CN110510602A - Method for growing graphene film on insulating substrate without catalyst - Google Patents

Abstract

The invention discloses a kind of methods of no catalyst dielectric base growth graphene film, the following steps are included: preparing a quartz ampoule, the both ends of quartz ampoule are respectively feed end and base terminal, a dielectric base is placed in the base terminal of quartz ampoule, raw material are placed in the feed end of quartz ampoule, quartz ampoule is vacuumized, sealed after being vacuumized quartz ampoule, so that the intraductal pressure of the quartz ampoule is 10^‑4~10^‑6Pa, wherein raw material are polyethylene or polypropylene；Feed end and base terminal to quartz ampoule heat 0.5~1h simultaneously, it cools to 20~25 DEG C of room temperature after heating with the furnace, obtains graphene film on a dielectric base, wherein, the heating temperature of feed end is 1000~1150 DEG C, and the heating temperature of base terminal is 200~900 DEG C.In method of the invention, graphene film can according to self-demand no catalyst in the case where covering 1cm × 2cm dielectric base it is even more big.

Description

Method for growing graphene film on insulating substrate without catalyst

technical field

The invention belongs to the technical field of graphene film preparation, and in particular relates to a method for growing a graphene film on a catalyst-free insulating substrate.

Background technique

Graphene is a typical representative of two-dimensional materials. There are many methods for preparing graphene. The common ones are mechanical exfoliation method, redox method, chemical vapor deposition method, arc discharge method, etc. It can be widely used in electronic devices field, battery field, ink spraying, textile field, biomedicine, aerospace, energy storage and many other fields.

At present, the graphene film prepared by mechanical exfoliation method is difficult to achieve consistent uniformity, and the yield is low. The preparation of graphene films by redox method requires high cost. The principle of graphene preparation by chemical vapor deposition is complex, easy to pollute, and subject to external interference; the preparation of graphene film by arc discharge method has high quality, low crystallinity, and small size.

Contents of the invention

In view of the deficiencies in the prior art, the object of the present invention is to provide a method for growing a graphene film on an insulating substrate without a catalyst, which can realize a graphene film on an insulating substrate by using a chemical vapor transport method under the condition of no catalyst. of large area growth.

The purpose of the present invention is achieved through the following technical solutions.

A method for growing a graphene film on a catalyst-free insulating substrate, comprising the following steps:

1) Prepare a quartz tube, the two ends of the quartz tube are the raw material end and the base end respectively, an insulating base is placed in the base end of the quartz tube, raw materials are placed in the raw material end of the quartz tube, and the Vacuum the quartz tube, and seal the quartz tube after vacuuming, so that the inner pressure of the quartz tube is 10 ^-4 ~ 10 ^-6 Pa, wherein the raw material is polyethylene or polypropylene;

In the step 1), the insulating substrate is sapphire, glass, quartz or mica.

In the step 1), the quartz tube has a length of 30-50 cm and an inner diameter of 10-20 mm.

In the step 1), the mass of the raw material is 0.5-2 mg, and the area of the insulating base is 1 cm×(2-5) cm.

2) Heating the raw material end and the base end of the quartz tube simultaneously for 0.5 to 1 h, cooling to room temperature 20 to 25°C with the furnace after heating, and obtaining a graphene film on the insulating substrate, wherein the heating temperature of the raw material end is 1000 ~1150°C, the heating temperature of the base end is 200-900°C.

In the step 2), the temperature gradient between the raw material end and the base end is 3-30° C./cm.

In the method of the present invention, the graphene film can cover an insulating substrate of 1 cm×2 cm or even larger without a catalyst according to its own needs.

Description of drawings

Fig. 1 is the Raman spectrum of the graphene thin film that embodiment of the present invention 1 obtains;

Fig. 2 is the Raman spectrum of the graphene film that embodiment 1 of the present invention obtains;

Fig. 3 is the Raman spectrum of the graphene thin film that embodiment of the present invention 2 obtains;

Fig. 4 is the Raman spectrum of the graphene thin film that embodiment of the present invention 3 obtains;

Fig. 5 is the Raman spectrum of the graphene film obtained in Example 4 of the present invention.

Detailed ways

The technical solutions of the present invention will be further described below in conjunction with specific embodiments.

