CN106328381A - All-solid-state quantum dot sensitized solar cell and preparation method thereof - Google Patents
All-solid-state quantum dot sensitized solar cell and preparation method thereof Download PDFInfo
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- CN106328381A CN106328381A CN201611037388.8A CN201611037388A CN106328381A CN 106328381 A CN106328381 A CN 106328381A CN 201611037388 A CN201611037388 A CN 201611037388A CN 106328381 A CN106328381 A CN 106328381A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000010949 copper Substances 0.000 claims abstract description 51
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052802 copper Inorganic materials 0.000 claims abstract description 34
- 239000003792 electrolyte Substances 0.000 claims abstract description 31
- 239000002070 nanowire Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 94
- 239000000243 solution Substances 0.000 claims description 67
- 239000008151 electrolyte solution Substances 0.000 claims description 50
- 239000000843 powder Substances 0.000 claims description 28
- 239000011259 mixed solution Substances 0.000 claims description 26
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 14
- 229910052717 sulfur Inorganic materials 0.000 claims description 14
- 239000011593 sulfur Substances 0.000 claims description 14
- 238000005516 engineering process Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 229910018162 SeO2 Inorganic materials 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000005864 Sulphur Substances 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 7
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 7
- 229920002307 Dextran Polymers 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- 206010070834 Sensitisation Diseases 0.000 claims description 5
- 230000008313 sensitization Effects 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000006193 liquid solution Substances 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 239000007784 solid electrolyte Substances 0.000 abstract 5
- 239000002135 nanosheet Substances 0.000 abstract 2
- 239000011701 zinc Substances 0.000 description 18
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 8
- 238000013019 agitation Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 6
- 238000005538 encapsulation Methods 0.000 description 5
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000004246 zinc acetate Substances 0.000 description 4
- 239000011244 liquid electrolyte Substances 0.000 description 3
- 229910052756 noble gas Inorganic materials 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000004065 semiconductor Substances 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
- H01G9/2004—Light-sensitive devices characterised by the electrolyte, e.g. comprising an organic electrolyte
- H01G9/2009—Solid electrolytes
-
- 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
- H01G9/0029—Processes of manufacture
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Hybrid Cells (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention discloses an all-solid-state quantum dot sensitized solar cell which comprises conductive glass and a copper substrate. The conductive glass is opposite to the copper substrate, the space between the conductive glass and the copper substrate is filled with solid electrolyte, a photo-anode is arranged on the conductive glass and positioned on one side of the solid electrolyte, a copper-based Cu2S nano-sheet counter electrode is arranged on the copper substrate and positioned on the other side of the solid electrolyte, and the photo-anode is a CdS/CdSe quantum dot sensitized ZnO nanowire array photo-anode. By synthesizing and heating the solid electrolyte with good conductivity, the microstructure gap between the ZnO nanowire array photo-anode and the copper-based Cu2S nano-sheet counter electrode is sufficiently filled with the solid electrolyte, the problems of unstable performance of a liquid quantum dot sensitized solar cell and electrolyte omission in the package process are solved, and the all-solid-state quantum dot sensitized solar cell is simple in preparation process, low in cost, good in large-area preparation repeatability and excellent in use value.
Description
Technical field
The invention belongs to quantum dot sensitized technical field of solar batteries, be specifically related to a kind of all solid state quantum dot sensitized too
Sun energy battery, the invention still further relates to the preparation method of a kind of all solid state quantum dot sensitized solaode.
Background technology
In recent years, along with the demand of the energy is continuously increased and the lasting minimizing of fossil fuel reserves by people, find one
One of new abundance, the energy of environmental protection important topic having become current scientific research.Solar energy as one take no
Most natural energy source is increasingly subject to global concern, especially solar energy is converted into the solaode research of electric energy
Become the focus of research at present.
Quantum dot sensitized solaode (QDSSC) is the third generation solar cell occurred the nineties in last century, i.e. profit
Base material with inorganic semiconductor quantum dot (QD) the sensitization broad stopband of low energy gap.Quantum dot has the biggest excellent relative to dyestuff
Gesture, on the one hand, it has quantum confined effect, can carry out the band gap width of quantum point by controlling its size and dimension, with
This regulates the scope of absorption spectrum;On the other hand, semiconductor-quantum-point has exciton multiplier effect (MEG), a high-energy
Photon excitation semiconductor-quantum-point, multiple electron-hole pair can be produced.If should by the two of semiconductor-quantum-point big advantages
Using in solaode, the theoretical value of quantum dot sensitized solar battery efficiency can reach 44%, and significantly larger than crystalline silicon is too
The theoretical value 32.9% of sun energy battery.Therefore, the potentiality of the development of quantum dot sensitized solaode are huge.
