WO2021212775A1

WO2021212775A1 - Preparation method for nickel-coated graphene silicon carbide

Info

Publication number: WO2021212775A1
Application number: PCT/CN2020/121410
Authority: WO
Inventors: 戴亚洲
Original assignee: 南京同诚节能环保装备研究院有限公司
Priority date: 2020-04-24
Filing date: 2020-10-16
Publication date: 2021-10-28
Also published as: CN111500104A

Abstract

A preparation method for a nickel-coated graphene silicon carbide. Nickel-coated graphene preparation, plating solution preparation, silicon carbide coarsening, and nickel plating are performed, a nickel-coated graphene silicon carbide solution is filtered, and the filtered nickel-coated graphene silicon carbide is dried at 120-160°C for 3-6 hours to obtain 1280 g of uniform nickel-coated graphene silicon carbide particles. Finally, 50-90 g of a high-temperature-resistant organic resin is added to 40-50 g of the nickel-coated graphene silicon carbide, and the two are stirred until evenly mixed. The described technical solution uses chemical kinetics to prepare a nickel-coated graphene silicon carbide. The preparation method is simple and can be used for mass production, and the prepared nickel-coated graphene silicon carbide is resistant to high temperatures and to corrosion, and has high toughness and stability, thus improving overall the longevity of the surface coating of the graphene.

Description

Preparation method of nickel-coated graphene silicon carbide

Technical field

The invention relates to the field of corrosion-resistant high-temperature super thermally conductive nanomaterials, in particular to a method for preparing nickel-coated graphene silicon carbide.

Background technique

At present, the use of heat exchanger titanium alloy plates in production has increased, and the cost has increased. The application of nickel-coated graphene silicon carbide coating can replace precious metals such as titanium alloys and achieve similar effects. Nickel-coated graphene silicon carbide solves the defects of expensive metal and corrosion resistance and thermal conductivity that cannot meet the needs of environmental protection development. Graphene is a superconducting and corrosion-resistant material. The disadvantage is that it is not resistant to high temperatures. Graphene will be carbonized above 500 degrees, and its thermal conductivity and corrosion resistance will decrease.

Summary of the invention

The purpose of the present invention is to solve the above problems and provide a method for preparing nickel-coated graphene silicon carbide. Nickel is an anti-oxidation material and also a corrosion-resistant material with high viscosity. Nickel-based materials are used to coat graphene silicon carbide. It is the key to solve the problem of graphene oxidation resistance and improve the comprehensive material capabilities. The main function of silicon carbide is to conduct heat conduction, wear resistance, corrosion resistance and toughness, and make graphene more susceptible to being coated with nickel. It is a catalytic material for coating stone alkene. The nickel-coated graphene silicon carbide material with a thermal conductivity of 58.8-73w/(m·℃) has improved thermal conductivity, corrosion resistance, high temperature resistance, corrosion resistance and high toughness.

The technical scheme of the present invention is achieved as follows: a method for preparing nickel-coated graphene silicon carbide, which is characterized in that the specific steps are as follows:

(1) Use an intermediate frequency furnace to melt the metallic nickel, and use a breeze to blow the nano graphene into a vacuum tube with a diameter of 1m and a length of 27m. At the same time, pour the molten nickel water into the high-speed tuyere. The nickel water is 46m/s per second. When the wind speed is blowing into the vacuum tube, the nano-graphene moves in a high-speed linear motion in the vacuum tube, and is distributed in a network. The metal nickel particles hit the graphene particles at an overspeed to fully coat the graphene, and the nitrogen gas is passed into the vacuum tube to prevent nickel from coating the graphite. Oxidation of olefin particles;

(2) Mix nickel sulfate, sodium hypophosphite, lactic acid, succinic acid, malic acid, citric acid, and potassium iodate under certain conditions to prepare a plating solution;

(3) Place the nano-silicon carbide particles in 70% nitric acid, oscillate with ultrasound, and then roughen them for 30 minutes, take them out and rinse them with deionized water to obtain clean and rough-surface nano-silicon carbide Particles

(4) Mix the nickel-coated graphene with absolute ethanol and acetic acid uniformly, add the silicon carbide particles with rough surface, and mix again, and vibrate ultrasonically for 30-60 minutes to make the material sol uniformly dispersed; combine the uniformly dispersed silicon carbide and nickel The coated graphene particle sol is dried in a drying oven at 300-350°C for 2-3 hours, taken out and cooled, and placed in the plating solution, stirred during the plating process at a stirring speed of about 300r/min, and stirred for 2 hours;

(5) Filter the nickel-coated graphene silicon carbide solution, and dry the filtered nickel-coated graphene silicon carbide at a temperature of 120-160°C for 3-6 hours to obtain uniform nickel-coated graphene silicon carbide particles ；

(6) Finally, 50-90g of high temperature resistant organic resin is added to 40-50g of nickel-coated graphene silicon carbide, stirred until the mixture is uniform, and finally a nickel-coated graphene silicon carbide coating is formed.

