CN107887168B - A kind of preparation method of the copper indium selenide of quantum dot sensitized solar battery to electrode - Google Patents
A kind of preparation method of the copper indium selenide of quantum dot sensitized solar battery to electrode Download PDFInfo
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- CN107887168B CN107887168B CN201711096501.4A CN201711096501A CN107887168B CN 107887168 B CN107887168 B CN 107887168B CN 201711096501 A CN201711096501 A CN 201711096501A CN 107887168 B CN107887168 B CN 107887168B
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- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000002096 quantum dot Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000004070 electrodeposition Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 22
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 5
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 4
- 238000005202 decontamination Methods 0.000 claims description 4
- 230000003588 decontaminative effect Effects 0.000 claims description 4
- 230000009977 dual effect Effects 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- LTUDISCZKZHRMJ-UHFFFAOYSA-N potassium;hydrate Chemical compound O.[K] LTUDISCZKZHRMJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 239000005361 soda-lime glass Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 230000005611 electricity Effects 0.000 claims 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims 1
- 229910052753 mercury Inorganic materials 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 239000003792 electrolyte Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 12
- 229910052711 selenium Inorganic materials 0.000 description 11
- 239000011669 selenium Substances 0.000 description 11
- 239000010949 copper Substances 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 9
- 229910052738 indium Inorganic materials 0.000 description 9
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 8
- 239000005864 Sulphur Substances 0.000 description 8
- 206010070834 Sensitisation Diseases 0.000 description 6
- 230000008313 sensitization Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 239000003708 ampul Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 229910052927 chalcanthite Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000003869 coulometry Methods 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Photovoltaic Devices (AREA)
- Hybrid Cells (AREA)
Abstract
The invention discloses a kind of copper indium selenide for quantum dot sensitized solar battery to the preparation method of electrode, is to prepare copper indium selenide to electrode film by the method for electrochemical deposition combination selenization.This method can be improved stability to electrode catalyst activity and its in the electrolyte, the final photoelectric conversion efficiency for improving photovoltaic device.The method that the present invention uses electrochemical deposition combination selenization, has many advantages, such as at low cost, easy to operate, easy industrial production.
Description
Technical field
The present invention relates to a kind of copper indium selenide for quantum dot sensitized solar battery to the preparation method of electrode, belongs to too
Positive energy battery thin film technical field.
Background technique
Increasingly the problems such as severe energy shortages, environmental pollution, promote people to explore and develop alternative new energy, such as
Solar energy.Solar energy can be converted directly into the device of electric energy as one kind, solar battery shows huge application
Prospect.Therefore, the solar cell device of exploitation efficiently, stable, inexpensive becomes the research hotspot in field.The quantum dot sun
Energy battery is a kind of novel third generation solar cell;It uses quantum dot as light absorbing material, makes its theoretical photoelectric conversion
Efficiency is up to 44%.Quantum dot is high with the absorption coefficient of light, spectral response range is adjustable, more excitons generate effect and can pass through letter
The advantages such as single solwution method preparation are a kind of very promising photoelectric functional material (Ru Zhou, et al., Nano
Energy 2016,30, 559–569;J.Du et al.,J.Am.Chem.Soc.2016,138,4201–4209).Therefore, closely
Nian Lai, quantum dot solar cell are quickly grown, and photoelectric conversion performance constantly breaks through soaring.
Sensitization type quantum dot solar cell device architecture mainly includes light anode, electrolyte and to electrode.Wherein, it is desirable that
There is good catalytic activity to electrode.However, common metal sulfide is to electrode, such as Cu2S, CoS, PbS etc., although right
The reduction activation of more sulphur electrolyte is very high, but long-time service can pollute electrolyte and light anode.Therefore, concern, which is explored, is used for quantum
Point sensitization solar battery it is novel to electrode, while its preparation process is optimized, improve its chemical property and its
Stability in electrolyte, to prepare high catalytic activity to electrode, improve Photovoltaic Device Performance be of great significance.
