CN102867918B - The method of low temperature liquid polymerization process synthesis CdSe/P3HT superstructure hybridized nanometer crystal - Google Patents

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

Method for Synthesizing CdSe/P3HT Superstructure Hybrid Nanocrystals by Low Temperature Liquid Phase Method

technical field

The invention belongs to the field of hybrid thin-film solar photovoltaic cell material preparation, in particular to a method for synthesizing CdSe/P3HT superstructure hybrid nanocrystals by a low-temperature liquid phase method.

Background technique

With the depletion of fossil fuels and the subsequent intensification of the global energy crisis, countries even waged wars for energy, which also prompted scientists from various countries to develop and utilize various renewable energy sources (such as: wind energy, water power, light energy, etc.) to replace Fossil fuels. This also promotes the rapid development of the solar energy industry. In recent years, solar photovoltaic products have emerged one after another, and the efficiency of the products has been updated day by day. The utilization of light energy has received unprecedented attention. The use of light energy has many advantages such as: more convenient, no pollution, no damage to the environment, sustainable and so on. Therefore, it is very important to study the conversion and utilization of light energy.

Due to the high price of silicon materials for traditional solar cells, and the research on silicon-based solar cells has become increasingly mature, there is little room for efficiency improvement; the research on thin-film solar cells, especially binary thin-film solar cells with simple processes, is even more important. New solar cells Organic-inorganic hybrid thin-film solar cells have recently received widespread attention due to their high photoelectric conversion efficiency, low manufacturing cost, and no performance degradation. The inorganic material CdSe nanocrystal is one of the most extensively researched thin-film battery materials, and has been highly valued by people.

CdSe nanocrystals are the first inorganic nanocrystals used in solar cells. It is a typical narrow band gap (1.7eV) semiconductor material. It has higher energy conversion efficiency than nanocrystals of other materials. In hybridization The application of solar cells has been widely concerned.

At present, the research on CdSe nanocrystals is very mature, and there are nanodots, nanorods and tetrapod nanostructures, but the hybrid CdSe nanocrystals of this kind of superstructure have not appeared.

Contents of the invention

The technical problem to be solved by the present invention is to provide a method for synthesizing CdSe/P3HT superstructure hybrid nanocrystals by a low-temperature liquid phase method, which is simple to operate, requires no equipment, and has low synthesis temperature; the product can be made into "nanocrystalline ink" , used to assemble solar cells, easy to scale; all solvents used are environmentally friendly, and no highly toxic by-products are produced.

A method for synthesizing CdSe/P3HT superstructure hybrid nanocrystals by a low-temperature liquid phase method of the present invention comprises: mixing dimethyl sulfoxide and trichlorobenzene, adding a cadmium source and poly-3-hexylthiophene P3HT under magnetic stirring, and Under nitrogen protection, heat up to 100°C and stir for 30 minutes, then heat to 180-200°C, inject selenium source at 180-200°C under stable temperature, react for 10-20 minutes, and then cool to room temperature naturally; dimethyl sulfoxide, trichloro The ratio of benzene, cadmium source, 3-hexylthiophene P3HT, and selenium source is 8mL: 16mL: 0.13-1.3g: 50-100mg: 0.0192-0.0768g; the obtained CdSe precipitate is washed with excess ethanol and dried after separation, that is CdSe/P3HT hybrid nanocrystals were obtained.

The cadmium source is cadmium acetate.

The selenium source is selenium powder.

The selenium source is added by injection.

The low-temperature liquid phase method is a one-step method for synthesizing P3HT-based CdSe hybrid superstructure nanocrystals.

The size of the CdSe superstructure hybrid nanocrystal is 80-200nm.

The present invention synthesizes a CdSe superstructure hybrid nanocrystal whose size can be regulated according to the amount of reactants and reaction time. This hybrid structure is different from the traditional single CdSe inorganic material. It uses P3HT as a ligand, which is beneficial to solar cells. The transport of electrons and holes can be used to improve the efficiency of solar cells. The CdSe/P3HT superstructure hybrid nanocrystal is synthesized by a method with low equipment requirements, low synthesis temperature, simple operation, easy scale-up and environmental protection, which can be used for organic-inorganic hybrid solar photovoltaic cells.