Further, the plating solution contains nickel sulfate 300-432g, sodium hypophosphite 300-400g, lactic acid 30-62ml/l, succinic acid 5-11.5g, malic acid 2-5.6g, citric acid 15-35g, Mixture of potassium iodate 1-4mg/l.

Further, the said plating solution has a pH value of 4.5-5 and a temperature of 85-90°C in a specific environment.

Beneficial effects:

The beneficial effects of the present invention: through the principle of chemical kinetics, metal nickel is used to solve the problem that graphene is not resistant to high temperature. The metal nickel is anti-oxidation, corrosion-resistant and highly viscous, and is coated on the graphene surface to prevent carbonization of graphene and improve thermal conductivity and corrosion resistance. Performance, silicon carbide has the characteristics of heat conduction, wear resistance, corrosion resistance and toughening, and it is also a catalyst for accelerating the metal nickel-coated graphene. The nickel-coated graphene silicon carbide obtained is resistant to high temperature, corrosion and toughness.

Detailed ways

In order to make it easy to understand the technical means, creative features, and objectives achieved by the present invention, the following examples are given to describe the present invention in detail.

The specific steps of the present invention are as follows:

First, use an intermediate frequency furnace to melt the metal nickel. A vacuum tube with a diameter of 1m and a length of 27m is used. The nanographene is blown into the tube with breeze. At the same time, the nickel water is poured into the high-speed tuyere. The nickel water is at a wind speed of 46m/s per second. Blow into the vacuum tube, the nano graphene moves linearly at a high speed in the vacuum tube, and is distributed in a net shape. The metal nickel particles hit the graphene particles at an overspeed to fully coat the graphene and pass nitrogen into the vacuum tube.

The nano-silicon carbide particles are then placed in 70% nitric acid, oscillated with ultrasonic waves, and then roughened for 30 minutes, taken out and rinsed with deionized water to obtain clean and rough-surfaced nano-silicon carbide particles.

The nickel-coated graphene particles are uniformly mixed with absolute ethanol and acetic acid, and silicon carbide particles are added to mix uniformly again, and ultrasonically oscillate for 30-60 minutes to make the material sol uniformly dispersed.

A plating solution is prepared, and the plating solution is a mixed solution of nickel sulfate, sodium hypophosphite, lactic acid, succinic acid, malic acid, and potassium citrate iodate.

Put the processed nickel-coated graphene particles and silicon carbide particles into a drying oven at 300-350°C for 2-3 hours, take them out for cooling, and then put the dried nickel-coated graphene particles and silicon carbide particles into a drying oven. Put it into the plating solution, ensure that the pH value of the plating solution is 4.5-5, and the temperature is 85-90°C, and stir during the plating process at a stirring speed of about 300r/min to obtain a nickel-coated graphene silicon carbide solution.

The nickel-coated graphene silicon carbide solution is filtered, and the filtered nickel-coated graphene silicon carbide is dried at a temperature of 120-160° C. for 3-6 hours to obtain uniform nickel-coated graphene silicon carbide particles.

Finally, 70-100 g of high temperature resistant water-based resin is added to 20-30 g of nickel-coated graphene silicon carbide, and stirred until the mixture is uniform.

In the present invention, the function of introducing nitrogen gas is to protect the nickel-coated graphene and prevent metal oxidation.

In the present invention, the plating solution is 300-432g nickel sulfate, 300-400g sodium hypophosphite, 30-62ml/l lactic acid, 5-11.5g succinic acid, 2-5.6g malic acid, 15-35g citric acid, Mixture of potassium iodate 1-4mg/l.

Example one:

Preparation of nickel-coated graphene: Use an intermediate frequency furnace to melt 1000g of metallic nickel. When the wind speed is 46m/s, blow 300g of nanographene into a vacuum tube with a diameter of 1m and a length of 27m, and pour the molten nickel water into it. With high-speed tuyere, nickel water is blown into the vacuum tube at a wind speed of 46m/s per second. The nano-graphene moves in a high-speed linear motion in the vacuum tube and is distributed in a network shape. The metal nickel particles hit the graphene particles at high speed to fully coat the graphene. Pour nitrogen into the vacuum tube to prevent oxidation of the nickel-coated graphene particles.

