CN204324888U - A kind of nonmetallic substrate intercalation formula N doping prepares the fixture of Graphene - Google Patents

Abstract

The utility model relates to the fixture that a kind of nonmetallic substrate intercalation formula N doping prepares Graphene, comprise the panel that polylith be arranged in parallel up and down, be provided with the pillar for fixing adjacent described panel between adjacent described panel, between adjacent described panel, can nonmetallic substrate be put into.The utility model utilizes laminar stent holder directly doped growing Graphene on nonmetallic substrate, growth has the nonmetallic substrate of Graphene can be directly used in the application of the electron devices such as transparency electrode, decrease the operation in the electron device preparation process such as graphene transparent electrode, reduce cost of manufacture.

Description

A non-metallic substrate intercalation nitrogen doping fixture for preparing graphene

technical field

The utility model relates to the technical field of graphene preparation, in particular to a non-metallic substrate intercalation type nitrogen doping fixture for preparing graphene.

Background technique

Graphene is a honeycomb single-layer carbon material composed of carbon atoms according to sp2 hybridization bonds. Its special crystal structure endows graphene with many excellent physical properties, such as room temperature quantum Hall effect, high carrier mobility, high thermal Conductivity, long-range ballistic transport properties, etc. These excellent physical properties make graphene one of the most promising electronic materials.

At present, the methods for preparing graphene mainly include mechanical exfoliation, SiC crystal epitaxial growth, graphite oxide reduction and chemical vapor deposition on transition metals. The mechanical exfoliation method is mainly used in the laboratory to prepare high-quality graphene samples, but the prepared graphene is small in size, the number of layers is difficult to control, and the yield is low. SiC crystal epitaxial growth method can prepare large-scale multilayer graphene, but SiC single crystal is expensive, which leads to high preparation cost. The graphite oxide reduction method can prepare a large number of multilayer graphene, but it is difficult to separate the different layers of graphene, and the prepared graphene is small in size and poor in quality. At present, the method of preparing large-area high-quality graphene is mainly the chemical vapor deposition method on metal films such as copper and nickel.

At present, the methods for preparing graphene mainly include chemical vapor deposition (CVD), solvothermal method, electrothermal doping method, etc., among which CVD method is widely used to prepare large-area high-quality graphene film materials. These graphenes prepared by CVD mainly use transition metal substrates as catalysts, such as copper foil, nickel foil, etc. Although the quality of graphene prepared by using metal substrates as catalysts is good, it cannot be directly applied to electronic devices because it grows on the surface of metal substrates.

Therefore, it is necessary to first transfer the graphene on the metal substrate to a specific substrate through an intermediate medium such as polymethyl methacrylate (PMMA), thermal release tape, etc. During the transfer process, it is easy to introduce a large number of impurities. This process is not only complicated and expensive, but also easily causes damage to the structure of graphene. Therefore, in order to obtain high-quality graphene, it is necessary to chemically dope the transferred graphene, which increases the preparation cost of graphene.

Utility model content

The technical problem to be solved by the utility model is to provide a non-metallic substrate intercalation type nitrogen doping fixture for preparing graphene directly doped with graphene on a non-metallic backing plate.

The technical scheme that the utility model solves the problems of the technologies described above is as follows:

A non-metallic substrate intercalation type nitrogen-doped fixture for preparing graphene, including a plurality of panels arranged in parallel up and down, adjacent panels are provided with pillars for fixing adjacent panels, adjacent panels A non-metallic substrate can be placed between the panels.

Further, the shape of the panel is circular.

Further, the shape of the panel is a rectangle, etc., and any shape that can place the non-metallic substrate stably is acceptable.

Further, the panel is a solid panel.

Further, the panel is a panel with mesh.

Further, the materials of the panels and the pillars are both quartz.

