CN102867918A - Method for synthesizing CdSe/P3HT (poly 3-hexylthiophene) superstructure hybrid nanocrystal through a low-temperature liquid phase method - Google Patents
Method for synthesizing CdSe/P3HT (poly 3-hexylthiophene) superstructure hybrid nanocrystal through a low-temperature liquid phase method Download PDFInfo
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- CN102867918A CN102867918A CN201210348244XA CN201210348244A CN102867918A CN 102867918 A CN102867918 A CN 102867918A CN 201210348244X A CN201210348244X A CN 201210348244XA CN 201210348244 A CN201210348244 A CN 201210348244A CN 102867918 A CN102867918 A CN 102867918A
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Abstract
The invention relates to a method for synthesizing a CdSe/P3HT (poly 3-hexylthiophene) superstructure hybrid nanocrystal through a low-temperature liquid phase method, which comprises the following steps: evenly mixing an organic solvent and a cadmium acetate precursor; then adding ligand P3HT; under a nitrogen protective atmosphere, slowly heating to 100 DEG C, and stirring for 30 minutes; then heating to 180-200 DEG C, injecting a Se source of 180-200 DEG C while keeping the temperature stable, and reacting for 10-20 minutes; then naturally cooling to room temperature; and washing the obtained precipitate with excessive ethanol, and separating to obtain the CdSe/P3HT superstructure hybrid nanocrystal. The method has the advantages of simple operation process, no equipment requirement and low synthesis temperature; and the product can be prepared into nanocrystal ink which can be used for the assembly of a solar cell and facilitates the mass production; and the various solvents used are environment-friendly, and no high-toxicity byproduct is produced.
Description
Technical field
The invention belongs to hybrid film solar-energy photo-voltaic cell field of material preparation, particularly the method for the synthetic CdSe/P3HT superstructure hybridized nanometer crystal of a kind of low temperature liquid polymerization process.
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 impels the various countries scientist to develop various regenerative resources (as: wind energy, waterpower, luminous energy etc.) to come substitute fossil fuels.This also just impels the develop rapidly of solar energy industry, and the photovoltaic product emerged in an endless stream in recent years, and the efficient of product is upgraded day by day, and the utilization of luminous energy is subject to unprecedented attention.The utilization of luminous energy have many a bit as: relatively more convenient, pollution-free, without destruction, sustainable etc. to environment.Therefore the research for the light energy conversion utilization seems rather important.
Traditional solar cell is because the silicon materials price is high, and the research of silica-based solar cell reaches its maturity, and the improved efficiency space is little; The thin-film solar cells especially research of the simple binary thin-film solar cells of technique more seems important.Novel solar battery organic inorganic hybridization thin-film solar cells is because photoelectric conversion efficiency is higher, cost of manufacture is lower, do not have the good characteristic such as performance degradation, recently is subject to extensive concern.Inorganic material CdSe is nanocrystalline to be to study the most widely one of hull cell material, is subject to people's great attention.
CdSe is nanocrystalline to be the inorganic nano-crystal that the first is applied to solar cell, it is a kind of typical narrow band gap (1.7eV) semi-conducting material, it has higher energy conversion efficiency with respect to other materials nanocrystalline, is paid close attention to widely in the hybrid solar cell application facet always.
At present very ripe to the nanocrystalline research of CdSe, nano dot, nanometer rods and four-footed shape nanostructure have been arranged, do not occur but the hydridization CdSe of this kind superstructure is nanocrystalline.
Summary of the invention
Technical problem to be solved by this invention provides the method for the synthetic CdSe/P3HT superstructure hybridized nanometer crystal of a kind of low temperature liquid polymerization process, and the method is simple to operate, and without equipment requirement, synthesis temperature is low; Product can be made into " nanocrystalline ink ", is used for the assembling solar battery, easily scale; Employed various solvent is all environmentally friendly, produces without the high toxicity accessory substance.