At present, the electrolyte that quantum dot sensitized solaode is used is many sulfur (Sn2-/S2-) liquid electrolyte, so
And study discovery (I be applicable to DSSC3-/I-) platinum of electrolyte is no longer appropriate for (Sn2-/S2-) electrolyte,
Because S2-Chemisorbed in platinum electrode surface reduces the electrode catalysis activity to electrolyte, thus have impact on the property of battery
Energy.In the battery about various quantum dot sensitized optimum efficiencies, prepared by the Copper Foil substrate that all uses without exception
Cu2S is to electrode, because the advantage of this electrode: one is that the micro structure that pine is dredged has huge catalysis activity, and two is that Copper Foil is as substrate
There is fabulous electric conductivity.But, this Cu2Electrode is caused battery performance unstable by S, and one is that liquid electrolyte is to Cu substrate
Constantly corrosion cause adhesiveness to reduce, contact resistance increases, two is the Cu come off2S and light positive contact cause in light anode
Poison, three is liquid electrolyte encapsulation difficulty in quantum dot sensitized solaode, and long-time preservation there will be electrolyte omission, lead
Cause battery performance heavy losses.
Summary of the invention
It is an object of the invention to provide a kind of all solid state quantum dot sensitized solaode, solved by this battery structure
Existing liquid quantum dot sensitized solaode in use unstable properties, the problem of encapsulation difficulty.
It is a further object to provide the preparation method of a kind of all solid state quantum dot sensitized solaode.
The technical solution adopted in the present invention is, a kind of all solid state quantum dot sensitized solaode, including being oppositely arranged
Electro-conductive glass and copper base, between electro-conductive glass and copper base, be filled with solid-state electrolytic solution, electro-conductive glass be positioned at solid-state
The side of electrolyte is provided with light anode;The side being positioned at solid-state electrolytic solution on copper base is provided with electrode.
It is a feature of the present invention that
Solid-state electrolytic solution is many sulfur electrolyte.
It is cuprio Cu to electrode2S nanometer sheet is to electrode, and light anode is ZnO nano linear array quantum dot sensitized for CdS/CdSe
Row light anode.
Another technical scheme of the present invention is, the preparation side of a kind of all solid state quantum dot sensitized solaode
Method, comprises the following steps:
Step 1, prepares ZnO nanowire array on electro-conductive glass;
Step 2, carries out the ZnO nanowire array in step 1 CdS/CdSe quantum dot deposition, obtains light anode;
Step 3, prepares Cu on copper base2S is to electrode;
Step 4, prepares solid-state electrolytic solution;
Step 5, the solid-state electrolytic solution in electrode and step 4 is gone forward side by side in light anode in heating steps 2, step 3
Row encapsulation, forms battery.
Inventive feature also resides in,
Step 1 particularly as follows:
Step 1.1, the precursor solution of preparation ZnO Seed Layer, the forerunner of ZnO Seed Layer is used in the side of electro-conductive glass
Liquid solution, prepares ZnO Seed Layer by spin-coating method and Technology for Heating Processing, and wherein spin speed is 3000-4500r/min, heat
The temperature processing technique is 300-350 DEG C, and the thickness of ZnO Seed Layer is 50-100nm;
Step 1.2, puts in growth-promoting media by the ZnO Seed Layer in step 1.1, and using temperature is the immersion method of 80-90 DEG C
Preparing ZnO nanowire array, wherein growth-promoting media is NaOH Yu the Zn (NO of molar concentration rate 20:13)2Mixed solution or molar concentration
Hexamethylenetetramine than 1:1 and Zn (NO3)2The ammonia of mixed solution or molar concentration rate 1:1 and Zn (NO3)2Mixed solution.
Step 2 particularly as follows:
Step 2.1, repeatedly alternately immerses the Na of same molar ratio by the ZnO nanowire array in step 12S solution with
Cd(NO3)2Methanol solution, obtains the ZnO nanowire array of CdS quantum dot sensitization;
Step 2.2, adding mol ratio in methanol solution is the KBH of 1-1.5:14Powder and SeO2Powder, adds thermal reduction and obtains
To solution a, step 2.1 is processed the ZnO nanowire array obtained and the most alternately immerses Cd (NO3)2Methanol solution and solution a,
To the ZnO nanowire array that CdS/CdSe is quantum dot sensitized, i.e. light anode, wherein Cd (NO3)2Methanol solution and SeO2Powder rubs
Your concentration is identical.
