CN104332315A - Preparation method of porous nanocrystalline Cu2S counter electrode of quantum-dot-sensitized solar cell - Google Patents
Preparation method of porous nanocrystalline Cu2S counter electrode of quantum-dot-sensitized solar cell Download PDFInfo
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Abstract
The invention belongs to the technical field of solar cells and energies, and particularly relates to a preparation method of a porous nanocrystalline Cu2S counter electrode of a quantum-dot-sensitized solar cell. The preparation method comprises the steps of: regarding copper acetate and thioacetamide as precursors; obtaining 20-100 nm cuprous sulfide (Cu2S) nanometer particles through solvothermal reaction; preparing the cuprous sulfide (Cu2S) nanometer particles and ethanol into a thick liquid; forming 5-10 microns Cu2S nanocrystalline porous film on a conductive base body by utilizing a knife coating method, a silk screen print method or a spin-coating method; sintering at 300-500 DEG C in an inert atmosphere or vacuum for 10-60 min to obtain a battery electrode. The prepared Cu2S nanometer porous counter electrode extremely increases contact area of the counter electrode and electrolyte, further increases catalytic reaction site of the Cu2S and the electrolyte, and improves performance of the solar cell. In addition, the preparation method of the porous nanocrystalline Cu2S counter electrode of the quantum-dot-sensitized solar cell is simple in preparation technology, relatively low in cost and has wide application foreground and wide research values.
Description
Technical field
The present invention relates to technical field of solar batteries, describe a kind of Cu for quantum dot sensitized solar cell
2s porous nanocrystalline is to the preparation method of electrode.
Background technology
Along with the exhaustion day by day of non-renewable energy resources, continuing to increase of energy resource consumption, energy problem has become the serious challenge of whole mankind's survival and development.Find and effectively utilize new forms of energy to be key subjects that the mankind enter that 21 century must solve.Solar energy, as a kind of clean, inexhaustible energy, is a kind of selection well.The crystal silicon solar energy battery technology of current extensive use is full-fledged, obtains the energy conversion efficiency more than 20%, but its cost is higher, limits its popularization.As the quantum dot sensitized solar cell of third generation solar cell, because quantum dot has unique quantum confined effect and many excitons excite effect, make the theoretical conversion efficiencies of quantum dot sensitized solar cell up to 44%.Along with development and the trend maturation of nanometer technology, the performance of quantum dot sensitized solar cell is improved rapidly, considers cost comparatively cheap compared with crystal silicon solar energy battery in addition, makes it have good development prospect.
Quantum dot sensitized solar cell is layer structure, inwardly also has nanocrystalline porous semiconductive thin film successively and be adsorbed in quantum dot sensitizer semiconductive thin film, electrolyte and to a few parts such as electrodes from outer field transparent conducting glass.This solar cell is derived by organic dye sensitized solar cell, adopts the quantum dot of low energy gap width to replace the sensitizer of organic dye molecule as electron excitation with it unlike quantum dot sensitized solar cell.Compared with organic dyestuff, quantum dot not only has many excitons excite effect, but also has other advantage: (1) spectral absorption is wider, and its band gap can regulate according to its size; (2) there is the extinction coefficient larger than organic dye molecule and photochemical stability; (3) there is large natural dipole moment, be beneficial to the separation of excitation state electron-hole.Battery operated principle: under the effect of incident photon, electronics in quantum dot transits to conduction band from valence band, the electronics of excitation state is injected in light anode conduction band fast, enrichment is also flowed to electrode by external circuit, ion generation redox reaction in the hole stayed in quantum dot and electrolyte, forms whole loop.
