CN102867918B - The method of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal - Google Patents
The method of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal Download PDFInfo
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- CN102867918B CN102867918B CN201210348244.XA CN201210348244A CN102867918B CN 102867918 B CN102867918 B CN 102867918B CN 201210348244 A CN201210348244 A CN 201210348244A CN 102867918 B CN102867918 B CN 102867918B
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Abstract
The present invention relates to the method for a kind of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal, organic solvent mixes with cadmium acetate presoma by the present invention, then adds part P3HT(and gathers 3-hexyl thiophene).Stir 30min at being slowly warming up to 100 DEG C under nitrogen protection, then be heated to 180-200 DEG C, inject the Se source of 180-200 DEG C under keeping temperature stabilization, reaction 10-20min, then naturally cools to room temperature.By the excessive ethanol washing of the precipitation of gained, be separated, namely obtain CdSe/P3HT superstructure hybridized nanometer crystal.The present invention is simple to operate, and without equipment requirement, synthesis temperature is low; Product can be made into " nanocrystalline ink ", for assembling solar battery, and easy scale; The various solvents used are all environmentally friendly, produce without high toxicity accessory substance.
Description
Technical field
The invention belongs to hybrid film solar-energy photo-voltaic cell field of material preparation, particularly a kind of method of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal.
Background technology
Along with the exhaustion of fossil fuel and the aggravation of thing followed global energy crisis, various countries even launch a war for the energy, this while also impel various countries scientist to develop various regenerative resource (as: wind energy, waterpower, luminous energy etc.) to carry out substitute fossil fuels.This also just impels the develop rapidly of solar energy industry, and photovoltaic product emerged in an endless stream in recent years, and the efficiency of product upgrades day by day, and the utilization of luminous energy is subject to unprecedented attention.The utilization of luminous energy have many a little as: more convenient, pollution-free, to environment without destruction, sustainable etc.Therefore the research utilized for light energy conversion seems rather important.
Traditional solar cell due to silicon materials price high, and the research of silica-based solar cell reaches its maturity, and improved efficiency space is little; The research of thin-film solar cells especially technique simple binary thin-film solar cells more seems important.Novel solar battery organic inorganic hybridization thin-film solar cells, because photoelectric conversion efficiency is higher, cost of manufacture is lower, does not have the good characteristics such as performance degradation, is recently subject to extensive concern.Inorganic material CdSe is nanocrystalline is study one of hull cell material the most widely, is subject to the great attention of people.
CdSe is nanocrystalline is that the first is applied to the inorganic nano-crystal of solar cell, it is a kind of typical narrow band gap (1.7eV) semi-conducting material, it has higher energy conversion efficiency relative to the nanocrystalline of other materials, is paid close attention to widely in hybrid solar cell application aspect always.
Very ripe to the research that CdSe is nanocrystalline at present, had nano dot, nanometer rods and four-footed shape nanostructure, but the hydridization CdSe of this kind of superstructure is nanocrystalline not to be occurred.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for a kind of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal, and the method is simple to operate, and without equipment requirement, synthesis temperature is low; Product can be made into " nanocrystalline ink ", for assembling solar battery, and easy scale; The various solvents used are all environmentally friendly, produce without high toxicity accessory substance.
The method of a kind of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal of the present invention, comprise: methyl-sulfoxide is mixed with trichloro-benzenes, cadmium source and poly-3-hexyl thiophene P3HT is added under magnetic agitation, 30min is stirred at being warming up to 100 DEG C under nitrogen protection, be heated to 180-200 DEG C again, inject the selenium source of 180-200 DEG C under temperature stabilization, then react 10-20min, then naturally cool to room temperature; The proportioning of methyl-sulfoxide, trichloro-benzenes, cadmium source, 3-hexyl thiophene P3HT, selenium source is 8mL: 16mL: 0.13-1.3g: 50-100mg: 0.0192-0.0768g; By gained CdSe the precipitation washing of excessive ethanol and drying after being separated, namely obtain CdSe/P3HT hybridized nanometer crystal.