Step 3 particularly as follows:
Step 3.1, by copper base in sand papering is placed on ethanol solution, carries out ultrasonic waves for cleaning 20-30min;
Step 3.2, copper base side step 3.1 processed is blocked 5-10min in the concentrated hydrochloric acid being placed in 70 DEG C, is taken
Deionized water and methanol is used to rinse and be dried after going out;
Step 3.3, copper base step 3.2 processed is placed in many sulfur electrolyte and carries out vulcanizing treatment 10-15min,
Use deionized water and methanol to rinse and be dried after taking-up, obtain the Cu of cuprio black2S is to electrode, and is placed on indifferent gas
Body preserves.
Step 4 particularly as follows:
Step 4.1, is slowly added to appropriate dextran in the KCL aqueous solution that quality is 3-5g, stirs at 85-100 DEG C
Mixing uniformly, wherein the concentration of KCL aqueous solution is 20-30%;
Step 4.2, is sequentially added into 0.09-0.10g high purity sulphur powder and 0.65-0.75g in the solution that step 4.1 obtains
Na2S·9H2O, is cooled to room temperature after stirring, obtain hydrosol electrolyte, i.e. solid-state electrolytic solution.
Step 5 particularly as follows:
Step 5.1, by all preheating with the solid-state electrolytic solution in step 4 electrode in the light anode in step 2, step 3
To 60-80 DEG C;
Step 5.2, drops to the light anode table after step 5.1 processes by the solid-state electrolytic solution processed through step 5.1 in right amount
Face, is i.e. engraved in evacuation 5-10min in the hermetic container of identical temperature;
Step 5.3, the solid-state electrolytic solution processed through step 5.1 in right amount is dropped to after step 5.1 processes to electrode table
Face, is i.e. engraved in evacuation 5-10min in the hermetic container of identical temperature;
Step 5.4, take step 5.2 process light anode and step 5.3 process to electrode, be respectively placed in certain thickness
The interval body both sides of degree are just to contact, and heating makes solid-state electrolytic solution fully merge, and is packaged into battery.
The invention has the beneficial effects as follows: the solid-state electrolytic solution that the present invention is good by synthesizing electric conductivity, by heating solid-state
Electrolyte so that it is be adequately filled in ZnO nanowire array light anode and cuprio Cu2The S nanometer sheet micro structure space to electrode,
Not only overcome the electrolyte that there will be in the unstable properties of the quantum dot sensitized solaode of liquid and encapsulation process to lose
Leakage problem, and preparation technology is simple, with low cost, large area is prepared reproducible, has good use value.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of all solid state quantum dot sensitized solaode of the present invention.
In figure, 1. solid-state electrolytic solution, 2. electro-conductive glass, 3. copper base, 4. pair electrode, the most smooth anode.
Detailed description of the invention
The present invention is described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
A kind of all solid state quantum dot sensitized solaode of the present invention, as it is shown in figure 1, include the electro-conductive glass being oppositely arranged
2 and copper base 3, between electro-conductive glass 2 and copper base 3, it is filled with solid-state electrolytic solution 1, electro-conductive glass 2 is positioned at solid state electrolysis
The side of liquid 1 is provided with light anode 5;The side being positioned at solid-state electrolytic solution 1 on copper base 3 is provided with electrode 4.
Solid-state electrolytic solution 1 is many sulfur electrolyte.
