Method for preparing graphene and titanium dioxide composite material by vapor phase reduction method

A technology of titanium dioxide and composite materials, applied in the direction of titanium dioxide, graphene, titanium oxide/hydroxide, etc., to achieve the effect of increasing porosity, improving electrical conductivity, and excellent performance

Active Publication Date: 2013-01-16
NANJING UNIV OF TECH
2 Cites 11 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0005] At present, there are few methods to make graphene and titanium dioxide into a uniform composi...
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Abstract

The invention relates to a method for preparing a graphene and titanium dioxide composite material by a vapor phase reduction method. The method comprises the following steps of: acidizing titanium dioxide powder; adding a prepared graphene aqueous solution into a titanium dioxide solution which is acidized; adding an organic solvent, and stirring to obtain slurry; adding a curing agent and high-molecular polymer cured slurry, and distilling to obtain concentrated graphene composite titanium dioxide slurry; printing the slurry on a substrate by a silk screen; and heating for reducing under the action of reducing gas to obtain the graphene and titanium dioxide composite material. The composite material obtained by the method provides an excellent electrode material for the subsequent manufacturing of dye-sensitized batteries, quantum dot sensitized batteries and photoelectrocatalysis equipment. According to the method, a preparation process is simple and convenient, and the novel composite material with high performance is provided for the field of solar battery materials in the future.

Application Domain

Technology Topic

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  • Method for preparing graphene and titanium dioxide composite material by vapor phase reduction method
  • Method for preparing graphene and titanium dioxide composite material by vapor phase reduction method
  • Method for preparing graphene and titanium dioxide composite material by vapor phase reduction method

Examples

  • Experimental program(10)

Example Embodiment

[0023] Example 1
[0024] 1) Acidification treatment: Titanium dioxide powder is pretreated. The acid solution is nitric acid with a mass concentration of 10%, and the acid solution mass is 6g. Add dropwise to 6g titanium dioxide powder. The average particle size of titanium dioxide is 1nm.
[0025] (2) Prepare the slurry: prepare a graphene oxide solution with a concentration of 0.1g/L and add it dropwise to the titanium dioxide slurry in step (1). After the graphene oxide solution is added to 60L, add 6g of methanol dropwise Organic solvent, stir.
[0026] (3) Curing slurry: Add curing agent polyethylene glycol (polymerization degree 2000) and p-isooctyl phenyl ether (abbreviation: Raton X-100) to the slurry in step (2), and add the amount 3g and 3g respectively, then stir. Then add 6 g of high molecular polymer, which is methyl cellulose, and stir.
[0027] (4) Concentrated slurry: Distill the slurry obtained in step (3) at 80°C to obtain a graphene composite titanium dioxide slurry, the concentration of titanium dioxide is 1 g/L, and the concentration of graphene oxide is 1 g/L.
[0028] (5) Gas phase reduction: Pass the slurry obtained in step (4) through a screen, print it on a substrate, and then reduce it in a hydrogen atmosphere with a heating temperature of 600°C for 2 hours to prepare a graphene and titanium dioxide composite material.
[0029] The SEM image of the material structure section prepared in this example is as figure 1 As shown in the figure, it can be seen that the graphene-composite titanium dioxide material has a uniform composition, the surface is reduced by gas, and there is no fracture on the surface of the material. The large porosity of the film material is beneficial to the adhesion of the sensitizer and improves the photoelectric conversion efficiency of the solar cell. . Resistivity test result: Resistivity 5.352×10 -8 Ω·m.

Example Embodiment

[0030] Example 2
[0031] 1) Acidification treatment: Use nitric acid with a mass concentration of 90% acid solution and 100g of acid solution. Add 1g of titanium dioxide powder dropwise. The average particle size of titanium dioxide is 100μm.
[0032] (2) Prepare slurry: prepare graphene oxide solution, the concentration of graphene oxide solution is 100g/L, add it to the titanium dioxide powder in step (1), after adding to 1L, add organic solvent, organic solvent is methanol and Isopropanol and the organic solution were added in 50 g and 50 g, respectively, and then stirred.
[0033] (3) Curing slurry: Add curing agent polyethylene glycol (polymerization degree of 20000) and alkyl phenol polyoxyethylene ether (abbreviation: OP-10 emulsifier) ​​into the container in step (2), and add the amount of After 50g and 50g, then stir, and then add the high molecular polymer, the high molecular polymer is methyl cellulose and hydroxypropyl cellulose, the respective masses are respectively 60g and 40g, and then stir.
[0034] (4) Concentrated slurry: Distill the slurry obtained in step (3) at 90°C to obtain a graphene composite titanium dioxide slurry, the concentration of titanium dioxide is 1 g/L, and the concentration of graphene oxide is 100 g/L.
[0035] (5) Gas phase reduction: Pass the slurry obtained in step (4) through a screen, print it on a substrate, and then reduce it in an atmosphere of hydrogen and argon. The volume ratio is 20:80, the heating temperature is 323°C, and the time is 18h. Prepare graphene and titanium dioxide composite material.
[0036] The SEM image of the material structure section prepared in this example is as figure 2 As shown in the figure, it can be seen that the graphene-composite titanium dioxide material has a uniform composition, the surface is reduced by gas, and there is no fracture on the surface of the material. The large porosity of the film material is conducive to the adhesion of the sensitizer and improves the photoelectric conversion efficiency of the solar cell. ; Resistivity test result: Resistivity 4.28×10 -8 Ω·m.

Example Embodiment

[0037] Example 3
[0038] (1) Acidification treatment: 100g of a nitric acid solution with a mass concentration of 65% of the acid solution is added dropwise to 100g of titanium dioxide powder, the average particle size of the titanium dioxide is 10μm.
[0039] (2) Preparation of slurry: prepare graphene oxide solution with a concentration of 1g/L, add dropwise to the titanium dioxide powder in step (1), after adding to 1L, then add 22g methanol and 72g ethanol as organic solvent dropwise , And then stir.
[0040] (3) Curing slurry: add the curing agent terpineol and alkylphenol polyoxyethylene ether (OP-10 emulsifier) ​​to the container in step (2), the adding amount is 500g and 500g respectively, then stir and add High-molecular polymer, the high-molecular polymer is methyl cellulose and ethyl cellulose, the respective masses are 500 g and 500 g, and the mixture is stirred.
[0041] (4) Concentrated slurry: Distill the slurry obtained in step (3) at 30°C to obtain graphene-composite titanium dioxide slurry. The concentration of titanium dioxide in the slurry is 100 g/L, and the concentration of graphene oxide is 1 g/L.
[0042] (5) Gas phase reduction: Pass the slurry obtained in step (4) through a screen, print it on a substrate, and then reduce it in an atmosphere of hydrogen and argon. The volume ratio is 80:20, the heating temperature is 523°C, and the time is 18h. Prepare graphene and titanium dioxide composite material.
[0043] The SEM image of the material structure section prepared in this example is as image 3 As shown in the figure, it can be seen that the graphene-composite titanium dioxide material has a uniform composition, the surface is reduced by gas, and there is no fracture on the surface of the material. The large porosity of the film material is conducive to the adhesion of the sensitizer and improves the photoelectric conversion efficiency of the solar cell. ; Resistivity test result: Resistivity 7.78×10 -8 Ω·m.
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PUM

PropertyMeasurementUnit
Resistivity5.35E-8m·Ω
Resistivity4.28E-8m·Ω
Resistivity7.78E-8m·Ω
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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