CN114506843A - Method for rapidly preparing graphene film on non-metal substrate - Google Patents
Method for rapidly preparing graphene film on non-metal substrate Download PDFInfo
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- CN114506843A CN114506843A CN202210175355.9A CN202210175355A CN114506843A CN 114506843 A CN114506843 A CN 114506843A CN 202210175355 A CN202210175355 A CN 202210175355A CN 114506843 A CN114506843 A CN 114506843A
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Abstract
The invention discloses a method for quickly preparing a graphene film on a nonmetal substrate, which comprises the following steps: step (1): covering a non-metal substrate on two surfaces of a conductive material with carbon source organic reagents coated on the surfaces to form a non-metal substrate/carbon source organic reagent/conductive material/carbon source organic reagent/non-metal substrate interlayer; step (2): and (2) placing the interlayer obtained in the step (1) in an electrode discharge chamber, and carrying out discharge treatment on the interlayer in a vacuum state. According to the invention, the graphene film can grow on the non-metal substrate in a short time by utilizing the fact that high current is instantaneously passed through the graphene paper to generate high temperature (>2000 ℃), and the problems of long time, high cost and the like in the existing graphene film preparation process are effectively solved.
Description
Technical Field
The invention relates to the technical field of graphene film preparation, in particular to a method for quickly preparing a graphene film on a non-metal substrate.
Background
Graphene is a polymer made of carbon atoms in sp2The two-dimensional carbon nanomaterial which is formed by the hybrid tracks and has a honeycomb lattice in a hexagonal shape has excellent performances such as extremely high mechanical strength and ultrahigh carrier mobility, and is considered to have wide application prospects in various fields.
The existing large-area graphene film is mainly prepared on a copper substrate by a chemical vapor deposition method, and generally needs to be transferred to a target substrate (generally a non-metal substrate such as a silicon wafer, glass, an acrylic plate and the like) during application, so that the transfer process not only increases the preparation cost, but also easily damages the graphene film and introduces impurities. Another method is to grow directly on a non-metallic substrate, also typically by chemical vapor deposition, but generally requires higher temperatures (>1000 degrees celsius), long growth times (tens of minutes to hours), and high defects.
Disclosure of Invention
In view of the above disadvantages, the present invention aims to provide a method for rapidly preparing a graphene film on a non-metal substrate, which can grow a graphene film on a non-metal substrate in a short time by using a high current instantaneously passed through graphene paper to generate a high temperature (>2000 ℃), and effectively solves the problems of long time, high cost, and the like in the existing graphene film preparation process.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for rapidly preparing a graphene film on a non-metal substrate, which comprises the following steps:
step (1): covering a non-metal substrate on two surfaces of a conductive material with carbon source organic reagents coated on the surfaces to form a non-metal substrate/carbon source organic reagent/conductive material/carbon source organic reagent/non-metal substrate interlayer;
step (2): and (2) placing the interlayer obtained in the step (1) in an electrode discharge chamber, and carrying out discharge treatment on the interlayer in a vacuum state.
The principle of the method for preparing the graphene film on the non-metal substrate is as follows: coating organic reagents serving as carbon sources on two sides of a conductive material, and then covering the two sides of the conductive material coated with the organic reagents with a non-metal substrate to form a sandwich structure (non-metal substrate/carbon source organic reagent/conductive material/carbon source organic reagent/non-metal substrate sandwich); and then placing the sandwich structure (the sandwich layer of the non-metal substrate/the carbon source organic reagent/the conductive material/the carbon source organic reagent/the non-metal substrate) in an electrode discharge chamber, carrying out discharge treatment on the sandwich layer in a vacuum state, wherein a large amount of Joule heat generated in the short-time high-voltage discharge treatment process can thermally crack the carbon source into carbon active species, and rapidly finishing recombination on the non-metal substrates on the two sides to obtain graphene. For example, two ends of a conductive material such as graphite paper are connected with electrodes, organic reagents such as n-hexane (or ethanol, acetone and the like) are coated on two sides of the graphite paper, then the two sides of the graphite paper are clamped by non-metal substrates (such as quartz plates, glass and the like), then the graphite paper is heated by electrifying, the temperature is adjusted by the current, and the reaction time is adjusted by the electrifying time, so that the graphene film can be rapidly prepared on the non-metal substrates.