Summary of the invention
The object of the present invention is to provide a kind of copper indium selenide for quantum dot sensitized solar battery to the preparation side of electrode
Method.This method can be improved stability to electrode catalyst activity and its in the electrolyte, the final photoelectricity for improving photovoltaic device
Transfer efficiency.The method that the present invention uses electrochemical deposition combination selenization has industry at low cost, easy to operate, easy raw
The advantages that production.
The present invention is used for preparation method of the copper indium selenide to electrode of quantum dot sensitized solar battery, is heavy by electrochemistry
Prepared by the method that product combines selenization, include the following steps:
Step 1: pretreatment
Conductive substrates are cut to required size, decontamination liquid is respectively placed in, acetone, ethyl alcohol, is cleaned by ultrasonic in deionized water
10~30min is subsequently placed at ultraviolet and ozone cleaning machine processing 20min, saves backup;
Step 2: the preparation of electroplate liquid
By monohydrate potassium (C6H8O7·H2O), Salzburg vitriol (CuSO4·5H2O), indium sulfate (In2(SO4)3)、
Selenium dioxide (SeO2) mixed with ultrapure water, stirring is to being completely dissolved acquisition electroplate liquid;The molar concentration of each component in electroplate liquid
Respectively 0.3~0.5M of citric acid, 0.006~0.008M of copper sulphate, 0.006~0.008M of indium sulfate, selenium dioxide 0.01~
0.012M;
Step 3: electrochemical deposition
The electroplate liquid that step 2 is prepared is added in electrolytic cell, using pretreated conductive substrates as working electrode, with sulphur
Sour mercurous electrode as reference electrode, using polishing stainless steel piece as to electrode, constitute three-electrode system;When using constant potentiometer
Coulometry carries out electrochemical deposition, to be deposited to finish, and takes out copper indium selenide prefabricated membrane, dries up after being rinsed with deionized water;It is depositing
Before, argon gas is bubbled 10min to electroplate liquid through glass tube, to exclude the oxygen in solution;Sedimentation potential be set as -1.0V to -
1.2V, sedimentation time are 10~60min, and depositing temperature is 25 DEG C.During the deposition process, guarantee conducting surface and the throwing of conductive substrates
Light stainless steel substrates level is opposite.
Step 4: selenization
Step 3 gained copper indium selenide prefabricated membrane is placed in dual temperature area tube type resistance furnace, using argon gas as protective atmosphere, is protected
It is -0.06MPa that opposite outer, which is negative pressure, in card quartz ampoule;Underlayer temperature is 350~450 DEG C, warm area where selenium powder is 175~
225 DEG C, it is heat-treated 30~60min, obtains copper indium selenide to electrode film.
In step 1, the deposition substrate is FTO electro-conductive glass, ITO electro-conductive glass, soda-lime glass of surface sputtering molybdenum etc..
In step 4, heating and rate of temperature fall are 10 DEG C/min.
Compared with the prior art, effective effect of the invention is embodied in:
The surfacing of present invention preparation gained copper, indium and selenium film, object is mutually pure, catalytic activity is good, is highly suitable for quick
Change solar battery to electrode;Preparation method of the present invention is at low cost, simple process, reaction condition are mild, has wide research
Value and application prospect.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) map of copper, indium and selenium film produced by the present invention.As seen from Figure 1, institute is prepared
It is mutually pure to obtain copper, indium and selenium film object.
Fig. 2 is scanning electron microscope (SEM) photo on copper, indium and selenium film surface produced by the present invention.It can be seen by Fig. 2
Out, preparation gained copper, indium and selenium film surface uniform ground.
Fig. 3 is that the copper, indium and selenium film prepared with embodiment 1 is total to sensitization solar battery to electrode, with CdS/ as quantum dot
CdSe quantum dot, more sulphur electrolyte, which combine, is assembled into battery, tests the photovoltaic property curve of obtained device.It can from Fig. 3
Out, photoelectric conversion efficiency 2.52%, short circuit current Jsc are 14.7mA/cm2, open-circuit voltage Voc is 0.55V, fill factor FF
It is 34%.