Preparation of plating solution: prepare 300-432g nickel sulfate, 300-400g sodium hypophosphite, 30-62ml/l lactic acid, 5-11.5g succinic acid, 2-5.6g malic acid, 15-35g citric acid, potassium iodate 1 -4mg/l, 300-1000g graphene colloidal nano carbonized silica gel under the conditions of pH 4.5-5 and temperature 85-90℃.

Silicon carbide roughening: Place 300g of nano-silicon carbide particles in 1000ml of 70% nitric acid, oscillate with ultrasound, and then roughen them for 30min, take them out and rinse with deionized water to get a clean and rough surface 280g of nano silicon carbide particles.

Nickel plating: Mix 1000g of nickel-coated graphene, 280ml of absolute ethanol, and 100ml of acetic acid, add 280g of silicon carbide particles with rough surface, and mix again, and ultrasonically shake for 30-60min to make the material sol evenly dispersed; The silicon carbide and nickel-coated graphene particle sol are dried in a drying oven at 300-350°C for 2-3 hours. After being taken out and cooled, they are placed in the plating solution and stirred during the plating process at a stirring speed of about 300r/min. Stir for 2 hours.

The nickel-coated graphene silicon carbide solution is filtered, and the filtered nickel-coated graphene silicon carbide is dried at a temperature of 120-160° C. for 3-6 hours to obtain 1280 g of uniform nickel-coated graphene silicon carbide particles.

Finally, add 50-90 g of high temperature resistant organic resin to 40-50 g of nickel-coated graphene silicon carbide, and stir until the mixture is uniform.

Claims

A method for preparing nickel-coated graphene silicon carbide, which is characterized in that it comprises the following steps:

(1) Use an intermediate frequency furnace to melt the metallic nickel, and use a breeze to blow the nano graphene into a vacuum tube with a diameter of 1m and a length of 27m. At the same time, pour the molten nickel water into the high-speed tuyere. The nickel water is 46m/s per second. When the wind speed is blowing into the vacuum tube, the nano-graphene moves in a high-speed linear motion in the vacuum tube, and is distributed in a network. The metal nickel particles hit the graphene particles at an overspeed to fully coat the graphene, and the nitrogen gas is passed into the vacuum tube to prevent nickel from coating the graphite. Oxidation of olefin particles;

(2) Mix nickel sulfate, sodium hypophosphite, lactic acid, succinic acid, malic acid, citric acid, and potassium iodate under certain conditions to prepare a plating solution;

(3) Place the nano-silicon carbide particles in 70% nitric acid, oscillate with ultrasound, and then roughen them for 30 minutes, take them out and rinse them with deionized water to obtain clean and rough-surface nano-silicon carbide Particles

(4) Mix the nickel-coated graphene with absolute ethanol and acetic acid uniformly, add the silicon carbide particles with rough surface, and mix again, and vibrate ultrasonically for 30-60 minutes to make the material sol uniformly dispersed; combine the uniformly dispersed silicon carbide and nickel The coated graphene particle sol is dried in a drying oven at 300-350°C for 2-3 hours, taken out and cooled, and placed in the plating solution, stirred during the plating process at a stirring speed of about 300r/min, and stirred for 2 hours;

(5) Filter the nickel-coated graphene silicon carbide solution, and dry the filtered nickel-coated graphene silicon carbide at a temperature of 120-160°C for 3-6 hours to obtain uniform nickel-coated graphene silicon carbide particles ；

(6) Finally, 50-90g of high temperature resistant organic resin is added to 40-50g of nickel-coated graphene silicon carbide, stirred until the mixture is uniform, and finally a nickel-coated graphene silicon carbide coating is formed.
The method for preparing nickel-coated graphene silicon carbide according to claim 1, wherein the plating solution contains 300-432g of nickel sulfate, 300-400g of sodium hypophosphite, and 30-62ml/l of lactic acid. , 5-11.5g of succinic acid, 2-5.6g of malic acid, 15-35g of citric acid, and 1-4mg/l of potassium iodate.
The method for preparing nickel-coated graphene silicon carbide according to claim 1, wherein the plating solution has a pH value of 4.5-5 and a temperature of 85-90°C in a specific environment.