PE: Purity≥99.99%, Sigma-Aldrich

OLYMPUS-bx53m-microscope WiTec confocal Raman and atomic force microscope system (Raman-AFM)

The quartz tube is heated using a tube furnace.

Embodiment 1-4

A method for growing a graphene film on a catalyst-free insulating substrate, comprising the following steps:

1) Prepare a quartz tube, the length and inner diameter of the quartz tube are shown in Table 1. The two ends of the quartz tube are the raw material end and the base end respectively, and an insulating base (with an area of 1 cm × 2 cm) is placed in the base end of the quartz tube. The insulating base is shown in Table 1. Put a raw material of quality X in the raw material end of the quartz tube, the raw material is polyethylene, vacuumize the quartz tube, seal the quartz tube after vacuuming, so that the pressure inside the quartz tube is P.

2) Heat the raw material end and the base end of the quartz tube for 60 minutes at the same time, and then cool to room temperature 20-25°C with the furnace after heating, and obtain a graphene film on the insulating substrate, wherein the temperature gradient between the raw material end and the base end is shown in the table 1.

Table 1

After the methods of Examples 1-4 are finished, it is found that the graphene film has covered the entire insulating substrate.

Fig. 1 is the Raman D peak and the G peak of the graphene film that the embodiment of the present invention 1 provides on the sapphire substrate, and the D peak is the characterization peak of the graphene with defect; The G peak is caused by the in-plane vibration of sp2 carbon atoms of. Fig. 2 is the Raman G, peak of the graphene film provided in Example 1 of the present invention on the sapphire substrate, and the G, peak is used to characterize the interlayer stacking mode of carbon atoms in the graphene sample. It can be seen from Figure 1 and Figure 2 that a graphene film is obtained on an insulating substrate. .

Fig. 3 is the Raman D peak and G peak of the graphene thin film provided by the embodiment of the present invention 2 on the glass substrate, D peak is the characterization peak of graphene with defects, and G peak is caused by the in-plane vibration of sp2 carbon atoms of. It can be seen from Figure 3 that a graphene film is obtained on an insulating substrate.

The Raman D peak and G peak of the graphene film that Fig. 4 embodiment 3 of the present invention provides on quartz substrate, D peak is the characterization peak of the graphene with defect, and G peak is caused by the in-plane vibration of sp2 carbon atom . As can be seen from Figure 4, a graphene film is obtained on an insulating substrate.

The Raman D peak and G peak of the graphene film that Fig. 5 embodiment 4 of the present invention provides on mica substrate, D peak is the characterization peak of the graphene with defect, and G peak is caused by the in-plane vibration of sp2 carbon atom . As can be seen from Figure 5, a graphene film is obtained on an insulating substrate.

The present invention has been described as an example above, and it should be noted that, without departing from the core of the present invention, any simple deformation, modification or other equivalent replacements that can be made by those skilled in the art without creative labor all fall within the scope of this invention. protection scope of the invention.

Claims (5)

1. a kind of method of no catalyst dielectric base growth graphene film, which comprises the following steps:

1) prepare a quartz ampoule, the both ends of the quartz ampoule are respectively feed end and base terminal, in the base terminal of the quartz ampoule One dielectric base of interior placement, places raw material in the feed end of the quartz ampoule, vacuumizes to the quartz ampoule, takes out true The quartz ampoule is sealed after sky, so that the intraductal pressure of the quartz ampoule is 10^-4~10^-6Pa, wherein the raw material are poly- second Alkene or polypropylene；

2) feed end to the quartz ampoule and base terminal heat 0.5~1h simultaneously, cool to room temperature 20~25 after heating with the furnace DEG C, graphene film is obtained on a dielectric base, wherein the heating temperature of the feed end is 1000~1150 DEG C, the base The heating temperature of bottom end is 200~900 DEG C.

2. the method according to claim 1, wherein in the step 1), the dielectric base be sapphire, Glass, quartz or mica.

3. method according to claim 1 or 2, which is characterized in that in the step 1), the length of the quartz ampoule is 30~50cm, internal diameter are 10~20mm.

4. according to the method described in claim 3, it is characterized in that, the quality of the raw material is 0.5 in the step 1) ~2mg, the area of the dielectric base are 1cm × (2~5) cm.

5. according to the method described in claim 4, it is characterized in that, in the step 2), the feed end and base terminal it Between temperature gradient be 3~30 DEG C/cm.