Fig. 4 is that the copper, indium and selenium film prepared with embodiment 2 is total to sensitization solar battery to electrode, with CdS/ as quantum dot
CdSe quantum dot, more sulphur electrolyte, which combine, is assembled into battery, tests the photovoltaic property curve of obtained device.It can from Fig. 4
Out, photoelectric conversion efficiency 1.16%, short circuit current Jsc are 9.2mA/cm2, open-circuit voltage Voc is 0.47V, fill factor FF
It is 27%.
Specific embodiment
Technical solution of the present invention is described in detail below by specific embodiment.Obviously, described embodiment
A part of the embodiment only of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Embodiment 1:
1, it pre-processes
FTO conductive substrates are cut into 4cm*2cm size, decontamination liquid is respectively placed in, acetone, ethyl alcohol, surpasses in deionized water
Sound cleans 15min, is subsequently placed at ultraviolet and ozone cleaning machine processing 20min, saves backup;
2, the preparation of electroplate liquid
By monohydrate potassium (C6H8O7·H2O), Salzburg vitriol (CuSO4·5H2O), indium sulfate (In2(SO4)3)、
Selenium dioxide (SeO2) mixed with ultrapure water, it is using magnetic stirring apparatus that mixed solution stirring 60min is electric to acquisition is completely dissolved
Plating solution;The molar concentration of each component is respectively citric acid 0.4M, copper sulphate 0.006M, indium sulfate 0.006M, dioxy in electroplate liquid
Change selenium 0.01M.
3, electrochemical deposition
The electroplate liquid that step 2 is prepared is added in electrolytic cell, using pretreated conductive substrates as working electrode, with sulphur
Sour mercurous electrode as reference electrode, using polishing stainless steel piece as to electrode, constitute three-electrode system;When using constant potentiometer
Coulometry carries out electrochemical deposition, to be deposited to finish, and takes out copper indium selenide prefabricated membrane, dries up after being rinsed with deionized water;It is depositing
Before, argon gas is bubbled 10min to electroplate liquid through glass tube, to exclude the oxygen in solution;Sedimentation potential is set as -1.1V, sinks
The product time is 20min, and depositing temperature is 25 DEG C.During the deposition process, guarantee the conducting surface and polishing stainless steel piece of conductive substrates
It is horizontal opposite.
4, selenization
Step 3 gained copper indium selenide prefabricated membrane is placed in dual temperature area tube type resistance furnace, using argon gas as protective atmosphere, is protected
It is -0.06MPa that opposite outer, which is negative pressure, in card quartz ampoule;Underlayer temperature is 400 DEG C, and warm area where selenium powder is 200 DEG C, heat treatment
30min, heating and rate of temperature fall are 10 DEG C/min, obtain copper indium selenide to electrode film.
Copper, indium and selenium film manufactured in the present embodiment is used as quantum dot and is total to sensitization solar battery to electrode, with CdS/CdSe
Quantum dot, more sulphur electrolyte, which combine, is assembled into battery, tests device photoelectric conversion energy, photovoltaic property curve is shown in Fig. 3.
Embodiment 2:
1, it pre-processes
The soda-lime glass substrate for sputtering molybdenum is cut into 4cm*2cm size, be respectively placed in decontamination liquid, acetone, ethyl alcohol, go from
It is cleaned by ultrasonic 15min in sub- water, is subsequently placed at ultraviolet and ozone cleaning machine processing 20min, saves backup;
2, the preparation of electroplate liquid
By monohydrate potassium (C6H8O7·H2O), Salzburg vitriol (CuSO4·5H2O), indium sulfate (In2(SO4)3)、
Selenium dioxide (SeO2) mixed with ultrapure water, it is using magnetic stirring apparatus that mixed solution stirring 60min is electric to acquisition is completely dissolved
Plating solution;The molar concentration of each component is respectively citric acid 0.4M, copper sulphate 0.006M, indium sulfate 0.006M, dioxy in electroplate liquid
Change selenium 0.01M.
