Method of preparing carbon-doped metal oxide nanoparticles

A technology of nanoparticles and oxides, which is applied in the field of preparation of carbon-doped metal oxide nanoparticles by high-temperature calcination, can solve problems that have not been reported yet, and achieve extended application value, easy control of operating conditions, and small particle size Effect

Active Publication Date: 2018-06-05
HUAQIAO UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The preparation technology of carbon-doped metal oxide nanoparticles based on supercritic

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  • Method of preparing carbon-doped metal oxide nanoparticles
  • Method of preparing carbon-doped metal oxide nanoparticles
  • Method of preparing carbon-doped metal oxide nanoparticles

Examples

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Embodiment 1

[0025] Dissolve zinc nitrate and methyl vinyl ether-maleic anhydride copolymer in acetone to form a mixed solution, control the mass ratio of zinc nitrate / methyl vinyl ether-maleic anhydride copolymer to 1:10, methyl vinyl ether The concentration of ether-maleic anhydride copolymer is 1wt%, and mixed solution is placed in the cylindrical plunger syringe, and the material of described cylindrical plunger syringe is made of stainless steel, and its length is 130mm, external diameter 32mm, inner diameter 24mm, can hold The solution volume is 20mL. The cylindrical piston syringe uses a high-pressure pump as the thrust source, and the end is connected to a nozzle. The mixed solution is sprayed into the precipitation kettle through the nozzle by the high-pressure pump at a flow rate of 0.5ml / min, and carbon dioxide is injected into the sedimentation tank through the high-pressure pump at a flow rate of 40g / min. In the kettle, the temperature of the precipitation kettle is controlled...

Embodiment 2

[0028] Dissolve nickel nitrate and methyl vinyl ether-maleic anhydride copolymer in ethanol, wherein the mass ratio of nickel nitrate / methyl vinyl ether-maleic anhydride copolymer is 1:2, methyl vinyl ether-maleic anhydride copolymer The concentration of anhydride copolymer is 5wt%, utilizes high-pressure pump to spray it in the sedimentation kettle through the nozzle with the flow velocity of 0.5ml / min, simultaneously carbon dioxide is injected in the sedimentation kettle with the flow rate of 40g / min through high-pressure pump, the temperature of precipitation kettle It is controlled at 308K, and the pressure of the precipitation tank is controlled at 10MPa. Under these conditions, the anti-solvent process occurred, so that the nickel nitrate-coated methyl vinyl ether-maleic anhydride copolymer nanospheres were prepared. After the prepared methyl vinyl ether-maleic anhydride copolymer nanospheres coated with nickel nitrate are calcined at 673K ​​for 4 hours, carbon-doped nan...

Embodiment 3

[0030] Dissolve cobalt nitrate and methyl vinyl ether-maleic anhydride copolymer in glycerin, wherein the mass ratio of cobalt nitrate / methyl vinyl ether-maleic anhydride copolymer is 1:20, methyl vinyl ether-maleic anhydride copolymer The concentration of the anhydride copolymer is 10wt%. Utilize a high-pressure pump to spray it into the precipitation kettle through a nozzle at a flow rate of 2ml / min, and simultaneously inject carbon dioxide into the precipitation kettle through a high-pressure pump at a flow rate of 40g / min. The temperature of the precipitation kettle is controlled At 328K, the pressure of the precipitation tank is controlled at 12MPa. Under these conditions, the anti-solvent process occurred, and the cobalt nitrate-coated methyl vinyl ether-maleic anhydride copolymer nanospheres were prepared. After calcining the prepared polymer nanospheres coated with nickel nitrate at 873K for 4 hours, carbon-doped nano-cobalt oxide particles with a particle diameter of ...

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Abstract

The invention provides a method of preparing carbon-doped metal oxide nanoparticles by means of the supercritical anti-solvent technology and high-temperature calcination. The method comprises the following steps: dissolving metal nitrate and a methyl vinyl ether-maleic anhydride copolymer in a solvent to form a mixed solution; then atomizing the mixed solution placed in a columnar piston injectorat a certain flow rate and injecting the mixed solution to a supercritical fluid; preparing polymer nanospheres of inorganic salt embedded with inorganic salt under the anti-solvent action of the supercritical fluid at a temperature of 308-330K and at a pressure of 10-12MPa; and calcining the nanospheres embedded with the metal nitrate and the methyl vinyl ether-maleic anhydride copolymer at a high temperature to finally obtain the carbon-doped metal oxide nanoparticles, the grain sizes of which are 10-100nm. The synthetic method is simple and easy to control operating condition, and the function and application of the metal oxide nanoparticles are improved greatly.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing carbon-doped metal oxide nanoparticles by supercritical antisolvent technology and high-temperature calcination. Background technique [0002] Due to the large specific surface, small size effect, interface effect and quantum effect, metal oxide nanoparticles exhibit unique electrical, thermal, magnetic, optical and mechanical properties, and are widely used in chemical, electronic, food, biological, medical and other fields. It has broad application prospects. The doping of carbon atoms will reduce the band gap of metal oxides and enhance the light absorption properties of metal oxides in the visible-near infrared band. In addition to optical properties, the electrical properties of metal oxides are also enhanced by the doping of carbon atoms. Therefore, the doping of carbon atoms will greatly enhance the application potential of metal o...

Claims

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Application Information

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IPC IPC(8): C01G53/04C01G9/02C01G51/04C01B32/15
CPCC01G9/02C01G51/04C01G53/04C01P2004/32C01P2004/64C01P2004/80Y02P20/54
Inventor 蒋妮娜陈爱政王士斌王祎玮
Owner HUAQIAO UNIVERSITY
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