CN102502604A

CN102502604A - Preparation method of multifunctional graphene tube

Info

Publication number: CN102502604A
Application number: CN2011103423593A
Authority: CN
Inventors: 郭新立; 刘建双; 汤铨
Original assignee: Southeast University
Current assignee: Southeast University
Priority date: 2011-11-03
Filing date: 2011-11-03
Publication date: 2012-06-20

Abstract

The invention discloses a preparation method of a multifunctional graphene tube. The preparation method comprises the following steps of: preparing: prefabricating a graphene tube stencil structure of a required shape by taking a copper metal wire or a nickel metal wire as a stencil; and transferring: (1) coating a polymethyl methacrylate (PMMA) protective coating in a spinning way; (2) putting a graphene tube into 0.1-0.2 mol/L of a (NH4)2S2O8 solvent by taking a copper wire as a stencil or putting the graphene tube into 0.1-0.2 mol/L of an FeCl3 solvent by taking the nickel wire as a stencil, and dissolving the metal wire out; and (3) dripping methylphenyl ether onto a PMMA-coated graphene tube surface, and slowly covering the methylphenyl ether on a PMMA thin layer. Due to the adoption of the method, a graphene tube which is of controllable shape and size and is conductive, transparent and easy to operate can be prepared effectively and stably at high quality.

Description

A kind of preparation method of multifunctional graphite vinyl pipe

Technical field

The invention belongs to materials science field, is a kind of technology that simply, effectively prepares the Graphene pipe of multiple shape and size.

Background technology

Carbon nanotube is owing to its high conduction, heat conduction and mechanical property are widely used, and Graphene has more excellent conduction, heat conduction, printing opacity and mechanical property with respect to carbon nanotube.Therefore, the preparation of Graphene pipe possibly have more excellent performance and more wide application.Present technique adopts the technology of sophisticated process for preparing graphenes by chemical vapour deposition, is substrate with the copper or the nickel wire of different size, prepares shape, controllable size, and conduction, transparent, the Graphene pipe that is easy to control.

Summary of the invention

Technical problem:The present invention is directed to the unmanageable shortcoming of shape, size, separation and operation of carbon nanotube, utilize the technology of process for preparing graphenes by chemical vapour deposition, prepare shape, controllable size, and conduction, transparent, the Graphene pipe that is easy to control.

Technical scheme:The preparation method of multifunctional graphite vinyl pipe of the present invention comprises following process step:

A. preparation: with copper metal line or nickel metal wire is masterplate, is prefabricated into the Graphene pipe die plate structure of desired shape, and with the outstanding constant temperature section of putting into chemical vapor deposition chamber of this stencil structure, sealed silica envelope vacuumizes in 10-15Pa, feeds Ar gas; Then at H ₂, be heated to 950-1000 ℃ in the Ar atmosphere, and insulation 30-40 minute is then at CH ₄And H ₂Growth Graphene 5-15min under the atmosphere is at last at H ₂, in-situ annealing and cool to room temperature under the Ar atmosphere;

B. shift: step is:

1) spin coating polymetylmethacrylate supercoat; The used instrument of spin coating is a sol evenning machine, and solution is the PMMA/ methyl-phenoxide, the coating procedure parameter: first low speed 600-620rpm applies 10s; High speed 4000-4200rpm applies 60s again, on warm table, heats 5min. in 130-150 ℃ then.

2) with the copper cash be masterplate, the Graphene pipe is put into 0.1-0.2mol/L (NH ₄) ₂S ₂O ₈In the solvent, or be masterplate, the Graphene pipe is put into 0.1-0.2mol/L FeCl with the nickel wire ₃In the solvent, with the metal wire stripping, it is clean to put into the clear water rinsing then, obtains after the taking-up outsidely coating support transparent, conduction, the various multifunctional graphite vinyl pipe of shape and size by PMMA.

3) methyl-phenoxide is dripped the Graphene tube-surface that coats in PMMA methyl-phenoxide slowly is covered on the PMMA thin layer, this moment, the PMMA film can be melted at once, with inhaling paper organic solvent was siphoned away on the edge of, repeated 2-3 time, and Graphene/substrate is cleaned up; Dry up at last and obtain not having that PMMA coats is transparent, conduction, the various multifunctional graphite vinyl pipe of shape and size.

Beneficial effect:Adopt the inventive method, can be efficiently, stablize, high-qualityly prepare shape, controllable size, and conduction, transparent, the Graphene pipe that is easy to control.

Embodiment

Instance 1

With the copper cash is that substrate is prepared trapezoidal Graphene pipe:

1. be that 1 millimeter copper wire bends to trapezoidal and is suspended in the constant temperature section in the silica tube in the chemical vapor depsotition equipment with diameter, sealed silica envelope vacuumizes in 10Pa, feeds Ar gas.Then at H ₂, be heated to 950 ℃ in the Ar atmosphere, and be incubated 30 minutes, again at CH ₄And H ₂The 5min that grows under the atmosphere is at last at H ₂, in-situ annealing and cool to room temperature under the Ar atmosphere, preparation Graphene pipe.