3, electrochemical deposition
The electroplate liquid that step 2 is prepared is added in electrolytic cell, using pretreated conductive substrates as working electrode, with sulphur
Sour mercurous electrode as reference electrode, using polishing stainless steel piece as to electrode, constitute three-electrode system;When using constant potentiometer
Coulometry carries out electrochemical deposition, to be deposited to finish, and takes out copper indium selenide prefabricated membrane, dries up after being rinsed with deionized water;It is depositing
Before, argon gas is bubbled 10min to electroplate liquid through glass tube, to exclude the oxygen in solution;Sedimentation potential is set as -1.1V, sinks
The product time is 40min, and depositing temperature is 25 DEG C.During the deposition process, guarantee the conducting surface and polishing stainless steel piece of conductive substrates
It is horizontal opposite.
4, selenization
Step 3 gained copper indium selenide prefabricated membrane is placed in dual temperature area tube type resistance furnace, using argon gas as protective atmosphere, is protected
It is -0.06MPa that opposite outer, which is negative pressure, in card quartz ampoule;Underlayer temperature is 400 DEG C, and warm area where selenium powder is 200 DEG C, heat treatment
30min, heating and rate of temperature fall are 10 DEG C/min, obtain copper indium selenide to electrode film.
Copper, indium and selenium film manufactured in the present embodiment is used as quantum dot and is total to sensitization solar battery to electrode, with CdS/CdSe
Quantum dot, more sulphur electrolyte, which combine, is assembled into battery, tests device photoelectric conversion energy, photovoltaic property curve is shown in Fig. 4.
Claims (2)
1. a kind of copper indium selenide for quantum dot sensitized solar battery is to the preparation method of electrode, it is characterised in that including as follows
Step:
Step 1: pretreatment
Conductive substrates are cut to required size, be respectively placed in decontamination liquid, acetone, ethyl alcohol, ultrasonic cleaning 10 in deionized water~
30min is subsequently placed at ultraviolet and ozone cleaning machine processing 20min, saves backup;
Step 2: the preparation of electroplate liquid
Monohydrate potassium, Salzburg vitriol, indium sulfate, selenium dioxide are mixed with ultrapure water, stirring is obtained to being completely dissolved
Obtain electroplate liquid;
Step 3: electrochemical deposition
The electroplate liquid that step 2 is prepared is added in electrolytic cell, using pretreated conductive substrates as working electrode, with sulfuric acid Asia
Mercury electrode as reference electrode, using polishing stainless steel piece as to electrode, constitute three-electrode system;Using electricity when constant potentiometer
Method carries out electrochemical deposition, to be deposited to finish, and takes out copper indium selenide prefabricated membrane, dries up after being rinsed with deionized water;
Step 4: selenization
Step 3 gained copper indium selenide prefabricated membrane is placed in dual temperature area tube type resistance furnace, using argon gas as protective atmosphere, guarantees stone
It is -0.06MPa that opposite outer, which is negative pressure, in English pipe;Underlayer temperature is 350~450 DEG C, and warm area where selenium powder is 175~225 DEG C,
It is heat-treated 30~60min, obtains copper indium selenide to electrode film;
In step 1, the deposition substrate is the soda-lime glass that FTO electro-conductive glass, ITO electro-conductive glass or surface sputter molybdenum;
In step 2, the molar concentration of each component is respectively 0.3~0.5M of citric acid in electroplate liquid, and copper sulphate 0.006~
0.008M, 0.006~0.008M of indium sulfate, 0.01~0.012M of selenium dioxide;
In step 3, before the deposition, argon gas is bubbled 10min to electroplate liquid through glass tube, to exclude the oxygen in solution;It is heavy
Product current potential is set as -1.0V to -1.2V, and sedimentation time is 10~60min, and depositing temperature is 25 DEG C.
2. preparation method according to claim 1, it is characterised in that:
In step 4, heating and rate of temperature fall are 10 DEG C/min.
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