Method for preparing nano metallic nickel granular material coating with carbon

Abstract

The invention relates to a preparation method for carbon-coated nano-metal nickel grain, which comprises the following steps: nickel precursor and macromolecule resin are respectively dissolved in organic solvent in proportion; the two solutions are mixed and 5% mass of auxiliary reagent is added in; the mixed solution is diffused uniformly via ultrasonic; the solvent is vaporized till approximately dry, and then the remainder is dried for 4 hours at 100 DEG C; the sample is crushed and then is solidified in inert or reducing gas and then carbonized to obtain the carbon-coated oxidation resisting nano-metal nickel. The grain size of the nano-metal nickel grain obtained with the method is about 40 to 80nm and the grain is coated with 5 to 10nm carbon layer outside. The metal content can becontrolled in a range of 1 to 90% with single phase. The material has the advantages of stability in air, oxidation resistance, simple preparation technology and easy realization of mass production, which is hopefully applied in sensors, magnetic storage medium, magnetic fluid, electromagnetic shielding and other fields.

Description

1. Technical field

[0001] The invention relates to a preparation method of a carbon-coated nano metal nickel particle material, which is prepared by mixing a nickel compound with a polymer resin, evaporating a solvent, solidifying and carbonizing. 2. Technical Background

[0002] Nanomaterials have attracted widespread attention due to their special structure, physical and chemical properties and potential huge application value. Since the discovery of C in 1985 60 Since then, carbon nanoscience has been continuously developed, and various forms of carbon materials such as carbon nanotubes, carbon nanofibers, hollow carbon nanospheres, metal-filled nanotubes and particles have been prepared one after another, opening up a new scientific research and technology applications.

[0003] Carbon-coated nano-metal is a new type of nano-functional material. The size of the metal particle is below 100nm, and the exterior is covered with a carbon layer. It is stable in the air for a...

Examples

Embodiment 1

[0024] Weigh 7.5g of nickel nitrate hexahydrate, dissolve in about 100ml of ethanol, and stir thoroughly to obtain solution A. Weigh 6.5g of thermosetting epoxy resin, dissolve it in 50ml of ethanol, add 0.7g of polyethylene glycol, mix it with the above-mentioned A solution, stir well, put it in a water bath at 80°C to evaporate the solvent until it is almost dry, and then dry it at 100°C for 4h After pulverization, polymer solids containing metal precursors are obtained. Take 10g of the solid in a porcelain container, place it in the center of the quartz tube in the tube furnace, and 2 Warming up in the air stream, H 2 The flow rate is 40ml / min, the heating rate is 1°C / min, the temperature is raised to 150°C, solidified for 1 hour, and then the temperature is continuously raised to 400°C, and the carbonization is carried out at a constant temperature for 4 hours. After the carbonization is completed, keep the gas flow, cool naturally to room temperature, and obtain a powde...

Embodiment 2

[0026] Weigh 0.62g of nickelocene, dissolve it in 20ml of acetone, stir well, and mix well. Weigh 34.3g of polyethylene resin with a molecular weight of 3000, dissolve it in 150ml of acetone, add 1.75g ​​of methylcellulose, mix with the above solution, stir evenly, evaporate the solvent in a water bath at 80°C until it is nearly dry, dry it at 100°C for about 4 hours, and then pulverize it. Polymer solids containing metal precursors were obtained. Take 10g of the solid in a porcelain container and place it in the center of the quartz tube in the tube furnace. 2 The temperature was raised in the air flow, the flow rate was 40ml / min, the heating rate was 1°C / min, the temperature was raised to 130°C, solidified for 1 hour, and then the temperature was further raised to 600°C, and the carbonization was carried out at a constant temperature for 4 hours. After carbonization, keep the gas flow, cool down to room temperature naturally, and take out the powder sample, which is carbon-...

