled carbon nano-tubes is to electrode, and metal sulfide is to the efficiency of the quantum dot sensitized solar cell of electrode
| Battery is numbered | Electrode is formed | Electricity conversion (%) |
| 8 | Cu xS/MWCNT/FTO | 4.00 |
| 13 | PbS/MWCNT/FTO | 3.82 |
| 14 | CoS/MWCNT/FTO | 3.78 |
| 15 | NiS/MWCNT/FTO | 3.24 |
| 16 | MWCNT/FTO | 1.76 |
| 17 | Cu xS/FTO | 3.35 |
| 18 | PbS/FTO | 3.21 |
| 19 | CoS/FTO | 3.10 |
| 20 | NiS/FTO | 2.74 |
Experimental group 3
With reference to experimental group 1, select the Parameter Conditions of battery numbering 8, keep other steps and parameter constant, just conductive substrates is changed respectively into the In mixing Sn
2o
3electro-conductive glass (ITO), stainless steel substrates, metal Ti sheet, obtained Cu
xs/MWCNT/ITO, Cu
xs/MWCNT/ stainless steel, Cu
xs/MWCNT/Ti combined counter electrode, become quantum dot sensitized solar cell to carry out photoelectric conversion efficiency test to electrode assembling obtained for embodiment 3, battery is numbered 21-23, as embodiments of the invention 21-embodiment 23, contrast with embodiment 8, test result is as shown in table 3.
Table 3 is based on Cu
xthe efficiency of the quantum dot sensitized solar cell of the combined counter electrode of the different conductive substrates of S/MWCNT/.、
| Battery is numbered | Conductive substrates | Electricity conversion (%) |
| 8 | FTO | 4.00 |
| 21 | ITO | 4.12 |
| 22 | Ti sheet | 4.54 |
| 23 | Stainless steel substrates | 4.31 |
Experimental group 4
With reference to experimental group 1, select the Parameter Conditions of battery numbering 8, adopt the metallic copper sulfide of water-soluble solvent and oil-dissolving solvent synthesis to prepare Cu respectively
xs/MWCNT/FTO is to electrode.In water-soluble solvent, the method for synthetic metals copper sulfide is with reference to the step (3) of experimental group 1, has just changed water into ethylene glycol; The concrete grammar of synthetic metals copper sulfide can the method that provides of list of references " Zhang Yiqiang, Zhang Hui etc., Materials Science and Engineering journal, 2008,26 (2), 208-212 " in oil-dissolving solvent (oleyl amine), seldom repeats at this.The metal sulfide just synthesized in oil-dissolving solvent does not add oleyl amine in step (4), keep other steps and parameter constant, be assembled into quantum dot sensitized solar cell and carry out photoelectric conversion efficiency test, battery is numbered 24-25, as embodiments of the invention 24-embodiment 25, test result is in table 4.
The Cu that table 4 is prepared based on the metallic copper sulfide of different synthetic
xthe efficiency of the quantum dot sensitized solar cell of S/MWCNT/FTO combined counter electrode
| Battery is numbered | The solvent of synthetic metals sulfide | Electricity conversion (%) |
| 8 | Water | 4.00 |
| 24 | Ethylene glycol (water-soluble) | 3.96 |
| 25 | Oleyl amine (oil-soluble) | 3.88 |
Embodiment 5
With reference to experimental group 1, the Parameter Conditions of battery numbering 8 is selected to prepare Cu
xs/MWCNT/FTO combined counter electrode, then prepares CuInS respectively
2, CdS quantum dot sensitization light anode, wherein CuInS
2the concrete grammar of quantum dot sensitized smooth anode can refer to document " J.Y.Chang, L.F.Su, etc, Chem.Commun., 2012,48,4848-4850 ", seldom repeats at this.The concrete grammar of CdS quantum dot sensitization light anode can refer to document " C.H.Chang, Y.L.Lee, Appl.Phys.Lett.2007,91,053503 ", seldom repeats at this.Keep other steps and parameter constant, with Cu
xs/MWCNT/FTO combined counter electrode is assembled into quantum dot sensitized solar cell and carries out photoelectric conversion efficiency test, and battery is numbered 26-27, and as embodiments of the invention 26-embodiment 27, test result is in table 5.
Table 5 is based on the efficiency of the quantum dot sensitized solar cell of different quantum dot type
| Battery is numbered | Quantum dot type | Electricity conversion (%) |
| 8 | CdS/CdSe | 4.00 |
| 26 | CuInS 2 | 2.24 |
| 27 | CdS | 2.65 |
Composition graphs 1-Fig. 3 is known, the metal sulfide combined counter electrode for quantum dot sensitized solar cell prepared by the inventive method, the metal sulfide that its catalytic activity is obviously better than generally using at present is to electrode, owing to introducing multi-walled carbon nano-tubes, the catalytic activity of electrode, electronic transmission performance and electrochemical stability improve, and then improve electricity conversion and the stability of quantum dot sensitized solar cell.
