CN104377036A - Method for preparing AgInS2 quantum dot sensitized TiO2 photoelectrode with In2S3 used as buffer layer - Google Patents

Method for preparing AgInS2 quantum dot sensitized TiO2 photoelectrode with In2S3 used as buffer layer Download PDF

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CN104377036A
CN104377036A CN201410606158.3A CN201410606158A CN104377036A CN 104377036 A CN104377036 A CN 104377036A CN 201410606158 A CN201410606158 A CN 201410606158A CN 104377036 A CN104377036 A CN 104377036A
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quantum dot
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CN104377036B (en
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李耀刚
王远强
王宏志
张青红
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Donghua University
National Dong Hwa University
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Abstract

The invention relates to a method for preparing an AgInS2 quantum dot sensitized TiO2 photoelectrode with In2S3 used as a buffer layer. The method comprises the steps that (1) a TiO2 porous membrane is prepared on an FTO conducting glass matrix; (2) an Ag2S quantum dot sensitized TiO2 electrode is obtained through the continuous ionic adsorption reaction method; (3) on the Ag2S quantum dot/TiO2 electrode, the chemical bath deposition and reaction of In2S3 is used for synthesizing the AgInS2 quantum dot sensitized TiO2 photoelectrode with In2S3 used as the buffer layer in a one-step in-situ mode. The method is simple in preparing process and low in requirement for equipment, and common organic solvents used for semiconductor quantum dot synthesis are not involved; the photoelectrode is composed of AgInS2, In2S3 and TiO2 which are low in toxicity, has high photoelectric response performance when being applied to solar cells, and has potential application prospects.