Described cadmium source is cadmium acetate.
Described selenium source is selenium powder.
Described selenium source is that injection adds.
Described low temperature liquid polymerization process is that one-step synthesis method is nanocrystalline based on the CdSe hydridization superstructure of P3HT.
Described CdSe superstructure hybridized nanometer crystal is of a size of 80-200nm.
The present invention has synthesized the CdSe superstructure hybridized nanometer crystal that a kind of size can regulate and control according to reaction volume and reaction time, this hybrid structure is different from traditional single CdSe inorganic material, it take P3HT as part, be conducive to the transmission in electronics and hole in solar cell, thus can be used for the raising of solar battery efficiency.Low for equipment requirements, synthesis temperature is low, simple to operate, easy scale and the method for environmental protection synthesis CdSe/P3HT superstructure hybridized nanometer crystal, for organic inorganic hybridization solar-energy photo-voltaic cell.
beneficial effect
The simple experimental provision of the present invention can prepare CdSe/P3HT superstructure hybridized nanometer crystal, product can be made into " nanocrystalline ink ", can be applicable to organic inorganic hybridization hull cell, this reaction has the advantages such as environmental friendliness, low, the required raw material of synthesis temperature are easy to get, cheap, operating process is easy, and can relatively largely prepare, easy scale; The various solvents used are all environmentally friendly, and producing without high toxicity accessory substance, is a kind of preparation method with boundless application prospect, for the thin-film solar cells preparing high efficiency low cost provides a kind of new method.
Accompanying drawing explanation
Fig. 1 is the TEM picture of CdSe/P3HT superstructure hybridized nanometer crystal prepared by embodiment 4, (a), and (b) is divided into the appearance structure figure under different multiples;
Fig. 2 is the XRD collection of illustrative plates of CdSe/P3HT superstructure hybridized nanometer crystal prepared by embodiment 4, and curve is the XRD collection of illustrative plates of the CdSe/P3HT superstructure hybridized nanometer crystal of preparation, and black vertical line is the standard XRD pattern (JCPDS:08 – 0459) of CdSe;
Fig. 3 is the FTIR collection of illustrative plates of CdSe/P3HT superstructure hybridized nanometer crystal prepared by embodiment 4.
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
The synthesis of hybridized nanometer crystal: measure 8mL methyl-sulfoxide, 16mL trichloro-benzenes puts into round-bottomed flask; 0.13g cadmium acetate is added under magnetic agitation; the P3HT(adding 100mg again gathers 3-hexyl thiophene); and stir; stir 30min at being slowly warming up to 100 DEG C under nitrogen protection afterwards, then be heated to 180 DEG C, under keeping temperature stabilization, inject the trichlorobenzene solution of the selenium source (0.0192) of 180 DEG C; after reaction 10min, naturally cool to room temperature.Gained CdSe is precipitated and is separated with the washing of excessive ethanol, namely obtain CdSe superstructure/P3HT hybridized nanometer crystal.
Embodiment 2
The synthesis of hybridized nanometer crystal: measure 8mL methyl-sulfoxide, 16mL trichloro-benzenes puts into round-bottomed flask; 1.3g cadmium acetate is added under magnetic agitation; the P3HT(adding 100mg again gathers 3-hexyl thiophene); and stir; stir 30min at being slowly warming up to 100 DEG C under nitrogen protection afterwards, then be heated to 190 DEG C, under keeping temperature stabilization, inject the trichlorobenzene solution of the selenium source (0.0768) of 190 DEG C; after reaction 20min, naturally cool to room temperature.Gained CdSe is precipitated and is separated with the washing of excessive ethanol, namely obtain CdSe/P3HT superstructure hybridized nanometer crystal.