The preparation method of a kind of all solid state quantum dot sensitized solaode of the present invention, comprises the following steps:
Step 1, prepares ZnO nanowire array on electro-conductive glass 2
Step 1.1, the precursor solution of preparation ZnO Seed Layer, before the side of electro-conductive glass 2 uses ZnO Seed Layer
Driving liquid solution, prepare ZnO Seed Layer by spin-coating method and Technology for Heating Processing, wherein spin speed is 3000-4500r/min,
The temperature of Technology for Heating Processing is 300-350 DEG C, and the thickness of ZnO Seed Layer is 50-100nm;
The precursor solution of ZnO Seed Layer particularly as follows: 16.46g zinc acetate is added 4.5ml monoethanolamine (MEA) with
In the mixed solution of 100ml ethylene glycol monomethyl ether, then magnetic agitation 30min under 60 DEG C of hydrothermal conditions, afterwards the perseverance of 30 DEG C
Incubator is aged 24h;
Step 1.2, puts in growth-promoting media by the ZnO Seed Layer in step 1.1, and using temperature is the immersion method of 80-90 DEG C
Preparing ZnO nanowire array, wherein growth-promoting media is NaOH Yu the Zn (NO of molar concentration rate 20:13)2Mixed solution or molar concentration
Hexamethylenetetramine than 1:1 and Zn (NO3)2The ammonia of mixed solution or molar concentration rate 1:1 and Zn (NO3)2Mixed solution;
Wherein, NaOH Yu the Zn (NO of molar concentration rate 20:13)2The concrete preparation of mixed solution: under magnetic agitation, first
By the Zn (NO of NaOH and 0.004mol of 0.08mol3)2·6H2O is dissolved separately in 50ml deionized water, then by Zn
(NO3)2·6H2O solution adds NaOH solution the most slowly and stirs;
The hexamethylenetetramine of molar concentration rate 1:1 and Zn (NO3)2The concrete preparation of mixed solution: under magnetic agitation, first
First by hexamethylenetetramine and the Zn (NO of 0.1mol of 0.1mol3)2·6H2O is dissolved separately in 50ml deionized water, then
By Zn (NO3)2·6H2It is uniform that O solution adds hexamethylenetetramine solution & stir the most slowly;
The ammonia of molar concentration rate 1:1 and Zn (NO3)2The concrete preparation of mixed solution: under magnetic agitation, join the most respectively
Concentration processed is the Zn (NO of 0.1mol/L3)2·6H2O solution and each 50ml of ammonia spirit, then by Zn (NO3)26H2O solution exists
Add ammonia spirit under magnetic agitation slowly and stir.
Step 2, carries out the ZnO nanowire array in step 1 CdS/CdSe quantum dot deposition, obtains light anode 5
Step 2.1, repeatedly alternately immerses the Na of same molar ratio by the ZnO nanowire array in step 12S solution with
Cd(NO3)2Methanol solution, obtains the ZnO nanowire array of CdS quantum dot sensitization;
Step 2.2, adding mol ratio in methanol solution is the KBH of 1-1.5:14Powder and SeO2Powder, adds thermal reduction and obtains
To solution a;Step 2.1 is processed the ZnO nanowire array obtained and the most alternately immerses Cd (NO3)2Methanol solution and solution a,
To the ZnO nanowire array that CdS/CdSe is quantum dot sensitized, i.e. light anode 5, wherein Cd (NO3)2Methanol solution and SeO2Powder rubs
Your concentration is identical.
Step 3, prepares Cu on copper base 32S is to electrode 4;
Step 3.1, by copper base 3 in sand papering is placed on ethanol solution, carries out ultrasonic waves for cleaning 20-30min;
Step 3.2, copper base 3 side step 3.1 processed blocks 5-10min in the concentrated hydrochloric acid being placed in 70 DEG C,
Deionized water and methanol is used to rinse and be dried after taking-up;
Step 3.3, the copper base 3 step 3.2 processed is placed in many sulfur electrolyte and carries out vulcanizing treatment 10-15min,
Use deionized water and methanol to rinse and be dried after taking-up, obtain the Cu of cuprio black2S is to electrode 4, and is placed on indifferent gas
Preserving in body, wherein many sulfur electrolyte is: be respectively the Na of 2mol/L by concentration2The high purity sulphur powder of S, 2mol/L and 0.2mol/L
KCl be dissolved in methanol that volume ratio is 7:3 and prepare in the mixed solution of deionized water.
Step 4, prepares solid-state electrolytic solution 1
Step 4.1, is slowly added to appropriate dextran in the KCL aqueous solution that quality is 3-5g, stirs at 85-100 DEG C
Mixing uniformly, wherein the concentration of KCL aqueous solution is 20-30%;
Step 4.2, is sequentially added into 0.09-0.10g high purity sulphur powder and 0.65-0.75g in the solution that step 4.1 obtains
Na2S·9H2O, is cooled to room temperature after stirring, obtain hydrosol electrolyte, i.e. solid-state electrolytic solution 1.
