A tib for aluminum electrolysis 2 -Graphene composite cathode material and preparation method thereof

Abstract

The invention relates to a TiB for aluminum electrolysis 2 ‑Graphene composite cathode material and preparation method thereof, in parts by weight, weighed TiB 2 88-95 parts of powder, 5-12 parts of graphene powder, 0.2-5 parts of dispersant, 1-5 parts of binder, and 1-10 parts of humic acid, after ball milling and mixing, drying to obtain mixed powder, for subsequent use; The mixed powder is shaped to obtain a green body; the green body is placed in an inert atmosphere, degreasing at 600-900°C for 16-64h, then heated to 1300-1600°C, sintered for 5-50h to obtain TiB 2 ‑Graphene composite cathode material. In the present invention, graphene is used as the reinforcing phase, compared with the existing aluminum electrolytic cell TiB 2 / C can wet the cathode and has better wettability; and the high electrical conductivity, corrosion resistance, low thermal expansion coefficient and tensile mechanical strength of graphene make the present invention have stronger resistance to high temperature molten salt erosion, High temperature structural stability, high electrical conductivity and other characteristics.

Description

technical field

[0001] The invention relates to a kind of TiB for aluminum electrolysis 2 -Graphene composite cathode material and preparation method thereof, specifically relating to a kind of TiB for aluminum electrolysis 2 - The graphene composite wettable cathode material and its preparation method belong to the field of aluminum electrolysis electrode material preparation. Background technique

[0002] The current aluminum electrolysis technology mainly adopts the Hall-Héroult molten salt electrolysis method, which requires the cathode material not only to have high conductivity, but also to withstand the chemical and physical erosion of the high-temperature cryolite electrolyte. Therefore, the choice of cathode material has a great influence on the performance of the electrolytic cell Has a big impact. At present, aluminum electrolytic cells have always used carbonaceous materials as cathode materials. In order not to expose the carbon cathode to the electrolyte, a c...

Examples

Embodiment 1

[0033] 95gTiB 2 Powder, 5g of graphene powder, 1g of water, 2g of epoxy resin and 1g of humic acid were mixed by ball mill for 4h, dried at 100°C for 10h, and subjected to vibration molding under a pressure of 200MPa to obtain TiB 2 - Graphene composite material green body, put the green body in an electric furnace, and perform degreasing treatment in an inert protective atmosphere, the degreasing temperature is 600 ° C, the degreasing time is 64h, and the oxygen content in the atmosphere is 50ppm; then in the Ar protective atmosphere The sintering process was carried out at a temperature of 50 °C / h to 1600 °C for sintering, and the temperature was kept for 5 h. During the sintering process, O 2 The content of TiB is 1ppm, and the sintering pressure is 2 tons; that is, TiB 2 - Graphene composite cathode material.

Embodiment 2

[0035] 60gTiB 2Powder, 40g graphene powder, 2g alcohol, 3g phenolic resin and 5g humic acid were mixed by ball mill for 6h, dried at 110°C for 10h, and vibrated under a pressure of 300MPa to obtain TiB 2 - Graphene composite green body, put the green body in an electric furnace, degrease in an inert protective atmosphere, the degreasing temperature is 800 ° C, the degreasing time is 48h, and the oxygen content in the atmosphere is 30ppm; then in the Ar protective atmosphere The sintering process was carried out at a temperature of 50 °C / h to 1500 °C for sintering, and the temperature was kept for 20 h. During the sintering process, O 2 The content of TiB is 5ppm, and the sintering pressure is 3 tons; that is, TiB 2 - Graphene composite cathode material.

Embodiment 3

[0037] 30gTiB 2 Powder, 70g of graphene powder, 5g of phthalic acid, 5g of polyethylene ethyl ester and 10g of humic acid were mixed by ball mill for 4 hours, dried at 100°C for 10 hours, and subjected to vibration molding under a pressure of 200MPa to obtain TiB 2 - Graphene composite material green body, put the green body in an electric furnace, degrease in an inert protective atmosphere, the degreasing temperature is 900 ° C, the degreasing time is 64h, and the oxygen content in the atmosphere is 10ppm; The sintering process was carried out at a temperature of 50°C / h to 1300°C for sintering, and the temperature was kept for 40h. During the sintering process, O 2 The content of TiB is 10ppm, and the sintering pressure is 4 tons; that is, TiB 2 - Graphene composite cathode material.

technical field

[0001] The invention relates to a kind of TiB for aluminum electrolysis 2 -Graphene composite cathode material and preparation method thereof, specifically relating to a kind of TiB for aluminum electrolysis 2 - The graphene composite wettable cathode material and its preparation method belong to the field of aluminum electrolysis electrode material preparation. Background technique

[0002] The current aluminum electrolysis technology mainly adopts the Hall-Héroult molten salt electrolysis method, which requires the cathode material not only to have high conductivity, but also to withstand the chemical and physical erosion of the high-temperature cryolite electrolyte. Therefore, the choice of cathode material has a great influence on the performance of the electrolytic cell Has a big impact. At present, aluminum electrolytic cells have always used carbonaceous materials as cathode materials. In order not to expose the carbon cathode to the electrolyte, a c...

Examples

Embodiment 1

[0033] 95gTiB 2 Powder, 5g of graphene powder, 1g of water, 2g of epoxy resin and 1g of humic acid were mixed by ball mill for 4h, dried at 100°C for 10h, and subjected to vibration molding under a pressure of 200MPa to obtain TiB 2 - Graphene composite material green body, put the green body in an electric furnace, and perform degreasing treatment in an inert protective atmosphere, the degreasing temperature is 600 ° C, the degreasing time is 64h, and the oxygen content in the atmosphere is 50ppm; then in the Ar protective atmosphere The sintering process was carried out at a temperature of 50 °C / h to 1600 °C for sintering, and the temperature was kept for 5 h. During the sintering process, O 2 The content of TiB is 1ppm, and the sintering pressure is 2 tons; that is, TiB 2 - Graphene composite cathode material.

Embodiment 2

[0035] 60gTiB 2Powder, 40g graphene powder, 2g alcohol, 3g phenolic resin and 5g humic acid were mixed by ball mill for 6h, dried at 110°C for 10h, and vibrated under a pressure of 300MPa to obtain TiB 2 - Graphene composite green body, put the green body in an electric furnace, degrease in an inert protective atmosphere, the degreasing temperature is 800 ° C, the degreasing time is 48h, and the oxygen content in the atmosphere is 30ppm; then in the Ar protective atmosphere The sintering process was carried out at a temperature of 50 °C / h to 1500 °C for sintering, and the temperature was kept for 20 h. During the sintering process, O 2 The content of TiB is 5ppm, and the sintering pressure is 3 tons; that is, TiB 2 - Graphene composite cathode material.

Embodiment 3

[0037] 30gTiB 2 Powder, 70g of graphene powder, 5g of phthalic acid, 5g of polyethylene ethyl ester and 10g of humic acid were mixed by ball mill for 4 hours, dried at 100°C for 10 hours, and subjected to vibration molding under a pressure of 200MPa to obtain TiB 2 - Graphene composite material green body, put the green body in an electric furnace, degrease in an inert protective atmosphere, the degreasing temperature is 900 ° C, the degreasing time is 64h, and the oxygen content in the atmosphere is 10ppm; The sintering process was carried out at a temperature of 50°C / h to 1300°C for sintering, and the temperature was kept for 40h. During the sintering process, O 2 The content of TiB is 10ppm, and the sintering pressure is 4 tons; that is, TiB 2 - Graphene composite cathode material.

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