In quantum dot sensitized battery, transferring charge is played to electrode, the effect of closed-loop path, vital effect is played to conversion efficiency of solar cell.To sensitization solar battery, adopt very high metal platinum (Pt) electrode of catalytic activity as to electrode.But in quantum dot sensitized solar cell, electrolyte is for being many sulfur systems, and in many sulphur electrolyte, the catalytic performance of Pt is lower, limits the raising of battery performance.1980, (the HodesG such as Hodes, ManassenJ, CahenD.J.J.Am.Chem.Soc., 1980,127 (3): 544-549) proposing CoS, NiS, Cu2S, PbS is used as to application of electrode in the catalysis of many sulphur electrolyte system, finds that battery open circuit voltage and short circuit current are all significantly improved, and illustrates that they have excellent catalytic performance to many sulphur redox couple.In addition, Graphene is as development in recent years material system more fast, studied more.But single employing Graphene cannot obtain good catalytic performance, must Material cladding good with catalytic activity.2011, Radich etc. (RadichJ.G, DwyerR., KamatP.V, J.Phys.Chem.Lett., 2011,2 (19): 2453-2460) were by Cu
2s and graphene oxide compound in the quantum dot sensitized battery of CdS/CdSe, obtain the quantum dot sensitized solar cell of the transformation efficiency of 4.4% and the fill factor, curve factor of 75% as being used for electrode.In the same year, a kind of method that Meng Qing ripple seminar (Chinese invention patent 201110052121.7) proposes electrochemical deposition prepares sulfide to electrode.2012, Yang etc. (Yueyong Yang, Lifeng Zhu, Huicheng Sun, Xiaoming Huang.ACSAppl.Mater.Interfaces2012,4,6162-6168) made TiO to be similar to
2the method of slurry is prepared PbS/ carbon black (carbonblack, CB) slurry and is then coated on FTO glass, dries, makes PbS/CB to electrode, obtain the quantum dot sensitized solar cell that conversion efficiency is 3.91%.2013, Kalanur etc. (Shankara Sharanappa Kalanur, Sang Youn Chae, Oh Shim Joo.Electrochimica Acta103 (2013) 91 – 95) the thin layer Cu that utilized hydro thermal method to prepare
1.8s/CuS is attached on FTO glass, as CdS sensitization TiO
2nano-crystalline solar battery to electrode, obtain the transformation efficiency of 1.66%.
Comprehensive said method, Cu
2s has good catalytic activity, be suitable for preparing quantum dot sensitization solar battery to electrode, usually adopt Cu prepared by Copper Foil
2s is fine and close stratotype to electrode surface, and specific area is little, and therefore catalytic site is on the low side, limits the raising of battery performance.Cu
2s and the combined counter electrode such as Graphene, carbon black, can exist in conjunction with defective tightness between particle and particle, between particle and conducting base, the shortcomings such as loss of charge is larger.For addressing these problems, needing to prepare that a kind of stability is good, catalytic performance is high, specific area is large to electrode material.
Summary of the invention
The object of this invention is to provide a kind of quantum dot sensitized solar cell porous nanocrystalline Cu2S to the preparation method of electrode, Cu prepared by the present invention
2s nanoporous, to electrode, greatly adds the contact area to electrode and electrolyte, and then adds Cu
2the catalytic reaction site of S and electrolyte, improves the performance of solar cell.In addition, preparation technology of the present invention is simple, and cost is lower, is with a wide range of applications and researching value.
The method with copper acetate and thioacetamide for presoma, cuprous sulfide (Cu2S) nano particle of size 20 ~ 100 nanometer is obtained by solvent thermal reaction, and be configured to slurry with ethanol, utilize knife coating, silk screen print method or spin-coating method to form the nanocrystalline porous film of Cu2S of 5 ~ 10 microns at conducting base, in inert atmosphere or vacuum, sinter 10 ~ 60 minutes at 300 ~ 500 DEG C obtain battery electrode.Concrete steps are as follows:
A) conductive substrates is used successively deionized water, absolute ethyl alcohol difference ultrasonic cleaning 5 ~ 15 minutes, then dry;
B) by copper acetate, thioacetamide is dissolved in diglycol respectively, be configured to the thioacetyl amine aqueous solution of copper acetate solution that concentration is 0.02 ~ 0.04 molar concentration and 0.03 ~ 0.05 molar concentration, two kinds of solution mix according to volume ratio 1:1, then react 2 ~ 3 hours under 160 ~ 180 DEG C of oil bath conditions, centrifugal, washing, dry, obtain the Cu of 20 ~ 100 nanometers
2s particle;
C) by Cu
2s particle and ethanol prepare slurry by 2:1 ~ 1:2 mass ratio;
D) adopt knife coating, silk screen print method or spin-coating method to be evenly coated in conductive substrates by above-mentioned slurry, then in protective atmosphere or vacuum, sinter 30 ~ 60 minutes at 350 ~ 450 DEG C, obtain electrode film.
