Low-temperature direct preparation method of graphene under double-temperature-zone control, and double-temperature-zone tube furnace

A dual-temperature zone and graphene technology, applied in the direction of graphene, nano-carbon, etc., can solve the problems that it is difficult to grow large-area and high-quality graphene films, and the carbon source gas cannot be fully cracked, and the growth process is simple, Realize the effect of large area growth and high crystal quality

CN102849733BInactive Publication Date: 2015-07-15SHANDONG NORMAL UNIV
2 Cites 0 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2015-07-15
Estimated Expiration
Not applicable · inactive patent

Smart Images

  • Figure 1
    Figure 1
  • Figure 2
    Figure 2
  • Figure 3
    Figure 3
Patent Text Reader

Abstract

The invention discloses a low-temperature direct preparation method of graphene under double-temperature-zone control, and a double-temperature-zone tube furnace. The method comprises the steps of dividing a vacuum reaction furnace into a high-temperature zone and a low-temperature zone, putting transition metal into the high-temperature zone, directly putting substrate material into the low-temperature zone, vacuumizing, injecting hydrogen gas into the vacuum reaction furnace, heating the low-temperature zone to 100-1,000 DEG C, heating the high-temperature zone to 1,000-1,100 DEG C, introducing carbon source into the vacuum reaction furnace, cracking the carbon source in the high-temperature zone, and performing chemical vapor deposition (CVD) for 5-180 min in the low-temperature zone while keeping constant hydrogen gas flow, to obtain graphene directly deposited on the substrate. The preparation method has the advantages of simple growth process, no need of catalysis, low growth temperature of 100-1,000 DEG C, no restriction on substrate material, and large-area growth of graphene. The grown graphene has low defect peak, high crystal quality, excellent light transmittance and electrical conductivity.
Need to check novelty before this filing date? Find Prior Art

Description

technical field

[0001] The invention relates to a preparation method of a graphene material, more specifically, relates to a method for directly preparing graphene at a low temperature controlled by dual temperature zones. The invention also relates to a tube furnace with two temperature zones for the method. Background technique

[0002] Carbon nanomaterials, including carbon nanotubes and graphene, are considered to be able to replace silicon materials as key materials for the preparation of nanoelectronic devices. Single-layer and double-layer graphene due to their singular properties (such as high carrier mobility (200000cm 2 / V·S) and current density (10 8 A / cm 2 )) have aroused widespread scientific interest. The relatively economical growth of large areas is the key requirement to effectively utilize the unique properties of graphene. Catalytic chemical vapor deposition (CVD) is the most promising and versatile growth technique. At elevated temperatures, transit...

Examples

Embodiment 1

[0048] Through the chemical vapor deposition method, dual temperature zone control directly prepares graphene at low temperature on quartz, such as figure 1 shown, including the following preparation steps

[0049] 1. Take the quartz substrate 6 and place it in the low temperature zone of the quartz tube 3; take the copper foil with a size of 6cm×8cm and place it in the high temperature zone;

[0050] 2. Turn on the vacuum pump to pump the air pressure of the quartz tube 3 to the ultimate vacuum state of 3×10-6 Torr;

[0051] 3. Keep vacuum 3×10 -6 After Torr for 15 minutes (the function of vacuum for 15 minutes is to remove impurities, air, etc. inside the quartz tube to ensure that the reaction chamber is clean), raise the air pressure of the quartz tube 3 to 3×10 -3 Torr;

[0052] 4. Set the hydrogen flow meter 1 to 100 sccm, inject hydrogen into the vacuum chamber;

[0053] 5. Raise the temperature of the temperature zone where the substrate is placed in the dual tempe...

Embodiment 2

[0062] Through the chemical vapor deposition method, dual temperature zone control directly prepares graphene on silicon at low temperature, including the following preparation steps:

[0063] 1. Take the silicon substrate 6 and place it in the quartz tube 3;

[0064] 2. Turn on the vacuum pump to pump the air pressure of the quartz tube 3 to the ultimate vacuum state of 3×10 -6 Torr;

[0065] 3. Keep vacuum 3×10 -6 After Torr for 15 minutes, increase the air pressure of the quartz tube 3 to 3×10 -3 Torr;

[0066] 4. Set the hydrogen flow meter 1 to 100 sccm, inject hydrogen into the vacuum chamber;

[0067] 5. Raise the temperature of the temperature zone where the substrate is placed in the dual temperature zone tube furnace to 450 degrees Celsius, and raise the temperature of the other temperature zone to 1050 degrees Celsius;

[0068] 6. After obtaining the predetermined temperature in the dual-temperature zone tube furnace, anneal at a constant temperature for 20 min...

Embodiment 3

[0075] Through the chemical vapor deposition method, dual temperature zone control directly prepares graphene at low temperature on the glass sheet, including the following preparation steps:

[0076] 1. Take the glass sheet substrate 6 and place it in the quartz tube 3;

[0077] 2. Turn on the vacuum pump to pump the air pressure of the quartz tube 3 to the ultimate vacuum state of 3×10 -6 Torr;

[0078] 3. Keep vacuum 3×10 -6 After Torr for 15 minutes, increase the air pressure of the quartz tube 3 to 3×10 -3 Torr;

[0079] 4. Set the hydrogen flow meter 1 to 100 sccm, inject hydrogen into the vacuum chamber;

[0080] 5. Raise the temperature of the temperature zone where the substrate is placed in the dual temperature zone tube furnace to 450 degrees Celsius, and raise the temperature of the other temperature zone to 1050 degrees Celsius;

[0081] 6. After obtaining the predetermined temperature in the dual-temperature zone tube furnace, anneal at a constant temperatur...