Step 5, in light anode 5 in heating steps 2, step 3 to the solid-state electrolytic solution 1 in electrode 4 and step 4 also
It is packaged, forms battery
Step 5.1, the most pre-with the solid-state electrolytic solution 1 in step 4 to electrode 4 by the light anode 5 in step 2, step 3
Heat is to 60-80 DEG C;
Step 5.2, drops to the light anode 5 after step 5.1 processes by the solid-state electrolytic solution 1 processed through step 5.1 in right amount
Surface, is i.e. engraved in evacuation 5-10min in the hermetic container of identical temperature;
Step 5.3, the solid-state electrolytic solution 1 processed through step 5.1 in right amount is dropped to after step 5.1 processes to electrode 4
Surface, is i.e. engraved in evacuation 5-10min in the hermetic container of identical temperature;
Step 5.4, takes light anode 5 that step 5.2 processes and step 5.3 processes to electrode 4, is respectively placed in certain
The interval body both sides of thickness are just to contact, and heating makes solid-state electrolytic solution 1 fully merge, and is packaged into battery.
Embodiment 1
(1) light anode 5 is prepared
The precursor solution of preparation ZnO Seed Layer: 16.46g zinc acetate is added 4.5ml monoethanolamine (MEA) and 100ml
In the mixed solution of ethylene glycol monomethyl ether, then magnetic agitation 30min under 60 DEG C of hydro-thermals, it is aged in the calorstat of 30 DEG C afterwards
24h。
Preparation solution a: adding mol ratio in methanol solution is the KBH of 1:14Powder and SeO2Powder, adds thermal reduction and obtains
Solution a.
Use the precursor solution of ZnO Seed Layer in the side of electro-conductive glass 2, prepared by spin-coating method and Technology for Heating Processing
ZnO Seed Layer, wherein spin speed is 3000r/min, and the temperature of Technology for Heating Processing is 300 DEG C, it is thus achieved that the thickness of ZnO Seed Layer
For 50nm;ZnO Seed Layer is placed in NaOH Yu the Zn (NO of molar concentration rate 20:13)2Mixed solution, raw in the water-bath of 80 DEG C
Long ZnO nanowire array;ZnO nanowire array is repeatedly alternately immersed the Na of same molar ratio2S solution and Cd (NO3)2First
Alcoholic solution, the most alternately immerses and SeO2Cd (the NO that powder molar concentration is identical3)2In methanol solution and solution a,
To light anode 5.
(2) preparation is to electrode 4
Prepare many sulfur electrolyte: be respectively the Na of 2mol/L by concentration2The high purity sulphur powder of S, 2mol/L is with 0.2mol/L's
KCl is dissolved in the methanol that volume ratio is 7:3 to be prepared in the mixed solution of deionized water.
By copper base 3 in sand papering is placed on ethanol solution, carry out ultrasonic waves for cleaning 20min, then by copper base 3
5min in the concentrated hydrochloric acid being placed in 70 DEG C is blocked in side, uses deionized water and methanol rinsing, drying after taking-up;It is placed in many sulfur again
Electrolyte carries out vulcanizing treatment 10min, uses deionized water and methanol rinsing, drying after taking-up, obtain cuprio black
Cu2Electrode 4 is placed in noble gas preserving by S, standby.
(3) solid-state electrolytic solution 1 is prepared
Appropriate dextran is slowly added in the KCL aqueous solution that quality is 3g, stirs at 85 DEG C, wherein KCL
The concentration of aqueous solution is 20%;Then in mixed solution, it is sequentially added into the Na of 0.09g high purity sulphur powder and 0.65g2S·9H2O, stirs
It is cooled to room temperature after mixing uniformly, obtains hydrosol electrolyte, i.e. solid-state electrolytic solution 1.
(4) assemble
By light anode 5, electrode 4 and solid-state electrolytic solution 1 are all preheated to 60 DEG C;The solid-state electrolytic solution 1 that will preheat in right amount
Add to light anode 5 surface of preheating, be i.e. engraved in evacuation 5min in the hermetic container of 60 DEG C;Solid-state electrolytic solution 1 by preheating
Add to preheating to electrode 4 surface, be i.e. engraved in evacuation 5min in the hermetic container of 60 DEG C;Then by light anode 5 with to electrode 4
It is respectively placed in certain thickness interval body both sides just to contact, and heats and make solid-state electrolytic solution 1 fully merge, be packaged into battery.