2. spin coating polymetylmethacrylate supercoat, solution is the PMMA/ methyl-phenoxide.The coating procedure parameter: first low speed (600rpm) applies 10s, and (4000rpm) applies 60s at a high speed again, on warm table, heats 5min. in 130-150 ℃ then.

3. apply the PMMA layer with the Graphene pipe is outside, and the Graphene pipe after will applying is positioned in the ammonium persulfate solution of 0.1mol/L, with the copper wire stripping, ultrasonic 5min, change water clean for 2-3 time clean, obtain the PMMA coating transparent, conduct electricity trapezoidal Graphene pipe.

4. methyl-phenoxide is dripped the Graphene tube-surface that coats in PMMA methyl-phenoxide slowly is covered on the PMMA thin layer, this moment, the PMMA film can be melted at once, with inhaling paper organic solvent was siphoned away on the edge of, repeated 2-3 time, and Graphene/substrate is cleaned up; Dry up at last and obtain not having transparent, the trapezoidal Graphene pipe of conduction that PMMA coats.

Instance 2

With the nickel wire is that substrate is prepared trapezoidal Graphene pipe:

1. be that 1 millimeter nickel wire bends to trapezoidal and is suspended in the constant temperature section in the silica tube in the chemical vapor depsotition equipment with diameter, sealed silica envelope vacuumizes in 10Pa, feeds Ar gas.Then at H ₂, be heated to 950 ℃ in the Ar atmosphere, and be incubated 30 minutes, again at CH ₄And H ₂The 10min that grows under the atmosphere is at last at H ₂, in-situ annealing and cool to room temperature under the Ar atmosphere, preparation Graphene pipe.

2. spin coating PMMA supercoat, solution is the PMMA/ methyl-phenoxide.The coating procedure parameter: first low speed (610rpm) applies 10s, and (4100rpm) applies 60s at a high speed again, on warm table, heats 5min. in 140 ℃ then.

3. Graphene pipe outside is applied the PMMA layer, and the Graphene pipe after will applying is positioned over the FeCl of 0.2mol/L ₃In the solution, with the nickel wire stripping, ultrasonic 8min changes water and cleans only for 2-3 time, obtains transparent, the trapezoidal Graphene pipe of conduction that PMMA coats.

Instance 3

With the copper cash is that substrate is prepared semicircle Graphene pipe:

1. be that 1 millimeter copper wire bends to semicircle and is suspended in the constant temperature section in the silica tube in the chemical vapor depsotition equipment with diameter, sealed silica envelope vacuumizes in 15Pa, feeds Ar gas.Then at H ₂, be heated to 1000 ℃ in the Ar atmosphere, and be incubated 30 minutes, again at CH ₄And H ₂The 15min that grows under the atmosphere is at last at H ₂, in-situ annealing and cool to room temperature under the Ar atmosphere, preparation Graphene pipe.

2. spin coating polymetylmethacrylate supercoat, solution is the PMMA/ methyl-phenoxide.The coating procedure parameter: first low speed (620rpm) applies 10s, and (4200rpm) applies 60s at a high speed again, on warm table, heats 5min. in 150 ℃ then.

3. apply the PMMA layer with the Graphene pipe is outside, and the Graphene pipe after will applying is positioned in the ammonium persulfate solution of 0.2mol/L, with the copper wire stripping, ultrasonic 10min changes water and cleans for 2-3 time only, obtains transparent, the semicircle Graphene pipe that conducts electricity of PMMA coating.

4. methyl-phenoxide is dripped the Graphene tube-surface that coats in PMMA methyl-phenoxide slowly is covered on the PMMA thin layer, this moment, the PMMA film can be melted at once, with inhaling paper organic solvent was siphoned away on the edge of, repeated 2-3 time, and Graphene/substrate is cleaned up; Dry up at last and obtain not having transparent, the semicircle Graphene pipe of conduction that PMMA coats.

Claims

1. the preparation method of a multifunctional graphite vinyl pipe is characterized in that this preparation method comprises following two portions:

B. shift: step is:

1) spin coating polymetylmethacrylate supercoat; The used instrument of spin coating is a sol evenning machine, and solution is the PMMA/ methyl-phenoxide, the coating procedure parameter: first low speed 600-620rpm applies 10s; High speed 4000-4200rpm applies 60s again, on warm table, heats 5min in 130-150 ℃ then;

2) with the copper cash be masterplate, the Graphene pipe is put into 0.1-0.2mol/L (NH ₄) ₂S ₂O ₈In the solvent, or be masterplate, the Graphene pipe is put into 0.1-0.2mol/L FeCl with the nickel wire ₃In the solvent, with the metal wire stripping, it is clean to put into the clear water rinsing then, obtains after the taking-up outsidely coating support transparent, conduction, the various multifunctional graphite vinyl pipe of shape and size by PMMA;