The method of the synthetic CdSe/P3HT superstructure hybridized nanometer crystal of a kind of low temperature liquid polymerization process of the present invention, comprise: methyl-sulfoxide is mixed with trichloro-benzenes, add cadmium source and poly-3-hexyl thiophene P3HT under the magnetic agitation, under nitrogen protection, be warming up to 100 ℃ of lower 30min of stirring, be heated to again 180-200 ℃, inject 180-200 ℃ selenium source under the temperature stabilization, react again 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; Gained CdSe precipitation with excessive ethanol washing with separates afterwards drying, is namely obtained the 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 method is synthetic 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 be regulated and control according to reaction volume and reaction time, this hybrid structure is different from traditional single CdSe inorganic material, it is take P3HT as part, be conducive to the transmission of electronics and hole in the solar cell, thereby can be used for the raising of solar battery efficiency.Low for equipment requirements, synthesis temperature is low, the synthetic CdSe/P3HT superstructure hybridized nanometer crystal of the method for simple to operate, easy scale and environmental protection, is used for the organic inorganic hybridization solar-energy photo-voltaic cell.
Beneficial effect
The present invention can prepare CdSe/P3HT superstructure hybridized nanometer crystal with simple experimental provision, product can be made into " nanocrystalline ink ", can be applicable to the organic inorganic hybridization hull cell, this reaction has that environmental friendliness, low, the required raw material of synthesis temperature are easy to get, cheap, the advantage such as operating process is easy, and can relatively largely prepare easily scale; Employed various solvent is all environmentally friendly, produces without the high toxicity accessory substance, and be a kind of preparation method with boundless application prospect, for the thin-film solar cells for preparing efficient cheapness provides a kind of new method.
Description of drawings
Fig. 1 is the TEM picture of the CdSe/P3HT superstructure hybridized nanometer crystal of embodiment 4 preparation, (a), (b) is divided into appearance structure figure under the different multiples;
Fig. 2 is the XRD collection of illustrative plates of the CdSe/P3HT superstructure hybridized nanometer crystal of embodiment 4 preparations, 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 x RD collection of illustrative plates (JCPDS:08 – 0459) of CdSe;
Fig. 3 is the FTIR collection of illustrative plates of the CdSe/P3HT superstructure hybridized nanometer crystal of embodiment 4 preparations.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Hybridized nanometer crystal synthetic: measure the 8mL methyl-sulfoxide, the 16mL trichloro-benzenes is put into round-bottomed flask; add the 0.13g cadmium acetate under the magnetic agitation; the poly-3-hexyl thiophene of P3HT(that adds again 100mg); and stir; under nitrogen protection, slowly be warming up to afterwards 100 ℃ of lower 30min of stirring, be heated to again 180 ℃, keep injecting under the temperature stabilization trichloro-benzenes solution of 180 ℃ selenium source (0.0192); behind the reaction 10min, naturally cool to room temperature.Gained CdSe precipitation is separated with excessive ethanol washing, namely obtain CdSe superstructure/P3HT hybridized nanometer crystal.
Embodiment 2
Hybridized nanometer crystal synthetic: measure the 8mL methyl-sulfoxide, the 16mL trichloro-benzenes is put into round-bottomed flask; add the 1.3g cadmium acetate under the magnetic agitation; the poly-3-hexyl thiophene of P3HT(that adds again 100mg); and stir; under nitrogen protection, slowly be warming up to afterwards 100 ℃ of lower 30min of stirring, be heated to again 190 ℃, keep injecting under the temperature stabilization trichloro-benzenes solution of 190 ℃ selenium source (0.0768); behind the reaction 20min, naturally cool to room temperature.Gained CdSe precipitation is separated with excessive ethanol washing, namely obtain CdSe/P3HT superstructure hybridized nanometer crystal.
Embodiment 3
Hybridized nanometer crystal synthetic: measure the 8mL methyl-sulfoxide, the 16mL trichloro-benzenes is put into round-bottomed flask; add the 1.3g cadmium acetate under the magnetic agitation; the poly-3-hexyl thiophene of P3HT(that adds again 50mg); and stir; under nitrogen protection, slowly be warming up to afterwards 100 ℃ of lower 30min of stirring; be heated to again 200 ℃, keep injecting under the temperature stabilization trichloro-benzenes solution of 200 ℃ selenium source (0.0768), naturally cool to room temperature behind the reaction 10min.Gained CdSe precipitation is separated with excessive ethanol washing, namely obtain CdSe/P3HT superstructure hybridized nanometer crystal.
