CN105914043A - Method for preparing photo-anode including graphene - Google Patents
Method for preparing photo-anode including graphene Download PDFInfo
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- CN105914043A CN105914043A CN201610540350.6A CN201610540350A CN105914043A CN 105914043 A CN105914043 A CN 105914043A CN 201610540350 A CN201610540350 A CN 201610540350A CN 105914043 A CN105914043 A CN 105914043A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000006256 anode slurry Substances 0.000 claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 27
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 14
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 14
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 14
- 230000010355 oscillation Effects 0.000 claims abstract description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 14
- -1 polyoxyethylene Polymers 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 26
- 239000011521 glass Substances 0.000 claims description 26
- 229910052707 ruthenium Inorganic materials 0.000 claims description 26
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 16
- ZVZFHCZCIBYFMZ-UHFFFAOYSA-N 6-methylheptoxybenzene Chemical compound CC(C)CCCCCOC1=CC=CC=C1 ZVZFHCZCIBYFMZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 238000010926 purge Methods 0.000 claims description 13
- 238000007650 screen-printing Methods 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 13
- 238000002791 soaking Methods 0.000 claims description 13
- 238000005507 spraying Methods 0.000 claims description 13
- 239000000758 substrate Substances 0.000 claims description 13
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-UHFFFAOYSA-N 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Classifications
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- 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
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
-
- 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
- H01G9/2045—Light-sensitive devices comprising a semiconductor electrode comprising elements of the fourth group of the Periodic System (C, Si, Ge, Sn, Pb) with or without impurities, e.g. doping materials
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- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Hybrid Cells (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention relates to a method for preparing a photo-anode including graphene. The method comprises the following steps of: (1), putting 5.1 g of titanium dioxide in a mortar to sufficiently grind, adding proper distilled water, 3.5 ml of acetone solution (the volume percentage of the solution is 10%), 2 ml of ethanol solution (the volume percentage of the solution is 15%), 1 g of polyethylene glycol para-isooctyl phenyl ether and 2 g of polyoxyethylene glycol, uniformly mixing after performing ultrasonic oscillation for 30 min so as to obtain anode slurry, and putting the configured anode slurry in a refrigerator to store and be standby.
Description
Technical field
The present invention relates to the preparation method of a kind of light anode containing Graphene.
Background technology
The preparation process of the light anode containing Graphene in prior art is sufficiently complex, and easily reunites in sintering process, affects general effect.
Summary of the invention
The present invention proposes the preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.1g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
The ability that the light anode containing Graphene being obtained by this method generates photoelectric current is strong, and stable performance, and the present invention is simple, it is easy to promote.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.1g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 2
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.2g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 3
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.3g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 4
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.4g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 5
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.5g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 6
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.6g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 7
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.7g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 8
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.8g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 9
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.9g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 10
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 6g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Embodiment 11
The preparation method of a kind of light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5g is put in mortar and is fully ground, add appropriate distilled water, (volume percent of this solution is 10% to the acetone soln of Nml, N chooses from following numerical value: 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4.0), (volume percent of this solution is 15% to the ethanol solution of M ml, M chooses from following numerical value: 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4.0), 1 gram of Polyethylene Glycol is to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
Claims (2)
1. a preparation method for the light anode containing Graphene, comprises the steps:
Step 1: the titanium dioxide of 5.1g is put in mortar and is fully ground, add appropriate distilled water, the acetone soln (volume percent of this solution is 10%) of 3.5ml, the ethanol solution (volume percent of this solution is 15%) of 2ml, 1 gram of Polyethylene Glycol to isooctyl phenyl ether, 2 grams of polyoxyethylene glycol, after sonic oscillation 30 minutes, mix homogeneously obtains anode slurry, and the anode slurry configured is positioned in refrigerator and stores for future use；
Step 2: the FTO glass of conduction cuts cleaned in advance, by spraying coating process deposited oxide graphene film in ITO electro-conductive glass substrate, graphene film is obtained again through electrochemical reduction, then put it in titanium tetrachloride solution, standing 1.5 hours at a temperature of 600C, taking-up subsequently is dried standby；
Step 3: use the method for silk screen printing to be imprinted on by above-mentioned slurry on the FTO conducting surface after titanium tetrachloride processes, place after 10 minutes in exsiccator, put in Muffle furnace and be calcined, temperature impose a condition for: keep 25 minutes under the conditions of 3200；
Step 4: take out after being down to room temperature, and put it in titanium disulfide solution, stand 1 hour at a temperature of 800C, taking-up subsequently is dried standby；
Step 5: put in Muffle furnace and be calcined 40 minutes under the conditions of 5000C；
Step 6: put into two-tetrabutylammonium-bis-(isothiocyano) double (2 of 0.0004mol/L, 2'-bipyridyl-4,4'-dicarboxyl) ruthenium (is commonly called as N719 ruthenium dye, molecular formula: C58H86N8O8RuS2) soaking at room temperature 24 hours in solution, i.e. obtain titanium dioxide photo anode after ethanol purge.
2. the ability that the light anode containing Graphene being obtained by this method generates photoelectric current is strong, and stable performance, and the present invention is simple, it is easy to promote.
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| CN102142317A (en) * | 2011-01-14 | 2011-08-03 | 天津师范大学 | Solar battery with graphite interface layer and manufacturing method thereof |
| CN103700502A (en) * | 2013-12-30 | 2014-04-02 | 中国科学院上海硅酸盐研究所 | Method for preparing titanium dioxide photo-anode of DSSC (Dye-Sensitized Solar Cell) |
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| CN102142317A (en) * | 2011-01-14 | 2011-08-03 | 天津师范大学 | Solar battery with graphite interface layer and manufacturing method thereof |
| CN103700502A (en) * | 2013-12-30 | 2014-04-02 | 中国科学院上海硅酸盐研究所 | Method for preparing titanium dioxide photo-anode of DSSC (Dye-Sensitized Solar Cell) |
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| T.UMEBAYASHI: "Band gap narrowing of titanium dioxide by sulfur doping", 《APPLIED PHYSICS LETTERS》 * |
| 李峰: "非金属自掺杂（S，C）-TiO2的制备与光催化性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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