Method for preparing high thermal conductivity graphite through catalytic graphitization

Abstract

The invention discloses a method for preparing high thermal conductivity graphite through catalytic graphitization. The method comprises the following steps: (1), preparing a carbon film material with an amorphous carbon structure by performing carbonization treatment on a polyimide film; (2), loading a catalyst onto the surface of the carbon film material obtained in the first step through any one method of solution impregnation, electroplating, chemical plating and liquid-phase precipitation; (3), performing graphitization treatment on the carbon film material, with the surface being loaded with the catalyst, obtained in the second step, so as to obtain the high thermal conductivity graphite. According to the method, a PI film is carbonized, so as to obtain the carbon film with the amorphous carbon structure, and then the catalyst is loaded onto the carbon film formed after carbonization, so that the catalyst is subjected to contact reaction with the film with the amorphous carbon structure from the outer part to the inner part, and damage caused by the overflow of the catalyst from the inner part is avoided. A graphite film prepared through the method can obtain high graphitization degree, excellent thermal conductivity and good bending resistance in low graphitization temperature.

Description

technical field

[0001] The invention belongs to the field of high thermal conductivity materials, in particular to a method for preparing high thermal conductivity graphite by catalytic graphitization. Background technique

[0002] With the rapid development of the microelectronics industry, electronic devices and equipment continue to develop in the direction of high power, high-density integration and miniaturization. The resulting heating problem poses a severe challenge to the performance, reliability and life of electronic products. . Highly oriented graphite film has excellent thermal conductivity and is an ideal and indispensable material for thermal field management in the field of microelectronic packaging and integration. In recent years, high thermal conductivity graphite films prepared by carbonization and graphitization using PI films as raw materials have been widely used in electronic products such as smartphones and notebook computers. However, at present, ...

Examples

Embodiment 1

[0034] A method for preparing high thermal conductivity graphite by catalytic graphitization of the present invention comprises the following steps:

[0035] (1) Carbonization treatment: stack the polyimide film and graphite paper of the required size cross-stacked and place them in the carbonization furnace; first vacuum the carbonization furnace to within 20Pa, then start the heating power supply at a heating rate of 10°C / min Raise the carbonization furnace from room temperature to 500 °C; then raise the temperature to 600 °C at a rate of 2 °C / min, and keep it for 30 min; then increase the rate of temperature to 800 °C at a rate of 2 °C / min; Raise the heating rate to 1000°C and hold it for 1 hour to obtain a carbon film material with an amorphous carbon structure;

[0036] (2) Loading catalyst: use nickel nitrate, iron sulfate and copper nitrate as solutes, deionized water as solvent, and configure a 0.2mol / L metal salt solution, in which the molar ratio of nickel ions, iron...

Embodiment 2

[0040] A method for preparing high thermal conductivity graphite by catalytic graphitization of the present invention comprises the following steps:

[0041] (1) Carbonization treatment: Stack the polyimide film and graphite paper of the required size crosswise and place them in the carbonization furnace; first vacuum the carbonization furnace to within 20Pa, then start the heating power supply at a heating rate of 15°C / min The carbonization furnace was raised from room temperature to 500°C; then raised to 600°C at a rate of 5°C / min, and held for 60 minutes; then raised to 800°C at a rate of 5°C / min; finally, at a rate of 15°C / min Raise the heating rate to 1300°C and hold for 2 hours to obtain a carbon film material with an amorphous carbon structure;

[0042] (2) Loading catalyst: use nickel nitrate as the solute, deionized water as the solvent, and configure a 0.15mol / L nickel nitrate solution as the electrolyte; use the carbon film material as the cathode, and the electroly...