Description

A kind of In 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole
Technical field
The invention belongs to quantum dot sensitized TiO 2optoelectronic pole field, particularly a kind of In 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole.
Background technology
At present unprecedented fieriness is entered to the research of semiconductor-quantum-point, the center of its application at photoelectric field present convergence especially.But obtaining main research progress quantum dot used (QDs) is at present the elements such as Cd, Pb, do not meet the current strategic requirement to environmental protection, environmental friendliness shaped material, thus limit its application in various fields.Novel tertiary I-II-VI race semiconductor-quantum-point has not only possessed the excellent properties that quantum dot has, and simultaneously with the advantage of its low toxic and environment-friendly, is expected to replace the application of Cd system quantum dot in each field.AgInS 2semiconductor is the ternary chalcogenide thing of direct band gap, and form the yellow copper structure of Tetragonal during low temperature, band gap is 1.87eV, and form orthorhombic phase structure during high temperature, its band gap is about 2.03eV, and the Exciton Bohr Radius of body material is about 5.5nm; It has good stability to heat and electricity, has higher absorption coefficient and hypotoxicity, in biological fluorescent labelling, LED, nonlinear device, visible light catalytic and area of solar cell, show huge application prospect.
Solar energy is one of energy being hopeful most to be used widely in 21 century, in it utilizes, solar cell generating attracts most attention, and it has and transforms that link is few, the resource amount of containing is inexhaustible, energy quality is high, the construction period is short, generation mode is close to advantages such as zero discharges.With nano-TiO 2material has caused the extensive concern of people as dye-sensitized solar cells (DSSCs) research of optoelectronic pole, be generally considered second generation solar cell, traditional solar cell will be replaced gradually, become the emphasis of solar cell development from now on.But some factors are as higher in cost of dye, dyestuff light degradation easily occurs and causes that efficiency reduces, the absorption spectrum of dyestuff is narrower, the absorption of dyestuff multilayer is unfavorable for that the problems such as electric transmission constrain the development of DSSCs.Therefore, find a kind of novel photosensitive materials and replace dyestuff, have important meaning to the development of solar cell.The inorganic semiconductor material of narrow band gap can replace dyestuff as sensitizer, if by these controls of material within the scope of quantum effect, then become quantum dot sensitizer.
The quantum dot sensitized TiO of I-II-VI race 2the preparation of optoelectronic pole is mainly based on two kinds of methods: one is pre-synthesis quantum dot, disperses in the solution after purifying, by nanoporous TiO 2film immerses in solution and adsorbs quantum dot.The quantum dot size synthesized by this method is even, purity is high, but because quantum dot is by physisorption and TiO 2film combines, the less stable of battery; Relate to more organic solvent in quantum dot building-up process, not only cause environmental pollution, also make preparation cost increase; Two is at TiO 2on film, " original position " synthesizes quantum dot sensitized optoelectronic pole, and as high-temperature spray pyrolysismethod, high temperature vulcanized method electrochemical deposition method, vapour deposition process etc., this class methods preparation condition is harsh and quantum dot purity that is that obtain is lower.I-II-VI race quantum dot and TiO 2lattice does not mate, in order to improve quantum dot and TiO 2interracial contact, conventional In 2s 3, Cu 2s, In 2se 3deng as interface resilient coating, thus electron recombination speed can be suppressed, improve battery performance.In 2s 3resilient coating obtains by the method such as chemical bath deposition, high temperature plated film mostly on pre-synthesis electrode, and preparation technology is more complicated, cost is also higher.
Summary of the invention
The invention provides a kind of In 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, the method preparation technology is simple, lower to the requirement of equipment, do not relate to the conventional organic solvent of semiconductor-quantum-point synthesis; Optoelectronic pole is by the lower AgInS of toxicity 2, In 2s 3and TiO 2form, application has stronger photoelectric response performance in solar cells, has potential application prospect.
A kind of In of the present invention 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, comprising:
(1) by TiO 2nano-powder roasting, obtains pretreated TiO 2nano-powder; TiO after the pre-treatment 2in nano-powder, add water, absolute ethyl alcohol, acetic acid and binding agent, ball milling (6 ~ 36h), (30 DEG C ~ 80 DEG C) decompression distillation concentrates, and obtains TiO 2viscous paste; Then be coated on FTO electro-conductive glass matrix, roasting, obtains TiO on glass basis 2perforated membrane;
(2) by TiO 2perforated membrane is immersed in Ag +in the aqueous solution, after deionized water, ethanol washing, put into S 2-impregnation in the aqueous solution, then with deionized water, ethanol washing, after continuous ion adsorbing method SILAR circulates (2 ~ 14 times), obtain Ag 2s-QDs sensitization TiO 2electrode;
(3) by the In containing indium salt, sulphur source, complexing agent 2s 3presoma homogeneous phase aqueous solution joins in water heating kettle, by Ag 2s-QDs sensitization TiO 2electrode is placed in solution, is heated to 80 ~ 200 DEG C after sealing, hydro-thermal 2 ~ 10h, uses deionized water, absolute ethanol washing, naturally dry and obtain In after being cooled to room temperature 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2optoelectronic pole.