Embodiment 2
(1) light anode 5 is prepared
The precursor solution of preparation ZnO Seed Layer: 16.46g zinc acetate is added 4.5ml monoethanolamine (MEA) and 100ml
In the mixed solution of ethylene glycol monomethyl ether, then magnetic agitation 30min under 60 DEG C of hydro-thermals, it is aged in the calorstat of 30 DEG C afterwards
24h。
Preparation solution a: adding mol ratio in methanol solution is the KBH of 1.2:14Powder and SeO2Powder, adds thermal reduction and obtains
To solution a.
Use the precursor solution of ZnO Seed Layer to be prepared by spin-coating method and Technology for Heating Processing in the side of electro-conductive glass 2
ZnO Seed Layer, wherein spin speed is 3800r/min, and the temperature of Technology for Heating Processing is 320 DEG C, it is thus achieved that the thickness of ZnO Seed Layer
For 80nm;ZnO Seed Layer is placed in hexamethylenetetramine and the Zn (NO of molar concentration rate 1:13)2Mixed solution, at the water of 85 DEG C
Growing ZnO nano-wire array in bath;ZnO nanowire array is repeatedly alternately immersed the Na of same molar ratio2S solution and Cd
(NO3)2Methanol solution, the most alternately immerses and SeO2Cd (the NO that powder molar concentration is identical3)2Methanol solution and solution
In a, obtain light anode 5.
(2) preparation is to electrode 4
Prepare many sulfur electrolyte: be respectively the Na of 2mol/L by concentration2The high purity sulphur powder of S, 2mol/L is with 0.2mol/L's
KCl is dissolved in the methanol that volume ratio is 7:3 to be prepared in the mixed solution of deionized water.
By copper base 3 in sand papering is placed on ethanol solution, carry out ultrasonic waves for cleaning 25min, then by copper base 3
8min in the concentrated hydrochloric acid being placed in 70 DEG C is blocked in side, uses deionized water and methanol rinsing, drying after taking-up;It is placed in many sulfur again
Electrolyte carries out vulcanizing treatment 12min, uses deionized water and methanol rinsing, drying after taking-up, obtain cuprio black
Cu2Electrode 4 is placed in noble gas preserving by S, standby.
(3) solid-state electrolytic solution 1 is prepared
Appropriate dextran is slowly added in the KCL aqueous solution that quality is 4g, stirs at 90 DEG C, wherein KCL
The concentration of aqueous solution is 25%;Then in mixed solution, it is sequentially added into the Na of 0.096g high purity sulphur powder and 0.70g2S·9H2O,
It is cooled to room temperature after stirring, obtains hydrosol electrolyte, i.e. solid-state electrolytic solution 1.
(4) assemble
By light anode 5, electrode 4 and solid-state electrolytic solution 1 are all preheated to 70 DEG C;By the solid-state electrolytic solution 1 of appropriate preheating
Drop to light anode 5 surface of preheating, be i.e. engraved in evacuation 8min in the hermetic container of 70 DEG C;By the solid-state electricity of appropriate preheating
Solve liquid 1 drop to preheating to electrode 4 surface, carry out evacuation 8min in being i.e. engraved in the hermetic container of 70 DEG C;Then by light sun
Pole 5 with electrode 4 is respectively placed in certain thickness interval body both sides just to contacting, and heat and make solid-state electrolytic solution 1 fully merge,
It is packaged into battery.
Embodiment 3
(1) light anode 5 is prepared
The precursor solution of preparation ZnO Seed Layer: 16.46g zinc acetate is added 4.5ml monoethanolamine (MEA) and 100ml
In the mixed solution of ethylene glycol monomethyl ether, then magnetic agitation 30min under 60 DEG C of hydro-thermals, it is aged in the calorstat of 30 DEG C afterwards
24h。
Preparation solution a: adding mol ratio in methanol solution is the KBH of 1.5:14Powder and SeO2Powder, adds thermal reduction and obtains
To solution a.
Use the precursor solution of ZnO Seed Layer to be prepared by spin-coating method and Technology for Heating Processing in the side of electro-conductive glass 2
ZnO Seed Layer, wherein spin speed is 4500r/min, and the temperature of Technology for Heating Processing is 350 DEG C, it is thus achieved that the thickness of ZnO Seed Layer
For 100nm;ZnO Seed Layer is placed in ammonia and the Zn (NO of molar concentration rate 1:13)2Mixed solution, raw in the water-bath of 90 DEG C
Long ZnO nanowire array;ZnO nanowire array is repeatedly alternately immersed the Na of same molar ratio2S solution and Cd (NO3)2First
Alcoholic solution, the most alternately immerses and SeO2Cd (the NO that powder molar concentration is identical3)2In methanol solution and solution a,
To light anode 5.