Embodiment 3
The synthesis of hybridized nanometer crystal: measure 8mL methyl-sulfoxide, 16mL trichloro-benzenes puts into round-bottomed flask; 1.3g cadmium acetate is added under magnetic agitation; the P3HT(adding 50mg again gathers 3-hexyl thiophene); and stir; 30min is stirred at being slowly warming up to 100 DEG C under nitrogen protection afterwards; be heated to 200 DEG C again, under keeping temperature stabilization, inject the trichlorobenzene solution of the selenium source (0.0768) of 200 DEG C, after reaction 10min, naturally cool to room temperature.Gained CdSe is precipitated and is separated with the washing of excessive ethanol, namely obtain CdSe/P3HT superstructure hybridized nanometer crystal.
Embodiment 4
The synthesis of hydridization hybridized nanometer crystal: measure 8mL methyl-sulfoxide, 16mL trichloro-benzenes puts into round-bottomed flask; 0.13g cadmium acetate is added under magnetic agitation; the P3HT(adding 50mg again gathers 3-hexyl thiophene); and stir; 30min is stirred at being slowly warming up to 100 DEG C under nitrogen protection afterwards; be heated to 180 DEG C again, under keeping temperature stabilization, inject the trichlorobenzene solution of 180 DEG C of selenium sources (0.0192), after reaction 10min, naturally cool to room temperature.Gained CdSe is precipitated and is separated with the washing of excessive ethanol, namely obtain CdSe/P3HT superstructure hybridized nanometer crystal.
Claims (5)
1. the method for a low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal, comprise: methyl-sulfoxide is mixed with trichloro-benzenes, cadmium source and poly-3-hexyl thiophene P3HT is added under magnetic agitation, 30min is stirred at being warming up to 100 DEG C under nitrogen protection, be heated to 180-200 DEG C again, inject the selenium source of 180-200 DEG C under temperature stabilization, then react 10-20min, then naturally cool to room temperature; The proportioning of methyl-sulfoxide, trichloro-benzenes, cadmium source, 3-hexyl thiophene P3HT, selenium source is 8mL:16mL:0.13-1.3g:50-100mg:0.0192-0.0768g; By gained CdSe the precipitation washing of excessive ethanol and drying after being separated, namely obtain CdSe/P3HT hybridized nanometer crystal.
2. the method for a kind of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal according to claim 1, is characterized in that: described cadmium source is cadmium acetate.
3. the method for a kind of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal according to claim 1, is characterized in that: described selenium source is selenium powder.
4. the method for a kind of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal according to claim 1, is characterized in that: described selenium source is that injection adds.
5. the method for a kind of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal according to claim 1, is characterized in that: described CdSe/P3HT superstructure hybridized nanometer crystal is of a size of 80-200nm.
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| CN105200523A (en) * | 2015-08-28 | 2015-12-30 | 内蒙古工业大学 | Method for synthesizing CdSe/P3HT composite nanocrystals by direct growth method |
| RU197989U1 (en) * | 2020-01-16 | 2020-06-10 | Константин Антонович Савин | Photoresistor based on a composite material consisting of a polymer of poly (3-hexylthiophene) and p-type silicon nanoparticles |
| CN111640875A (en) * | 2020-05-15 | 2020-09-08 | 中国地质大学（武汉） | Mixed type photoelectric transistor constructed by poly (3-hexylthiophene) and mercury telluride quantum dots, and preparation method and application thereof |
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| CN102447064B (en) * | 2010-10-06 | 2016-03-23 | 张国庆 | A kind of polymer solar battery and preparation method thereof |
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| Direct Synthesis of CdSe Nanoparticles in Poly(3-hexylthiophene);Smita Dayal,Nikos Kopidakis, Dana C.Olson,David S.Ginley;《J.AM.CHEM.SOC》;20091117;第131卷(第49期);第1页第4段 * |
| In-Situ Growing CdS Single-Crystal Nanorods via P3HT Polymer as a Soft Template for Enhancing Photovoltaic Performance;Hung-Chou Liao, San-Yuan Chen, Dean-Mo Liu;《Macromolecules》;20090807;第42卷(第17期);第2页第2-3段 * |
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