Conductive substrates of the present invention is mix the tin dioxide thin film glass (FTO) of F, mix the indium oxide (ITO) of Sn, Copper Foil or aluminium foil.
The advantage of the inventive method
1, the present invention is porous nanocrystalline film, Cu
2the specific area of S to electrode is large, and then the contact-making surface added electrode and electrolyte, active site increases, thus collects more electronics, impel electronics to be reduced into reducing substances by high efficiency for the oxidizing substance in electrolyte, promote the reducing/regenerating of quantum dot.
2, formed the porous nanocrystalline film be interconnected by sintering, solve the shortcoming of general compound powder film poor connectivity, thus improve electric transmission efficiency, and reduce electron recombination loss.
3, the porous nanocrystalline film performance prepared of the present invention is stable, technique is simple, cost is low, can suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the Cu of preparation
2the electron scanning micrograph of S nano particle;
Fig. 2 is Cu after knifing sintering
2the electron scanning micrograph of S porous nanocrystalline film surface;
Fig. 3 is Cu after knifing sintering
2the electron scanning micrograph of S porous nanocrystalline film cross section;
Fig. 4 is the Cu prepared with the present invention
2s porous nanocrystalline film is to the current-voltage characteristic curve figure of the quantum dot sensitized solar cell that electrode assembling becomes.
Embodiment 1
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 15 minutes, then dry; By 0.03 molar concentration copper acetate, 0.04 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 170 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2.5 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:1 mass ratio; Adopt knife coating to be evenly coated on FTO electro-conductive glass by above-mentioned slurry, then in argon gas atmosphere, sinter 40min at 400 DEG C, namely obtain Cu
2s porous nanocrystalline is to electrode.
By the Cu prepared
2s porous nanocrystalline becomes quantum dot sensitized battery to carry out battery performance test to electrode assembling, what wherein light anode adopted is the standby nano-titanium oxide porous membrane of knifing legal system, and quantum dot sensitizer is the cadmium sulfide and CdSe quantum dots that adopt SILAR method and chemical bath deposition method to prepare.Electrolyte is the aqueous solution of 1 molar concentration vulcanized sodium and 1 molar concentration elemental sulfur.Experimental result asks for an interview table 1.