Embodiment 4
Hydridization hybridized nanometer crystal synthetic: measure the 8mL methyl-sulfoxide, the 16mL trichloro-benzenes is put into round-bottomed flask; add the 0.13g cadmium acetate under the magnetic agitation; the poly-3-hexyl thiophene of P3HT(that adds again 50mg); and stir; under nitrogen protection, slowly be warming up to afterwards 100 ℃ of lower 30min of stirring; be heated to again 180 ℃, keep injecting under the temperature stabilization trichloro-benzenes solution of 180 ℃ of selenium sources (0.0192), naturally cool to room temperature behind the reaction 10min.Gained CdSe precipitation is separated with excessive ethanol washing, namely obtain CdSe/P3HT superstructure hybridized nanometer crystal.
Claims (5)
1. the method for the synthetic CdSe/P3HT superstructure hybridized nanometer crystal of a low temperature liquid polymerization process, comprise: methyl-sulfoxide is mixed with trichloro-benzenes, add cadmium source and poly-3-hexyl thiophene P3HT under the magnetic agitation, under nitrogen protection, be warming up to 100 ℃ of lower 30min of stirring, be heated to again 180-200 ℃, inject 180-200 ℃ selenium source under the temperature stabilization, react again 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; Gained CdSe precipitation with excessive ethanol washing with separates afterwards drying, is namely obtained the CdSe/P3HT hybridized nanometer crystal.
2. a kind of low temperature liquid polymerization process according to claim 1 synthesizes the method for CdSe/P3HT superstructure hybridized nanometer crystal, and it is characterized in that: described cadmium source is cadmium acetate.
3. a kind of low temperature liquid polymerization process according to claim 1 synthesizes the method for CdSe/P3HT superstructure hybridized nanometer crystal, and it is characterized in that: described selenium source is selenium powder.
4. a kind of low temperature liquid polymerization process according to claim 1 synthesizes the method for CdSe/P3HT superstructure hybridized nanometer crystal, it is characterized in that: described selenium source is that injection adds.
5. a kind of low temperature liquid polymerization process according to claim 1 synthesizes the method for CdSe/P3HT superstructure hybridized nanometer crystal, and it is characterized in that: described CdSe superstructure hybridized nanometer crystal is of a size of 80-200nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| US20080149174A1 (en) * | 2006-12-26 | 2008-06-26 | Fang-Chung Chen | Polymer solar cell and manufacturing method thereof |
| US20120061659A1 (en) * | 2009-05-27 | 2012-03-15 | Sumitomo Chemical Company, Limited | Organic photoelectric conversion element |
| CN102447064A (en) * | 2010-10-06 | 2012-05-09 | 曾永斌 | Polymer solar cell and preparation method thereof |
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Patent Citations (3)
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| US20080149174A1 (en) * | 2006-12-26 | 2008-06-26 | Fang-Chung Chen | Polymer solar cell and manufacturing method thereof |
| US20120061659A1 (en) * | 2009-05-27 | 2012-03-15 | Sumitomo Chemical Company, Limited | Organic photoelectric conversion element |
| CN102447064A (en) * | 2010-10-06 | 2012-05-09 | 曾永斌 | Polymer solar cell and preparation method thereof |
Non-Patent Citations (4)
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| HUNG-CHOU LIAO, SAN-YUAN CHEN, DEAN-MO LIU: "In-Situ Growing CdS Single-Crystal Nanorods via P3HT Polymer as a Soft Template for Enhancing Photovoltaic Performance", 《MACROMOLECULES》 * |
| JINGJING XU, JIANCHEN HU, XINFENG LIU, XIAOHUI QIU, ZHIXIANG WEI: "Stepwise Self-Assembly of P3HT/CdSe Hybrid Nanowires with Enhanced Photoconductivity", 《MACROMOL. RAPID COMMUN.》 * |
| QINGLING ZHANG, THOMAS P. RUSSELL, TODD EMRICK: "Synthesis and Characterization of CdSe Nanorods Functionalized with Regioregular Poly(3-hexylthiophene)", 《CHEM. MATER.》 * |
| SMITA DAYAL,NIKOS KOPIDAKIS, DANA C.OLSON,DAVID S.GINLEY: "Direct Synthesis of CdSe Nanoparticles in Poly(3-hexylthiophene)", 《J.AM.CHEM.SOC》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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