TiO in described step (1) 2the particle diameter of nano-powder is 20 ~ 50 nanometers, and crystal formation is one or both in anatase titanium dioxide or rutile-type.
Binding agent in described step (1) is one or more in polyethylene glycol, polyvinyl pyrrole, polyvinyl alcohol, poly-ethyl cellulose, binding agent and TiO 2the mass ratio of powder is 0.5:1 ~ 10:1.
Coating method in described step (1) is silk screen printing or knife coating; Coating layer thickness is 4 μm ~ 20 μm, and coating size is 0.5 ~ 6cm 2.
TiO in described step (1) 2the roasting of nano-powder is roasting 1 ~ 10h at 200 DEG C ~ 600 DEG C; TiO 2the roasting of viscous paste is roasting 1 ~ 6h at 200 DEG C ~ 500 DEG C.
Ag in described step (2) +be selected from one or more in silver nitrate, silver sulfate, silver acetate, S 2-for one or both in vulcanized sodium, NaHS.
Ag in described step (2) +the molar concentration of the aqueous solution is 0.001 ~ 0.5mol/L, S 2-the molar concentration of the aqueous solution is 0.001 ~ 0.5mol/L.
At Ag in described step (2) +the aqueous solution or S 2-the dip time of the aqueous solution is 10 ~ 120s.
Indium salt in described step (3) is selected from one or more in indium nitrate, indium sulfate, indium acetate; Sulphur source is selected from one or more in thioacetyl, thiocarbamide, vulcanized sodium, mercaptopropionic acid; Complexing agent is selected from one or more in polyvinylpyrrolidone, ethylenediamine tetra-acetic acid, citric acid, nitrilotriacetic acid.
In in described step (3) 2s 3in presoma homogeneous phase aqueous solution, the molar concentration of indium salt is 0.001 ~ 0.1mol/L, and the molar concentration in sulphur source is 0.004 ~ 0.4mol/L, and the molar concentration of complexing agent is 0.004 ~ 1.0mol/L.
beneficial effect
The present invention is simple for technique, and cost is lower, not etching apparatus, especially prepares in aqueous phase system, does not relate to the organic solvent that quantum dot synthesis is conventional, can meet the requirement of environmental protection in course of reaction; The solar cell that prepared optoelectronic pole becomes electrode assembling with polysulfide electrolyte, platinum, has stronger photoelectric response performance, has potential application prospect under standard analog sunlight conditions.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Take 2.0g nano-TiO 2powder (mixed crystal type, the weight ratio of anatase and rutile is approximately 80/20), puts into Muffle furnace, roasting 3h at 200 DEG C.TiO 2the particle diameter of nano-powder is 25 nanometers.Pretreated nano-TiO is added in 60mL absolute ethyl alcohol 2powder, stirs, then adds 1.0g deionized water, 0.5g acetic acid and 6.0g and gather ethyl cellulose.After ball milling 24h, remove excessive ethanol with Rotary Evaporators 50 DEG C of decompression distillation, obtain TiO 2viscous paste.By the TiO prepared 2viscous paste knife coating is coated on the glass basis after cleaning, and coating layer thickness is about 10 μm, and coating size is 3cm 2.Then roasting 1h at 480 DEG C, heating rate is 1 DEG C/min, obtains TiO on glass basis 2perforated membrane.
Porous TiO 2electrode is immersed in the 0.02mol/L silver acetate aqueous solution after 30s, with deionized water, ethanol washing, then puts into 0.05mol/L sodium sulfide solution and floods 30s, then wash with deionized water, ethanol.Ag is obtained after 6 SILAR circulations 2s-QDs/TiO 2electrode.
Join in water heating kettle by 0.02mol/L indium acetate, 0.08mol/L thiocarbamide, 0.12mol/L citric acid precursor water solution, circulate 6 SILAR the Ag obtained 2s-QDs/TiO 2electrode is placed in solution, is heated to 150 DEG C, hydro-thermal 3h after sealing, uses deionized water, absolute ethanol washing, naturally dry and obtain In after being cooled to room temperature 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2optoelectronic pole.
The solar cell that prepared optoelectronic pole becomes electrode assembling with polysulfide electrolyte, platinum, under standard analog sunlight conditions, photoelectric conversion efficiency and density of photocurrent are respectively 0.70%, 7.87mA/cm 2.
Embodiment 2
Take 2.0g nano-TiO 2powder (mixed crystal type, the weight ratio of anatase and rutile is approximately 80/20), puts into Muffle furnace, roasting 3h at 200 DEG C.TiO 2the particle diameter of nano-powder is 25 nanometers.Pretreated nano-TiO is added in 60mL absolute ethyl alcohol 2powder, stirs, then adds 1.0g deionized water, 0.5g acetic acid and 6.0g and gather ethyl cellulose.After ball milling 24h, remove excessive ethanol with Rotary Evaporators 50 DEG C of decompression distillation, obtain TiO 2viscous paste.By the TiO prepared 2viscous paste knife coating is coated on the glass basis after cleaning, and coating layer thickness is about 8 μm, and coating size is 3cm 2.Then roasting 1h at 480 DEG C, heating rate is 1 DEG C/min, obtains TiO on glass basis 2perforated membrane.
Porous TiO 2electrode is immersed in 0.02mol/L silver nitrate aqueous solution after 30s, with deionized water, ethanol washing, then puts into 0.05mol/L sodium sulfide solution and floods 30s, then wash with deionized water, ethanol.Ag is obtained after 4 SILAR circulations 2s-QDs/TiO 2electrode.
Join in water heating kettle by the precursor water solution of 0.01mol/L inidum chloride, 0.04mol/L thioacetamide, 0.06mol/L citric acid, circulate 4 SILAR the Ag obtained 2s-QDs/TiO 2electrode is placed in solution, is heated to 150 DEG C, hydro-thermal 3h after sealing, uses deionized water, absolute ethanol washing, naturally dry and obtain In after being cooled to room temperature 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2optoelectronic pole.
The solar cell that prepared optoelectronic pole becomes electrode assembling with polysulfide electrolyte, platinum, under standard analog sunlight conditions, photoelectric conversion efficiency and density of photocurrent are respectively 0.54%, 6.82mA/cm 2.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claim.