The method for preparing graphene by using the above-mentioned clamp to carry out intercalation type nitrogen doping of a non-metallic substrate comprises the following steps:

Step 1, cleaning and pretreating the jig and the non-metallic substrate;

Step 2, put the non-metallic substrate on the jig, put the jig with the non-metallic substrate into the quartz tube, and extract the air in the quartz tube to below 0Pa;

Step 3, feed carrier gas into the quartz tube, raise the temperature inside the tube to 800-1200°C, and keep it warm for 30-80min;

Step 4, feed carbon source gas and nitrogen source gas into the quartz tube for doped growth of graphene (if the fixture contains carbon, it can be used as carbon source, just feed nitrogen source gas), and the growth time is 20-100min;

Step 5, after the growth is completed, stop heating, turn off the carbon source gas and nitrogen source gas, continue to feed the carrier gas, wait for the inside of the quartz tube to cool down to room temperature, take out the jig and the non-metallic substrate, and remove the non-metallic substrate from the jig, That is, a non-metallic substrate with graphene grown on it is obtained.

On the basis of the above technical solutions, the utility model can also be improved as follows.

Further, the cleaning and pretreatment of the fixture in the first step is to place the fixture in acetone and ethanol in sequence for ultrasonic cleaning for 10-30 minutes, and then put it in an oven for drying at 60-80°C.

Further, the cleaning and pretreatment method of the non-metallic substrate in the step 1 is to ultrasonically clean the non-metallic substrate in a solution mixed with one or more of acetone, isopropanol, ethanol, and deionized water , the cleaning time is 15-30min, and then blow dry with nitrogen gas with a purity of 99.999%.

Further, the carrier gas is hydrogen or argon.

Further, the carbon source gas is methane or ethylene or acetylene.

Further, the nitrogen source gas is ammonia gas.

Further, the non-metallic substrate is one or more of a silicon wafer or a silicon wafer with a silicon dioxide layer or a silicon wafer with a silicon nitride coating, a quartz wafer, and sapphire.

The beneficial effects of the utility model are: the utility model directly utilizes the non-metallic liner to dope and grow graphene, and the grown non-metallic liner with graphene can be directly used for the introduction of electronic devices such as transparent electrodes, avoiding the After the graphene is grown on a metal substrate, it needs to be transferred, while avoiding the structure damage of the graphene during the transfer process, reducing the steps in the preparation process of electronic devices such as graphene transparent electrodes, and reducing the production cost.

Description of drawings

Fig. 1 is the structural representation of fixture of the present utility model, and the shape of panel is rectangle among the accompanying drawings;

Fig. 2 is a structural schematic diagram of the fixture of the present invention, in which the shape of the panel is circular.

In the accompanying drawings, the list of parts represented by each label is as follows:

1. Panel, 2. Pillar.

Detailed ways

The principles and features of the present utility model are described below in conjunction with the accompanying drawings, and the examples given are only used to explain the utility model, and are not used to limit the scope of the utility model.

The fixture described in the utility model includes a plurality of panels 1 arranged in parallel up and down, and a pillar 2 for fixing the adjacent panels 1 is arranged between the adjacent panels 1, and between the adjacent panels 1 The non-metallic substrate can be put in, and the shape of the panel 1 is circular or rectangular, etc., and various shapes that can place the non-metallic substrate smoothly are all available. The panel 1 is a solid panel or a panel with mesh holes, so The materials of the panel 1 and the pillar 2 are both quartz.

The method for preparing graphene by using the layered support fixture described in the utility model to carry out non-metallic substrate intercalation type nitrogen doping includes the following embodiments:

Embodiment one

Using a plurality of circular panels 1 arranged in parallel, adjacent panels 1 are fixedly connected with a layered support fixture through pillars 2, and non-metallic substrates can be placed between adjacent panels 1, as shown in Figure 2 , put the bracket into acetone and ethanol in turn to clean for 10 minutes respectively, and then put the cleaned layered bracket fixture into an oven at 60°C for drying. Place the silicon wafer in acetone for ultrasonic cleaning for 15 min, and then dry it with nitrogen gas with a purity of 99.999%. Place the cleaned and pretreated silicon wafer on the panel 1, put the layer bracket fixture with the silicon wafer into the quartz tube, use the air pump to extract the air in the quartz tube to below 0Pa, and then pass hydrogen into the quartz tube and argon, raise the temperature in the quartz tube to 800°C, keep it warm for 80 minutes, and feed methane and ammonia into the quartz tube to grow graphene doped (if the layer bracket fixture contains carbon, it can be used as a carbon source, just feed Nitrogen source gas), the growth time is 20min, stop heating after the growth is completed, stop feeding methane and ammonia, continue to feed hydrogen and argon, and take out the layered support fixture and non-metallic substrate after the temperature in the quartz tube drops to room temperature , remove the non-metallic substrate from the layered support fixture to obtain the non-metallic substrate grown with graphene.

