CN115072711B - Preparation method of graphene nanoribbon - Google Patents
Preparation method of graphene nanoribbon Download PDFInfo
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- CN115072711B CN115072711B CN202110266957.0A CN202110266957A CN115072711B CN 115072711 B CN115072711 B CN 115072711B CN 202110266957 A CN202110266957 A CN 202110266957A CN 115072711 B CN115072711 B CN 115072711B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/06—Graphene nanoribbons
Abstract
The invention provides a preparation method of a graphene nanoribbon, which is based on a catalytic chemical vapor deposition method, wherein the preparation method adopts a crystal material with an atomic-level flatness surface as a growth substrate, adopts metal nanoparticles as a growth catalyst and adopts carbon source gas containing carbon atoms as a growth gas, so that the graphene nanoribbon with a micron-sized length and a neat edge structure can be obtained.
Description
Technical Field
The invention belongs to the technical field of chemical material synthesis, and relates to a preparation method of a graphene nanoribbon.
Background
In recent years, graphene nanoribbons as one-dimensional materials have attracted attention. The special energy band structure of the graphene nanoribbon enables the graphene nanoribbon to have unique electrical, magnetic and optical properties. The graphene nanoribbon has a huge application prospect in the fields of field effect transistors, gas sensing, optical detectors, energy storage and the like.
At present, the methods for preparing graphene nanoribbons mainly have two main types: the first is a top-down method, namely, processing large-area graphene into nanoribbons by micro-nano processing technology; the second type is a bottom-up method, namely, a surface chemical catalytic synthesis technology is adopted to catalyze and polymerize small molecules containing benzene rings on the surface of noble metals into graphene nanoribbons. However, the former has a major problem of insufficient processing precision, resulting in a disordered edge structure of the prepared graphene nanoribbon, thereby losing the intrinsic properties of the graphene nanoribbon; the main problem of the latter is that the preparation cost is high, the length of the prepared graphene nanoribbon is short, generally only tens of nanometers, and the graphene nanoribbon with the size cannot be applied to devices, so that a preparation method of the graphene nanoribbon with high quality, large size and economy is lacked, the mass production of the graphene nanoribbon is realized, and the application of the graphene nanoribbon is greatly limited.
Therefore, a preparation method of the graphene nanoribbon is provided, which is necessary.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a preparation method of graphene nanoribbons, which is used for solving the problem that it is difficult to prepare graphene nanoribbons with high quality, large size and economy in the prior art.
To achieve the above and other related objects, the present invention provides a method for preparing graphene nanoribbons, comprising the steps of:
providing a substrate with atomic level flatness;
forming metal nano-catalyst particles on the substrate;
placing the substrate with the metal nano catalyst particles in a heating furnace for heating, and introducing carbon source gas to form graphene nano belts on the substrate;
and closing the carbon source gas, and cooling to room temperature under the action of the protective gas.
Optionally, the substrate comprises a hexagonal boron nitride substrate or a graphite substrate.
Optionally, the metal nano-catalyst particles include one of iron metal nano-catalyst particles, cobalt metal nano-catalyst particles, nickel metal nano-catalyst particles, alloy nano-catalyst particles, and metal oxide nano-catalyst particles.
Optionally, the carbon source gas includes one of methane, acetylene, and ethanol.
Optionally, the step of forming the graphene nanoribbons on the substrate includes:
providing a tube furnace, and introducing hydrogen and carbon source gas into the tube furnace;
heating under the conditions of 1 standard atmospheric pressure, the temperature of 600-1000 ℃ and the heat preservation time of 20-40 min to enable the carbon source gas to be cracked under the action of the metal nano catalyst particles to form carbon atoms, and the carbon atoms are separated out of the metal nano catalyst particles to grow so as to form the graphene nano belt on the substrate.
Optionally, the flow ratio of the hydrogen gas to the carbon source gas is 1:5.
Optionally, the shielding gas comprises one or a combination of hydrogen, nitrogen, or an inert gas.
Optionally, the length of the graphene nanoribbons formed comprises a micrometer scale.
As described above, the preparation method of the graphene nanoribbon according to the present invention prepares the graphene nanoribbon based on the catalytic chemical vapor deposition method, wherein the method adopts a crystalline material having an atomic-level flatness surface as a growth substrate, adopts metal nanoparticles as a growth catalyst, and adopts a carbon source gas containing carbon atoms as a growth gas, so that the graphene nanoribbon having a micrometer-sized length and a neat edge structure can be obtained, and the preparation method is simple to operate, low in cost, and suitable for mass production.
Drawings
Fig. 1 is a schematic process flow diagram of preparing graphene nanoribbons according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of an apparatus for preparing graphene nanoribbons according to an embodiment of the present invention.
Fig. 3 shows an atomic force microscope picture of graphene nanoribbons prepared in an example of the present invention.
Description of element reference numerals
10. Tube furnace
20. Furnace tube
30. Gas and its preparation method
100. Substrate
200. Metal nano catalyst particles
300. Graphene nanoribbons
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
As described in detail in the embodiments of the present invention, the cross-sectional view of the device structure is not partially enlarged to a general scale for convenience of explanation, and the schematic drawings are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in actual fabrication.
For ease of description, spatially relative terms such as "under", "below", "beneath", "above", "upper" and the like may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that these spatially relative terms are intended to encompass other orientations of the device in use or operation in addition to the orientation depicted in the figures. Furthermore, when a layer is referred to as being "between" two layers, it can be the only layer between the two layers or one or more intervening layers may also be present. As used herein, "between … …" is meant to include both endpoints.
In the context of this application, a structure described as a first feature being "on" a second feature may include embodiments where the first and second features are formed in direct contact, as well as embodiments where additional features are formed between the first and second features, such that the first and second features may not be in direct contact.