(2) preparation is to electrode 4
Prepare many sulfur electrolyte: be respectively the Na of 2mol/L by concentration2The high purity sulphur powder of S, 2mol/L is with 0.2mol/L's
KCl is dissolved in the methanol that volume ratio is 7:3 to be prepared in the mixed solution of deionized water.
By copper base 3 in sand papering is placed on ethanol solution, carry out ultrasonic waves for cleaning 30min, then by copper base 3
10min in the concentrated hydrochloric acid being placed in 70 DEG C is blocked in side, uses deionized water and methanol rinsing, drying after taking-up;It is placed in many again
Sulfur electrolyte carries out vulcanizing treatment 15min, uses deionized water and methanol rinsing, drying after taking-up, obtain cuprio black
Cu2Electrode 4 is placed in noble gas saving backup by S.
(3) solid-state electrolytic solution 1 is prepared
Appropriate dextran is slowly added in the KCL aqueous solution that quality is 5g, stirs at 100 DEG C, wherein KCL
The concentration of aqueous solution is 30%;Then in mixed solution, it is sequentially added into the Na of 0.10g high purity sulphur powder and 0.75g2S·9H2O, stirs
It is cooled to room temperature after mixing uniformly, obtains hydrosol electrolyte, i.e. solid-state electrolytic solution 1.
(4) assemble
By light anode 5, electrode 4 and solid-state electrolytic solution 1 are all preheated to 80 DEG C;Take the solid-state electrolytic solution 1 of appropriate preheating
Drop to light anode 5 surface of preheating, be i.e. engraved in evacuation 10min in the hermetic container of 80 DEG C;Take the solid-state of appropriate preheating
Electrolyte 1 drop to preheating to electrode 4 surface, be i.e. engraved in evacuation 10min in the hermetic container of 80 DEG C;Then by light anode
5 with electrode 4 is respectively placed in certain thickness interval body both sides just to contacting, and heat and make solid-state electrolytic solution 1 fully merge, envelope
Dress up battery.
The solid-state electrolytic solution 1 that the present invention is good by synthesizing electric conductivity, by heating solid-state electrolytic solution 1 so that it is fully
It is filled in ZnO nanowire array light anode and cuprio Cu2The S nanometer sheet micro structure space to electrode, not only overcomes liquid amount
The electrolyte omission problem occurred in the unstable properties of son point sensitization solar battery and encapsulation process, and preparation technology
Simply, with low cost, large area prepare reproducible, have good use value.
Claims (9)
1. an all solid state quantum dot sensitized solaode, it is characterised in that include electro-conductive glass (2) and the copper being oppositely arranged
Substrate (3), is filled with solid-state electrolytic solution (1), described electro-conductive glass between described electro-conductive glass (2) and copper base (3)
(2) side being positioned at solid-state electrolytic solution (1) on is provided with light anode (5);It is positioned at solid-state electrolytic solution on described copper base (3)
(1) side is provided with electrode (4).
The all solid state quantum dot sensitized solaode of one the most according to claim 1, it is characterised in that described solid-state
Electrolyte (1) is many sulfur electrolyte.
The all solid state quantum dot sensitized solaode of one the most according to claim 1, it is characterised in that described to electricity
Pole (4) is cuprio Cu2S nanometer sheet is ZnO nano linear array quantum dot sensitized for CdS/CdSe to electrode, described light anode (5)
Row light anode.
4. the preparation method of an all solid state quantum dot sensitized solaode as claimed in claim 1, it is characterised in that bag
Include following steps:
Step 1, prepares ZnO nanowire array on electro-conductive glass (2);
Step 2, carries out CdS/CdSe quantum dot deposition by the ZnO nanowire array in step 1, obtains light anode (5);
Step 3, prepares Cu on copper base (3)2S is to electrode (4);
Step 4, prepares solid-state electrolytic solution (1);
Step 5, in light anode (5) in heating steps 2, step 3 to the solid-state electrolytic solution (1) in electrode (4) and step 4
And be packaged, form battery.