Embodiment 2
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 5 minutes, then dry; By 0.04 molar concentration copper acetate, 0.05 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 180 DEG C of oil bath conditions by two kinds of solution hybrid reactions 3 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:2 mass ratio; Adopt knife coating to be evenly coated on FTO electro-conductive glass by above-mentioned slurry, then in argon gas atmosphere, sinter 60 minutes at 450 DEG C, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
Embodiment 3
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 10 minutes, then dry; By 0.02 molar concentration copper acetate, 0.03 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 160 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 2:1 mass ratio; Adopt knife coating to be evenly coated on FTO electro-conductive glass by above-mentioned slurry, then in argon gas atmosphere, sinter 30 minutes at 350 DEG C, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
Embodiment 4
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 10 minutes, then dry; By 0.03 molar concentration copper acetate, 0.04 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 170 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2.5 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:1 mass ratio; Adopt knife coating to be evenly coated on ITO electro-conductive glass by above-mentioned slurry, then in argon gas atmosphere, sinter 40 minutes at 400 DEG C, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
Embodiment 5
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 10 minutes, then dry; By 0.03 molar concentration copper acetate, 0.04 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 170 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2.5 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:1 mass ratio; Adopt knife coating to be evenly coated on Copper Foil by above-mentioned slurry, then in argon gas atmosphere, sinter 40 minutes at 400 DEG C, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
Embodiment 6
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 10 minutes, then dry; By 0.03 molar concentration copper acetate, 0.04 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 170 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2.5 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:1 mass ratio; Adopt knife coating to be evenly coated on aluminium foil by above-mentioned slurry, then in argon gas atmosphere, sinter 40 minutes at 400 DEG C, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
Embodiment 7
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 10 minutes, then dry; By 0.03 molar concentration copper acetate, 0.04 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 170 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2.5 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:1 mass ratio; Adopt knife coating to be evenly coated on electro-conductive glass by above-mentioned slurry, then sintering 40 minutes at 400 DEG C under vacuum, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
Embodiment 8
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 10 minutes, then dry; By 0.03 molar concentration copper acetate, 0.04 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 170 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2.5 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:1 mass ratio; Adopt silk screen print method to be evenly coated on electro-conductive glass by above-mentioned slurry, then sintering 40 minutes at 400 DEG C under an argon atmosphere, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
Embodiment 9
By conductive substrates successively with deionized water, the ultrasonic cleaning of absolute ethyl alcohol difference 10 minutes, then dry; By 0.03 molar concentration copper acetate, 0.04 molar concentration thioacetamide respectively ultrasonic dissolution in diglycol, then under 170 DEG C of oil bath conditions by two kinds of solution hybrid reactions 2.5 hours, be prepared into Cu
2s nano particle, then itself and ethanol are prepared slurry by 1:1 mass ratio; Adopt spin-coating method to be evenly coated on electro-conductive glass by above-mentioned slurry, then sintering 40 minutes at 400 DEG C under an argon atmosphere, namely obtain Cu
2s porous nanocrystalline is to electrode.
Assembled battery process is identical with embodiment 1, and test result asks for an interview table 1.
The experimental result of the different embodiment of table 1
Claims (3)
1. a quantum dot sensitized solar cell porous nanocrystalline Cu
2s, to the preparation method of electrode, is characterized in that: with copper acetate and thioacetamide for presoma, is obtained the Cu of size 20 ~ 100 nanometer by solvent thermal reaction
2s nano particle, and be configured to slurry with ethanol, utilize knife coating, silk screen print method or spin-coating method to form the Cu of 5 ~ 10 microns at conducting base
2the nanocrystalline porous film of S, sinters 10 ~ 60 minutes at 300 ~ 500 DEG C and obtains battery electrode in inert atmosphere or vacuum.
2. quantum dot sensitized solar cell porous nanocrystalline Cu according to claim 1
2s, to the preparation method of electrode, is characterized in that: concrete preparation process is as follows:
A) conductive substrates is used successively deionized water, absolute ethyl alcohol difference ultrasonic cleaning 5 ~ 15 minutes, then dry;
B) by copper acetate, thioacetamide is dissolved in diglycol respectively, be configured to the thioacetyl amine aqueous solution of copper acetate solution that concentration is 0.02 ~ 0.04 molar concentration and 0.03 ~ 0.05 molar concentration, two kinds of solution mix according to volume ratio 3:1 ~ 1:1, then react 2 ~ 3 hours under 160 ~ 180 DEG C of oil bath conditions, centrifugal, washing, dry, obtain the Cu of 20 ~ 100 nanometers
2s particle;
C) by Cu
2s particle and ethanol prepare slurry by 2:1 ~ 1:2 mass ratio;
D) adopt knife coating, silk screen print method or spin-coating method to be evenly coated in conductive substrates by above-mentioned slurry, then in protective atmosphere or vacuum, sinter 30 ~ 60 minutes at 350 ~ 450 DEG C, obtain electrode film.