Embodiment 3

[0028]Weigh 6.4g of nickel acetylacetonate, dissolve it in about 100ml of ethylene glycol, stir well, and mix well. Weigh 31.2g of styrene resin with a molecular weight of 5000, dissolve it in 130ml of ethylene glycol, add 1.87g of methyl cellulose, mix with the above solution, stir evenly, evaporate the solvent in a water bath at 80°C until it is nearly dry, and dry it at 100°C for about 4 hours Pulverize to obtain polymer solids containing metal precursors. Take 10g of the solid in a porcelain container, place it in the center of the quartz tube in a tube furnace, raise the temperature in the He flow, the flow rate is 40ml / min, the heating rate is 1°C / min, the temperature is raised to 140°C, solidified for 1h, and then continue Raise the temperature to 800°C, and carbonize at a constant temperature for 4 hours. After carbonization, keep the gas flow, cool naturally to room temperature, and take out the powder sample, which is the carbon-coated nano-metal nickel particle mat...

1. Technical field

[0001] The invention relates to a preparation method of a carbon-coated nano metal nickel particle material, which is prepared by mixing a nickel compound with a polymer resin, evaporating a solvent, solidifying and carbonizing. 2. Technical Background

[0002] Nanomaterials have attracted widespread attention due to their special structure, physical and chemical properties and potential huge application value. Since the discovery of C in 1985 60 Since then, carbon nanoscience has been continuously developed, and various forms of carbon materials such as carbon nanotubes, carbon nanofibers, hollow carbon nanospheres, metal-filled nanotubes and particles have been prepared one after another, opening up a new scientific research and technology applications.

[0003] Carbon-coated nano-metal is a new type of nano-functional material. The size of the metal particle is below 100nm, and the exterior is covered with a carbon layer. It is stable in the air for a...

Examples

Embodiment 1

[0024] Weigh 7.5g of nickel nitrate hexahydrate, dissolve in about 100ml of ethanol, and stir thoroughly to obtain solution A. Weigh 6.5g of thermosetting epoxy resin, dissolve it in 50ml of ethanol, add 0.7g of polyethylene glycol, mix it with the above-mentioned A solution, stir well, put it in a water bath at 80°C to evaporate the solvent until it is almost dry, and then dry it at 100°C for 4h After pulverization, polymer solids containing metal precursors are obtained. Take 10g of the solid in a porcelain container, place it in the center of the quartz tube in the tube furnace, and 2 Warming up in the air stream, H 2 The flow rate is 40ml / min, the heating rate is 1°C / min, the temperature is raised to 150°C, solidified for 1 hour, and then the temperature is continuously raised to 400°C, and the carbonization is carried out at a constant temperature for 4 hours. After the carbonization is completed, keep the gas flow, cool naturally to room temperature, and obtain a powde...

Embodiment 2

[0026] Weigh 0.62g of nickelocene, dissolve it in 20ml of acetone, stir well, and mix well. Weigh 34.3g of polyethylene resin with a molecular weight of 3000, dissolve it in 150ml of acetone, add 1.75g ​​of methylcellulose, mix with the above solution, stir evenly, evaporate the solvent in a water bath at 80°C until it is nearly dry, dry it at 100°C for about 4 hours, and then pulverize it. Polymer solids containing metal precursors were obtained. Take 10g of the solid in a porcelain container and place it in the center of the quartz tube in the tube furnace. 2 The temperature was raised in the air flow, the flow rate was 40ml / min, the heating rate was 1°C / min, the temperature was raised to 130°C, solidified for 1 hour, and then the temperature was further raised to 600°C, and the carbonization was carried out at a constant temperature for 4 hours. After carbonization, keep the gas flow, cool down to room temperature naturally, and take out the powder sample, which is carbon-...

Embodiment 3

[0028]Weigh 6.4g of nickel acetylacetonate, dissolve it in about 100ml of ethylene glycol, stir well, and mix well. Weigh 31.2g of styrene resin with a molecular weight of 5000, dissolve it in 130ml of ethylene glycol, add 1.87g of methyl cellulose, mix with the above solution, stir evenly, evaporate the solvent in a water bath at 80°C until it is nearly dry, and dry it at 100°C for about 4 hours Pulverize to obtain polymer solids containing metal precursors. Take 10g of the solid in a porcelain container, place it in the center of the quartz tube in a tube furnace, raise the temperature in the He flow, the flow rate is 40ml / min, the heating rate is 1°C / min, the temperature is raised to 140°C, solidified for 1h, and then continue Raise the temperature to 800°C, and carbonize at a constant temperature for 4 hours. After carbonization, keep the gas flow, cool naturally to room temperature, and take out the powder sample, which is the carbon-coated nano-metal nickel particle mat...

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