The preparation method of a kind of all solid state quantum dot sensitized solaode the most according to claim 4, it is characterised in that
Described step 1 particularly as follows:
Step 1.1, the precursor solution of preparation ZnO Seed Layer, the forerunner of ZnO Seed Layer is used in the side of electro-conductive glass (2)
Liquid solution, prepares ZnO Seed Layer by spin-coating method and Technology for Heating Processing, and wherein spin speed is 3000-4500r/min, heat
The temperature processing technique is 300-350 DEG C, and the thickness of ZnO Seed Layer is 50-100nm;
Step 1.2, puts in growth-promoting media by the ZnO Seed Layer in step 1.1, prepared by the immersion method using temperature to be 80-90 DEG C
ZnO nanowire array, wherein growth-promoting media is NaOH Yu the Zn (NO of molar concentration rate 20:13)2Mixed solution or molar concentration rate 1:
The hexamethylenetetramine of 1 and Zn (NO3)2The ammonia of mixed solution or molar concentration rate 1:1 and Zn (NO3)2Mixed solution.
The preparation method of a kind of all solid state quantum dot sensitized solaode the most according to claim 4, it is characterised in that
Described step 2 particularly as follows:
Step 2.1, repeatedly alternately immerses the Na of same molar ratio by the ZnO nanowire array in step 12S solution and Cd
(NO3)2Methanol solution, obtains the ZnO nanowire array of CdS quantum dot sensitization;
Step 2.2, adding mol ratio in methanol solution is the KBH of 1-1.5:14Powder and SeO2Powder, adds thermal reduction and obtains molten
Liquid a;Step 2.1 is processed the ZnO nanowire array obtained and the most alternately immerses Cd (NO3)2Methanol solution and solution a, obtain
The ZnO nanowire array that CdS/CdSe is quantum dot sensitized, i.e. light anode (5), wherein Cd (NO3)2Methanol solution and SeO2Powder rubs
Your concentration is identical.
The preparation method of a kind of all solid state quantum dot sensitized solaode the most according to claim 4, it is characterised in that
Described step 3 particularly as follows:
Step 3.1, by copper base (3) in sand papering is placed on ethanol solution, carries out ultrasonic waves for cleaning 20-30min;
Step 3.2, copper base step 3.1 processed (3) side is blocked 5-10min in the concentrated hydrochloric acid being placed in 70 DEG C, is taken
Deionized water and methanol is used to rinse and be dried after going out;
Step 3.3, copper base step 3.2 processed (3) is placed in many sulfur electrolyte and carries out vulcanizing treatment 10-15min, takes
Use deionized water and methanol to rinse and be dried after going out, obtain the Cu of cuprio black2S is to electrode (4), and is placed on indifferent gas
Body preserves.
The preparation method of a kind of all solid state quantum dot sensitized solaode the most according to claim 4, it is characterised in that
Described step 4 particularly as follows:
Step 4.1, is slowly added to appropriate dextran in the KCL aqueous solution that quality is 3-5g, 85-100 DEG C of stirring all
Even, wherein the concentration of KCL aqueous solution is 20-30%;
Step 4.2, is sequentially added into 0.09-0.10g high purity sulphur powder and 0.65-0.75g Na in the solution that step 4.1 obtains2S·
9H2O, is cooled to room temperature after stirring, obtain hydrosol electrolyte, i.e. solid-state electrolytic solution (1).
The preparation method of a kind of all solid state quantum dot sensitized solaode the most according to claim 4, it is characterised in that
Described step 5 particularly as follows:
Step 5.1, equal to the solid-state electrolytic solution (1) in electrode (4) and step 4 by the light anode (5) in step 2, step 3
It is preheated to 60-80 DEG C;
Step 5.2, drops to the light anode (5) after step 5.1 processes through step 5.1 by the solid-state electrolytic solution (1) processed in right amount
Surface, is i.e. engraved in evacuation 5-10min in the hermetic container of identical temperature;
Step 5.3, the solid-state electrolytic solution (1) processed through step 5.1 in right amount is dropped to after step 5.1 processes to electrode (4)
Surface, is i.e. engraved in evacuation 5-10min in the hermetic container of identical temperature;
Step 5.4, takes light anode (5) that step 5.2 processes and step 5.3 processes to electrode (4), is respectively placed in necessarily
The interval body both sides of thickness are just to contact, and heating makes solid-state electrolytic solution (1) fully merge, and is packaged into battery.
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