Last it is noted that to those skilled in the art, should be appreciated that, the metal sulfide combined counter electrode prepared in the present invention except can with except the nano-size titania porous membrane light anode composition solar cell on FTO glass, can also and other conductive substrates on the titanium dioxide of other patterns and the porous membrane light anode assembling solar cell such as the zinc oxide of various pattern.
Further, above embodiment only in order to the present invention is described and and unrestricted technical scheme described in the invention; Therefore, although this specification with reference to each above-mentioned embodiment to present invention has been detailed description, those of ordinary skill in the art should be appreciated that and still can modify to the present invention or equivalent to replace; And all do not depart from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in right of the present invention.
Claims (9)
1. for the preparation method of the combined counter electrode of quantum dot sensitized solar cell, it is characterized in that, comprise the following steps:
(1) dispersion of carboxylated multi-walled carbon nano-tubes is made into suspension in organic solvent;
(2) with electrophoresis, multi-walled carbon nano-tubes is deposited in conductive substrates;
(3) metal sulfide of liquid phase synthesis is separated from synthetic, dry;
(4) by dried metal sulfide dispersion in organic solvent;
(5) with electrophoresis, metal sulfide is deposited in the conductive substrates of multi-walled carbon nano-tubes;
(6) combined counter electrode is heat-treated.
2. preparation method according to claim 1, is characterized in that, disperse the organic solvent of described multi-walled carbon nano-tubes to be toluene or chloroform, and the concentration of multi-walled carbon nano-tubes is 0.5-6mg/ml.
3. preparation method according to claim 1, it is characterized in that, described metal sulfide is any one in CuxS (x=1-2), CoS, PbS or NiS, and described metal sulfide liquid phase synthesis in water-soluble or oil-soluble solvent.
4. preparation method according to claim 3, is characterized in that, described metal sulfide synthesizes in water miscible solvent, and is added with the oleyl amine of the promotion dispersion of 2-5mg/ml in described water miscible solvent.
5. preparation method according to claim 1, is characterized in that, what the electrophoretic deposition of described multi-walled carbon nano-tubes adopted is constant voltage method, and voltage is 100-120V, and sedimentation time is 3-5min.
6. preparation method according to claim 1, is characterized in that, described conductive substrates is any one in electro-conductive glass, stainless steel substrates, metal titanium sheet or conductive plastic film.
7. preparation method according to claim 1, it is characterized in that, the concentration of described metal sulfide is 0.2-3mg/ml, and disperses the organic solvent of described metal sulfide to be volume ratio to be the chloroform of 3:2-3:4.5 and the mixed solvent of acetonitrile or volume ratio to be the toluene of 3:2-3:4.5 and the mixed solvent of acetonitrile.
8. preparation method according to claim 1, is characterized in that, what the electrophoretic deposition of described metal sulfide adopted is constant voltage method, and voltage is 40-60V, and sedimentation time is 10-30s.
9. preparation method according to claim 1, is characterized in that, the heat treatment temperature of described combined counter electrode is no more than 150 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107633951A (en) * | 2017-09-26 | 2018-01-26 | 哈尔滨工业大学 | A kind of method and its application that homogeneity barrier layer/skeleton structure is prepared using titanium tetrachloride hydrolysis |
| CN107785173A (en) * | 2016-08-30 | 2018-03-09 | 东北师范大学 | It is a kind of be applied to low light condition under quantum dot sensitized solar cell to electrode material and preparation method thereof |
| CN109950052A (en) * | 2019-03-22 | 2019-06-28 | 北京石油化工学院 | A kind of preparation method of supercapacitor |
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| CN102522219A (en) * | 2011-12-15 | 2012-06-27 | 东南大学 | Quantum dot sensitized solar cell and preparation method thereof |
Non-Patent Citations (2)
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| YAOMING XIAO等: ""Pulse electrodeposition of CoS on MWCNT/Ti as a high performance counter electrode for a Pt-free dye-sensitized solar cell"", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107785173A (en) * | 2016-08-30 | 2018-03-09 | 东北师范大学 | It is a kind of be applied to low light condition under quantum dot sensitized solar cell to electrode material and preparation method thereof |
| CN107633951A (en) * | 2017-09-26 | 2018-01-26 | 哈尔滨工业大学 | A kind of method and its application that homogeneity barrier layer/skeleton structure is prepared using titanium tetrachloride hydrolysis |
| CN107633951B (en) * | 2017-09-26 | 2019-02-19 | 哈尔滨工业大学 | It is a kind of to prepare homogeneity barrier layer/skeleton structure method and its application using titanium tetrachloride hydrolysis |
| CN109950052A (en) * | 2019-03-22 | 2019-06-28 | 北京石油化工学院 | A kind of preparation method of supercapacitor |
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