Further, the carbon source organic reagent is any carbon-containing liquid organic reagent; the graphene may be doped with a liquid organic reagent containing no heteroatom such as sulfur or nitrogen, such as N-hexane, ethanol, or acetone, or with a liquid organic reagent containing a heteroatom such as sulfur or nitrogen, such as acetonitrile, N-dimethylformamide, dimethyl sulfoxide, pyridine, or carbon disulfide, or with a polymer such as polyethylene glycol.
Further, non-metallic substrates include, but are not limited to, silicon wafers, quartz wafers, boron nitride, glass, alumina, silicon wafers with silica coatings, mica wafers, sapphire, and the like.
Further, the conductive material includes, but is not limited to, graphene felt, carbon fiber cloth, and metal foils such as gold, silver, copper, platinum, tungsten, iron, chromium, cobalt, nickel, and the like.
Further, the working parameters of the electrode discharge chamber are as follows: the voltage is 180-250V, preferably 200-220V; the discharge time is 300-1000ms, preferably 300-600 ms.
The reaction temperature is adjusted by the voltage and the discharge time together, the higher the voltage is, the shorter the discharge time is, the larger the heat obtained by the reaction system is, and the higher the quality of the graphene obtained on the non-metal substrate is; the reaction time is adjusted by the energization time.
Furthermore, the electrode discharge chamber is at least connected with a power supply anode, a power supply cathode, a vacuum device and a controller, and the power supply anode and the power supply cathode are connected with two ends of the graphite paper to realize the heating of the graphite paper by current; the vacuum device can be a device such as a vacuum pump and the like and is used for vacuumizing the electrode discharge chamber; the controller can adopt a relay matched controller, thereby realizing the control of the discharge working parameters. For example, the electrode discharge chamber can be modified by a plastic vacuum drying box (three holes are formed and are respectively connected with a positive electrode, a negative electrode and a vacuum pump of a power supply, a vacuum meter is arranged on the top of the cover, and vacuumizing treatment is carried out before each reaction).
Further, before the interlayer is subjected to the discharge treatment in the step (2), the method further comprises the following steps: the reaction chamber is vacuumized, and the sample is pretreated at the voltage of 130-150V within the time of 300-1000 ms.
The pretreatment step in the present invention is mainly used for a carbon source reagent having low volatility such as esters (e.g., methyl benzoate).
In summary, the invention has the following advantages:
1) the invention provides a method for rapidly preparing a graphene film on a non-metal substrate, which can grow the graphene film on the non-metal substrate in a short time by utilizing the fact that high current is instantaneously passed through graphene paper to generate high temperature (>2000 ℃), and effectively solves the problems of long time, high cost and the like in the existing graphene film preparation process.
2) Compared with the method for preparing the graphene film by adopting the conventional chemical vapor deposition reaction chamber, the method has the following advantages: 1. the device is simple and the cost is low; 2. the reaction position is directly heated, and the energy utilization rate is high; 3. the temperature is high (>2000 ℃), and a high-quality graphene film can be obtained.
Drawings
FIG. 1 is a schematic view of a sandwich structure according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Thus, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a method for rapidly preparing a graphene film on a non-metal substrate, as shown in fig. 1, comprising the following steps:
(1) preparation of a reaction system: taking graphite paper with the length of 10cm and the width of 6cm, and respectively spin-coating 10ml of n-hexane on two surfaces of the graphite paper; then, two surfaces of the substrate are respectively covered by quartz plates (with the length of 5cm and the width of 2cm), and the substrate is clamped on two sides by alligator clips for fixing, so that an interlayer of a nonmetal substrate/a carbon source organic reagent/a conductive material/a carbon source organic reagent/a nonmetal substrate interlayer-quartz plates/n-hexane/graphite paper/n-hexane/quartz plates is obtained;
(2) preparing a graphene film: placing the sandwich layer of the quartz plate/n-hexane/graphite paper/n-hexane/quartz plate in a reaction chamber, and closing the reaction chamber after two ends of the graphite paper are respectively connected with a positive electrode and a negative electrode of a power supply; after the reaction chamber is vacuumized, the interlayer is subjected to discharge treatment under the discharge condition of 300ms at 220V by a controller; and opening the reaction chamber when the voltage of the reaction chamber is reduced to 0V, and taking out the quartz plate substrate to obtain the graphene on the quartz plate substrate.