3. quantum dot sensitized solar cell porous nanocrystalline Cu according to claim 2
2s, to the preparation method of electrode, is characterized in that: described conductive substrates is mix the tin dioxide thin film glass (FTO) of F, mix the indium oxide (ITO) of Sn, Copper Foil or aluminium foil.
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Cited By (7)
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| CN104835649A (en) * | 2015-05-06 | 2015-08-12 | 上海交通大学 | Dye-sensitized solar cell silver sulfide counter electrode preparation method |
| CN105513805A (en) * | 2016-01-11 | 2016-04-20 | 上海交通大学 | Copper cadmium germanium sulphur nanocrystalline, copper cadmium germanium sulphur counter electrode, and preparation methods and application of copper cadmium germanium sulphur nanocrystalline and copper cadmium germanium sulphur counter electrode |
| CN106219997A (en) * | 2016-07-26 | 2016-12-14 | 北京航空航天大学 | A kind of technique preparing copper sulfide film on electro-conductive glass |
| CN106847513A (en) * | 2016-12-29 | 2017-06-13 | 陕西理工学院 | The preparation method of the sulfide nano-composite counter electrode based on porous C uS frameworks |
| CN109037640A (en) * | 2018-08-07 | 2018-12-18 | 河源广工大协同创新研究院 | A kind of preparation method of lithium ion battery negative material |
| CN111312522A (en) * | 2018-12-12 | 2020-06-19 | 南京理工大学 | Quantum dot sensitized solar cell CuS/Ti3C2Composite counter electrode and preparation method thereof |
| CN111524712A (en) * | 2020-04-13 | 2020-08-11 | 昆明理工大学 | Preparation method of three-dimensional porous structure dye-sensitized solar cell counter electrode |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104835649A (en) * | 2015-05-06 | 2015-08-12 | 上海交通大学 | Dye-sensitized solar cell silver sulfide counter electrode preparation method |
| CN104835649B (en) * | 2015-05-06 | 2018-06-26 | 上海交通大学 | A kind of dye-sensitized solar cells silver sulfide is to the preparation method of electrode |
| CN105513805A (en) * | 2016-01-11 | 2016-04-20 | 上海交通大学 | Copper cadmium germanium sulphur nanocrystalline, copper cadmium germanium sulphur counter electrode, and preparation methods and application of copper cadmium germanium sulphur nanocrystalline and copper cadmium germanium sulphur counter electrode |
| CN106219997A (en) * | 2016-07-26 | 2016-12-14 | 北京航空航天大学 | A kind of technique preparing copper sulfide film on electro-conductive glass |
| CN106847513A (en) * | 2016-12-29 | 2017-06-13 | 陕西理工学院 | The preparation method of the sulfide nano-composite counter electrode based on porous C uS frameworks |
| CN109037640A (en) * | 2018-08-07 | 2018-12-18 | 河源广工大协同创新研究院 | A kind of preparation method of lithium ion battery negative material |
| CN109037640B (en) * | 2018-08-07 | 2021-04-27 | 河源广工大协同创新研究院 | Preparation method of lithium ion battery negative electrode material |
| CN111312522A (en) * | 2018-12-12 | 2020-06-19 | 南京理工大学 | Quantum dot sensitized solar cell CuS/Ti3C2Composite counter electrode and preparation method thereof |
| CN111312522B (en) * | 2018-12-12 | 2022-02-18 | 南京理工大学 | Quantum dot sensitized solar cell CuS/Ti3C2Composite counter electrode and preparation method thereof |
| CN111524712A (en) * | 2020-04-13 | 2020-08-11 | 昆明理工大学 | Preparation method of three-dimensional porous structure dye-sensitized solar cell counter electrode |
| CN111524712B (en) * | 2020-04-13 | 2022-07-05 | 昆明理工大学 | Preparation method of three-dimensional porous structure dye-sensitized solar cell counter electrode |
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Application publication date: 20150204 |