Embodiment 3

[0046] A method for preparing high thermal conductivity graphite by catalytic graphitization of the present invention comprises the following steps:

[0047] (1) Carbonization treatment: Stack the polyimide film and graphite paper of the required size crosswise and place them in the carbonization furnace; first vacuum the carbonization furnace to within 20Pa, then start the heating power supply at a heating rate of 15°C / min The carbonization furnace was raised from room temperature to 500°C; then raised to 600°C at a rate of 1°C / min, and held for 30 minutes; then raised to 800°C at a rate of 1°C / min; finally, at a rate of 15°C / min Raise the heating rate to 1300°C and hold for 2 hours to obtain a carbon film material with an amorphous carbon structure;

[0048] (2) Loading catalyst: First, soak the carbon film in concentrated nitric acid with a temperature of 80°C and a mass fraction of 65% for 2 hours, take it out and clean it, and complete the roughening treatment; Soak in a...

technical field

[0001] The invention belongs to the field of high thermal conductivity materials, in particular to a method for preparing high thermal conductivity graphite by catalytic graphitization. Background technique

[0002] With the rapid development of the microelectronics industry, electronic devices and equipment continue to develop in the direction of high power, high-density integration and miniaturization. The resulting heating problem poses a severe challenge to the performance, reliability and life of electronic products. . Highly oriented graphite film has excellent thermal conductivity and is an ideal and indispensable material for thermal field management in the field of microelectronic packaging and integration. In recent years, high thermal conductivity graphite films prepared by carbonization and graphitization using PI films as raw materials have been widely used in electronic products such as smartphones and notebook computers. However, at present, ...

Examples

Embodiment 1

[0034] A method for preparing high thermal conductivity graphite by catalytic graphitization of the present invention comprises the following steps:

[0035] (1) Carbonization treatment: stack the polyimide film and graphite paper of the required size cross-stacked and place them in the carbonization furnace; first vacuum the carbonization furnace to within 20Pa, then start the heating power supply at a heating rate of 10°C / min Raise the carbonization furnace from room temperature to 500 °C; then raise the temperature to 600 °C at a rate of 2 °C / min, and keep it for 30 min; then increase the rate of temperature to 800 °C at a rate of 2 °C / min; Raise the heating rate to 1000°C and hold it for 1 hour to obtain a carbon film material with an amorphous carbon structure;

[0036] (2) Loading catalyst: use nickel nitrate, iron sulfate and copper nitrate as solutes, deionized water as solvent, and configure a 0.2mol / L metal salt solution, in which the molar ratio of nickel ions, iron...

Embodiment 2

[0040] A method for preparing high thermal conductivity graphite by catalytic graphitization of the present invention comprises the following steps:

[0041] (1) Carbonization treatment: Stack the polyimide film and graphite paper of the required size crosswise and place them in the carbonization furnace; first vacuum the carbonization furnace to within 20Pa, then start the heating power supply at a heating rate of 15°C / min The carbonization furnace was raised from room temperature to 500°C; then raised to 600°C at a rate of 5°C / min, and held for 60 minutes; then raised to 800°C at a rate of 5°C / min; finally, at a rate of 15°C / min Raise the heating rate to 1300°C and hold for 2 hours to obtain a carbon film material with an amorphous carbon structure;

[0042] (2) Loading catalyst: use nickel nitrate as the solute, deionized water as the solvent, and configure a 0.15mol / L nickel nitrate solution as the electrolyte; use the carbon film material as the cathode, and the electroly...

Embodiment 3

[0046] A method for preparing high thermal conductivity graphite by catalytic graphitization of the present invention comprises the following steps:

[0047] (1) Carbonization treatment: Stack the polyimide film and graphite paper of the required size crosswise and place them in the carbonization furnace; first vacuum the carbonization furnace to within 20Pa, then start the heating power supply at a heating rate of 15°C / min The carbonization furnace was raised from room temperature to 500°C; then raised to 600°C at a rate of 1°C / min, and held for 30 minutes; then raised to 800°C at a rate of 1°C / min; finally, at a rate of 15°C / min Raise the heating rate to 1300°C and hold for 2 hours to obtain a carbon film material with an amorphous carbon structure;

[0048] (2) Loading catalyst: First, soak the carbon film in concentrated nitric acid with a temperature of 80°C and a mass fraction of 65% for 2 hours, take it out and clean it, and complete the roughening treatment; Soak in a...