Beneficial effect

The invention can prepare CdSe/P3HT superstructure hybrid nanocrystals with a simple experimental device, and the product can be made into "nanocrystal ink", which can be applied to organic-inorganic hybrid thin-film batteries. The reaction has the advantages of environmental friendliness, low synthesis temperature, The required raw materials are easy to obtain, low in price, easy to operate, etc., and can be prepared in large quantities, and are easy to scale up; the various solvents used are environmentally friendly, and no highly toxic by-products are produced. It is a very wide range of applications. The promising preparation method provides a new method for preparing high-efficiency and cheap thin-film solar cells.

Description of drawings

Figure 1 is a TEM picture of the CdSe/P3HT superstructure hybrid nanocrystal prepared in Example 4, (a), (b) are divided into morphology and structure diagrams under different multiples;

Fig. 2 is the XRD spectrum of the CdSe/P3HT superstructure hybrid nanocrystal prepared in embodiment 4, and the curve is the XRD spectrum of the prepared CdSe/P3HT superstructure hybrid nanocrystal, and the black vertical line is the standard XRD spectrum of CdSe (JCPDS: 08–0459);

Fig. 3 is the FTIR spectrum of the CdSe/P3HT superstructure hybrid nanocrystal prepared in Example 4.

Detailed ways

Below in conjunction with specific embodiment, further illustrate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Example 1

Synthesis of hybrid nanocrystals: Measure 8mL dimethyl sulfoxide and 16mL trichlorobenzene into a round bottom flask, add 0.13g cadmium acetate under magnetic stirring, then add 100mg of P3HT (poly-3-hexylthiophene), and stir Uniform, then slowly heated up to 100°C under nitrogen protection and stirred for 30 minutes, then heated to 180°C, and injected a trichlorobenzene solution of selenium source (0.0192) at 180°C while keeping the temperature stable, reacted for 10 minutes, and cooled naturally to room temperature. The obtained CdSe precipitate was washed and separated with excess ethanol to obtain the CdSe superstructure/P3HT hybrid nanocrystal.

Example 2

Synthesis of hybrid nanocrystals: Measure 8mL dimethyl sulfoxide and 16mL trichlorobenzene into a round bottom flask, add 1.3g cadmium acetate under magnetic stirring, then add 100mg P3HT (poly-3-hexylthiophene), and stir Uniform, then slowly heated up to 100°C under nitrogen protection and stirred for 30 minutes, then heated to 190°C, and injected a trichlorobenzene solution of selenium source (0.0768) at 190°C while keeping the temperature stable, reacted for 20 minutes, and cooled naturally to room temperature. The obtained CdSe precipitate was washed and separated with excess ethanol to obtain CdSe/P3HT superstructure hybrid nanocrystal.

Example 3

Synthesis of hybrid nanocrystals: Measure 8mL dimethyl sulfoxide and 16mL trichlorobenzene into a round bottom flask, add 1.3g cadmium acetate under magnetic stirring, then add 50mg P3HT (poly-3-hexylthiophene), and stir Uniform, then slowly heated up to 100°C under nitrogen protection and stirred for 30 minutes, then heated to 200°C, and injected a trichlorobenzene solution of selenium source (0.0768) at 200°C while keeping the temperature stable, reacted for 10 minutes and then naturally cooled to room temperature. The obtained CdSe precipitate was washed and separated with excess ethanol to obtain CdSe/P3HT superstructure hybrid nanocrystal.

Example 4

Synthesis of hybrid hybrid nanocrystals: measure 8mL dimethyl sulfoxide and 16mL trichlorobenzene into a round bottom flask, add 0.13g cadmium acetate under magnetic stirring, then add 50mg of P3HT (poly-3-hexylthiophene), Stir evenly, then slowly heat up to 100°C under nitrogen protection and stir for 30 minutes, then heat to 180°C, inject a trichlorobenzene solution of 180°C selenium source (0.0192) while keeping the temperature stable, react for 10 minutes, and then naturally cool to room temperature. The obtained CdSe precipitate was washed and separated with excess ethanol to obtain CdSe/P3HT superstructure hybrid nanocrystal.

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.