Claims (10)

1. an In 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, comprising:
(1) by TiO 2nano-powder roasting, obtains pretreated TiO 2nano-powder; TiO after the pre-treatment 2in nano-powder, add water, absolute ethyl alcohol, acetic acid and binding agent, ball milling, decompression distillation concentrates, and obtains TiO 2viscous paste; Then be coated on FTO electro-conductive glass matrix, roasting, obtains TiO on glass basis 2perforated membrane;
(2) by TiO 2perforated membrane is immersed in Ag +in the aqueous solution, after deionized water, ethanol washing, put into S 2-impregnation in the aqueous solution, then with deionized water, ethanol washing, after continuous ion adsorbing method SILAR circulates, obtain Ag 2s-QDs sensitization TiO 2electrode;
(3) by the In containing indium salt, sulphur source, complexing agent 2s 3presoma homogeneous phase aqueous solution joins in water heating kettle, by Ag 2s-QDs sensitization TiO 2electrode is placed in solution, is heated to 80 ~ 200 DEG C after sealing, hydro-thermal 2 ~ 10h, uses deionized water, absolute ethanol washing, naturally dry and obtain In after being cooled to room temperature 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2optoelectronic pole.
2. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: the TiO in described step (1) 2the particle diameter of nano-powder is 20 ~ 50 nanometers.
3. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: the binding agent in described step (1) is one or more in polyethylene glycol, polyvinyl pyrrole, polyvinyl alcohol, poly-ethyl cellulose, binding agent and TiO 2the mass ratio of powder is 0.5:1 ~ 10:1.
4. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: the coating method in described step (1) is silk screen printing or knife coating; Coating layer thickness is 4 μm ~ 20 μm, and coating size is 0.5 ~ 6cm 2.
5. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: the TiO in described step (1) 2the roasting of nano-powder is roasting 1 ~ 10h at 200 DEG C ~ 600 DEG C; TiO 2the roasting of viscous paste is roasting 1 ~ 6h at 200 DEG C ~ 500 DEG C.
6. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: Ag in described step (2) +be selected from one or more in silver nitrate, silver sulfate, silver acetate, S 2-for one or both in vulcanized sodium, NaHS.
7. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: Ag in described step (2) +the molar concentration of the aqueous solution is 0.001 ~ 0.5mol/L, S 2-the molar concentration of the aqueous solution is 0.001 ~ 0.5mol/L.
8. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: at Ag in described step (2) +the aqueous solution or S 2-the dip time of the aqueous solution is 10 ~ 120s.
9. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: the indium salt in described step (3) is selected from one or more in indium nitrate, indium sulfate, indium acetate; Sulphur source is selected from one or more in thioacetyl, thiocarbamide, vulcanized sodium, mercaptopropionic acid; Complexing agent is selected from one or more in polyvinylpyrrolidone, ethylenediamine tetra-acetic acid, citric acid, nitrilotriacetic acid.
10. a kind of according to claim 1 2s 3for the AgInS of resilient coating 2quantum dot sensitized TiO 2the preparation method of optoelectronic pole, is characterized in that: the In in described step (3) 2s 3in presoma homogeneous phase aqueous solution, the molar concentration of indium salt is 0.001 ~ 0.1mol/L, and the molar concentration in sulphur source is 0.004 ~ 0.4mol/L, and the molar concentration of complexing agent is 0.004 ~ 1.0mol/L.
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CN112466982A (en) * 2020-11-03 2021-03-09 中国科学院海洋研究所 Nanosheet array composite photoelectric material for photoelectrochemical cathodic protection, and preparation and application thereof
CN115125539A (en) * 2022-05-31 2022-09-30 中国科学院海洋研究所 Multiphase composite photoelectric material for photoinduced cathode protection and preparation and application thereof
CN115125539B (en) * 2022-05-31 2023-08-22 中国科学院海洋研究所 Multiphase composite photoelectric material for photocathode protection and preparation and application thereof

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