Embodiment two

Using a plurality of square panels 1 arranged in parallel, adjacent panels 1 are fixedly connected to each other through pillars 2. Non-metallic substrates can be placed between adjacent panels 1, as shown in Figure 1, Put the bracket into acetone and ethanol in turn to clean for 30 minutes respectively, and then put the cleaned layered bracket fixture into an oven with a temperature of 80°C to dry. Place the quartz plate in ethanol for ultrasonic cleaning for 15 min, and then dry it with nitrogen gas with a purity of 99.999%. Place the cleaned and pretreated quartz slices on the panel 1, put the layered bracket fixture with the quartz slices into the quartz tube, use the air pump to extract the air in the quartz tube to below 0 Pa, and pass hydrogen and gas into the quartz tube. Argon, raise the temperature inside the quartz tube to 1200°C, keep it warm for 30 minutes, feed ethylene and ammonia gas into the quartz tube to grow graphene (if the layered support fixture contains carbon, it can be used as a carbon source, just feed nitrogen Source gas), the growth time is 100min, stop heating after the growth is completed, stop feeding ethylene and ammonia, continue feeding hydrogen and argon, and take out the layered support fixture and non-metallic substrate after the temperature in the quartz tube drops to room temperature, The non-metallic substrate is removed from the layered support fixture to obtain the non-metallic substrate with graphene grown on it.

Embodiment three

Using a plurality of circular panels 1 arranged in parallel, adjacent panels 1 are fixedly connected with a layered support fixture through pillars 2, and non-metallic substrates can be placed between adjacent panels 1, as shown in Figure 2 , put the brackets in acetone and ethanol in turn for 20 minutes, and then put the cleaned layered bracket fixtures into an oven at 70°C for drying. The sapphire was ultrasonically cleaned in deionized water for 15 minutes, and then dried with nitrogen gas with a purity of 99.999%. Place the cleaned and pretreated sapphire on the panel 1, put the layered bracket fixture with sapphire into the quartz tube, use the air pump to extract the air in the quartz tube to below 0Pa, and pass hydrogen and argon into the quartz tube , raise the temperature inside the quartz tube to 1000°C, keep it warm for 50 minutes, pass acetylene and ammonia gas into the quartz tube to do the doped growth of graphene (if the layer bracket fixture contains carbon, it can be used as a carbon source, only need to pass in nitrogen source gas ), the growth time is 60min. After the growth is completed, stop heating, stop feeding acetylene and ammonia, continue feeding hydrogen and argon, and take out the layered support fixture and non-metallic substrate after the temperature in the quartz tube drops to room temperature, and remove the Remove the non-metallic substrate from the type support fixture to obtain the non-metallic substrate with graphene grown on it.

The above descriptions are only preferred embodiments of the present utility model, and are not intended to limit the present utility model. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present utility model shall be included in this utility model. within the scope of protection of utility models.

Claims (4)

1. a nonmetallic substrate intercalation formula N doping prepares the fixture of Graphene, it is characterized in that, comprise the panel (1) that polylith be arranged in parallel up and down, be provided with the pillar (2) for fixing adjacent described panel between adjacent described panel (1), between adjacent described panel (1), can nonmetallic substrate be put into.

2. a kind of nonmetallic substrate intercalation formula N doping according to claim 1 prepares the fixture of Graphene, it is characterized in that, the shape of described panel (1) is circular or rectangle.

3. a kind of nonmetallic substrate intercalation formula N doping according to claim 1 and 2 prepares the fixture of Graphene, it is characterized in that, described panel is solid panels or band mesh panel.

4. a kind of nonmetallic substrate intercalation formula N doping according to claim 1 and 2 prepares the fixture of Graphene, and it is characterized in that, the material of described panel (1) and described pillar (2) is quartz.