The graphene film obtained by the embodiment has a defect-free structure and has the characteristics of good appearance and excellent electrical properties.
It should be noted that the present embodiment is only used for illustrating and explaining the technical solutions and technical concepts of the present invention, and is not used for limiting the present invention; it is particularly noted that the carbon source organic reagent in this example is any liquid organic reagent; for example, N-hexane is replaced by liquid organic reagents which do not contain heteroatoms such as sulfur or nitrogen, such as ethanol and acetone, or polymers such as polyethylene glycol, or liquid organic reagents which contain heteroatoms such as sulfur or nitrogen, such as acetonitrile, N-dimethylformamide, dimethyl sulfoxide, pyridine and carbon disulfide, so as to realize doping of graphene; in this example, the quartz plate can be replaced by other conventional non-metallic substrates such as silicon wafer, boron nitride, glass, alumina, silicon wafer with silica coating, mica plate, sapphire, etc. In this embodiment, the graphite paper can be replaced by other conductive materials such as graphene felt, carbon fiber cloth, and metal foils such as gold, silver, copper, platinum, tungsten, iron, chromium, cobalt, nickel, etc.; the graphene film without a defect structure and with excellent morphology and electrical properties can be successfully prepared, and the method is not repeated.
Example 2
The present example provides a method for rapidly preparing a graphene thin film on a non-metal substrate, which is different from example 1 only in that: the working parameters of the electrode discharge chamber are as follows: the voltage is 180V, and the discharge time is 900 ms; the rest steps and parameters are the same.
Example 3
The present example provides a method for rapidly preparing a graphene thin film on a non-metal substrate, which is different from example 1 only in that: the working parameters of the electrode discharge chamber are as follows: the voltage is 200V, and the discharge time is 400 ms; the rest steps and parameters are the same.
Example 4
The present example provides a method for rapidly preparing a graphene thin film on a non-metal substrate, which is different from example 1 only in that: adjusting a carbon source reagent into methyl benzoate; before the discharge treatment is carried out to sandwich structure, still include: vacuumizing the reaction chamber, and pretreating the sample within 500ms under the voltage of 140V; the rest steps and parameters are the same.
The foregoing is merely exemplary and illustrative of the present invention and it is within the purview of one skilled in the art to modify or supplement the embodiments described or to substitute similar ones without the exercise of inventive faculty, and still fall within the scope of the claims.
Claims (6)
1. A method for rapidly preparing a graphene film on a non-metal substrate is characterized by comprising the following steps:
step (1): covering a non-metal substrate on two surfaces of a conductive material with carbon source organic reagents coated on the surfaces to form a non-metal substrate/carbon source organic reagent/conductive material/carbon source organic reagent/non-metal substrate interlayer;
step (2): and (2) placing the interlayer obtained in the step (1) in an electrode discharge chamber, and carrying out discharge treatment on the interlayer in a vacuum state.
2. The method for rapidly preparing the graphene thin film on the non-metallic substrate according to claim 1, wherein the carbon source organic reagent is a carbon-containing liquid organic reagent.
3. The method for rapidly preparing a graphene thin film on a non-metallic substrate according to claim 1, wherein the non-metallic substrate comprises at least one of a silicon wafer, a quartz plate, boron nitride, glass, alumina, a silicon wafer with a silica coating, a mica plate and sapphire.
4. The method for rapidly preparing a graphene film on a non-metallic substrate according to claim 1, wherein the conductive material comprises at least one of a graphene felt, a carbon fiber cloth and a metal foil.
5. The method for rapidly preparing the graphene film on the non-metallic substrate according to claim 1, wherein the working parameters of the electrode discharge chamber are as follows: the voltage is 180-250V, and the discharge time is 300-1000 ms.
6. The method for rapidly preparing the graphene film on the non-metallic substrate according to claim 1, wherein before the step (2) of performing the discharge treatment on the interlayer, the method further comprises: the reaction chamber is vacuumized, and the sample is pretreated at the voltage of 130-150V within the time of 300-1000 ms.
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