It should be noted that, the illustrations provided in the present embodiment merely illustrate the basic concept of the present invention by way of illustration, and only the components related to the present invention are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of each component in actual implementation may be changed at will, and the layout of the components may be more complex.
As shown in fig. 1, the embodiment provides a preparation method of a graphene nanoribbon, which includes the following steps:
providing a substrate with an atomically flat surface;
forming metal nano-catalyst particles on the substrate;
placing the substrate with the metal nano catalyst particles in a heating furnace for heating, and introducing carbon source gas to form graphene nano belts on the substrate;
and closing the carbon source gas, and cooling to room temperature under the action of the protective gas.
The preparation method of the graphene nanoribbon is based on a catalytic chemical vapor deposition method, the method adopts a crystal material with an atomic-level flatness surface as a growth substrate, adopts the metal nano catalyst particles as a growth catalyst, and adopts the carbon source gas containing carbon atoms as a growth gas, so that the graphene nanoribbon with the micrometer-scale length and the neat edge structure can be obtained, and the method is simple to operate, low in cost and suitable for large-scale production.
Referring to fig. 2 to 3, each step of preparing the graphene nanoribbon will be described with reference to the accompanying drawings.
First, referring to fig. 2, a substrate 100 having atomic-level flatness is provided.
As an example, the substrate 100 may include a hexagonal boron nitride substrate or a graphite substrate.
Specifically, the substrate 100 may be a composite substrate structure including a silicon wafer and the hexagonal boron nitride substrate or the graphite substrate on the surface of the silicon wafer, but the structure of the substrate 100 is not limited thereto. The crystal material with the atomic-level flatness surface is used as a growth substrate, so that the formation of the subsequent graphene nanoribbon can be facilitated.
Then, a metal thin film (not shown) is formed on the substrate 100.
As an example, the metal thin film may include one of an iron metal thin film, a cobalt metal thin film, a nickel metal thin film, an alloy thin film, and a metal oxide thin film.
As an example, the method of forming the metal thin film may include one of an evaporation method, a spin coating method, and a dip coating method; the thickness of the metal film may be in the range of
Specifically, by preparing the metal thin film, iron metal, cobalt metal and nickel metal may be formed on the surface of the substrate 100 to prepare for the subsequent preparation of the metal nano-catalyst particles, wherein the kind of the metal thin film is not limited thereto, and when the kind of the metal thin film is selected, a transition metal capable of being co-melted with carbon is selected as a metal material. The method of forming the metal thin film may employ a vapor deposition method, a spin coating method or a dip coating method, is not excessively limited thereto, and the thickness range of the metal thin film formed may beFor example->Etc.
Next, first heating is performed in a heating furnace to form the metal nano-catalyst particles 200.
As an example, the step of forming the metal nano-catalyst particles 200 may include:
providing a tube furnace 10, and introducing hydrogen and argon into the tube furnace 10;
and (3) at 1 standard atmospheric pressure, raising the temperature from room temperature to 600-800 ℃ for 10-20 min, and performing first heating to agglomerate the metal thin film so as to form the metal nano-catalyst particles 200 on the substrate 100.
Specifically, referring to fig. 2, the heating furnace provided in the present embodiment employs the tube furnace 10 with the furnace tube 20, so that a heating furnace with good sealing property, insulation box and temperature control stability can be provided, but the type of heating furnace is not limited thereto. When the substrate 100 having the metal particles on the surface is placed in the furnace tube 20 and the first heating is performed, the metal particles are agglomerated and the metal nano-catalyst particles 200 having a certain size are formed on the substrate 100. Before the first heating, a gas 30, such as hydrogen and argon, is preferably introduced into the tube furnace 10 to facilitate the discharge of impurity gases, such as oxygen, in the tube furnace 20, i.e. the argon may be used as a shielding gas, and the introduced hydrogen may be used as a shielding gas or a reducing gas to facilitate the reduction of some carbon-containing impurity substances generated by the carbon source during the subsequent high-temperature heating. In this embodiment, the temperature is raised from room temperature to 600 ℃ to 800 ℃, such as 600 ℃, 700 ℃, 800 ℃, etc., at 1 standard atmospheric pressure, and the heating time may include 10min to 20min, such as 10min, 15min, 20min, etc., and the heating process parameters related to the first heating are not excessively limited herein. The flow ratio of the hydrogen to the argon may be 2:1, for example, the flow of the hydrogen may be 40SCCM, the flow of the argon may be 20SCCM, and the specific flow may be set as required, which is not excessively limited herein.
Next, a carbon source gas is introduced into the heating furnace and a second heating is performed, so that the graphene nanoribbons 300 are formed on the substrate 100.
As an example, the carbon source gas includes one of methane, acetylene, and ethanol.
As an example, the step of forming the graphene nanoribbons on the substrate 100 includes:
providing a tube furnace 10, and introducing hydrogen and carbon source gas into the tube furnace 10;
and under the condition of 1 standard atmosphere, the temperature is 600-1000 ℃, the heat preservation time is 20-40 min, the second heating is carried out, the carbon source gas is cracked under the action of the metal nano catalyst particles to form carbon atoms, the carbon atoms are separated out from the metal nano catalyst particles, and the graphene nano belt 300 is formed on the substrate 100 by growth.
Specifically, in the second heating, the gas 30 introduced into the furnace tube 20 may include the carbon source gas, such as methane, acetylene, or ethanol, at a high temperature of 600 to 1000 ℃, such as 600 to 800 to 1000 ℃, or the like, for cracking the carbon source gas and obtaining carbon atoms therefrom with the catalytic assistance of the metal nano-catalytic particles 200, and after the carbon concentration in the metal nano-catalytic particles 200 reaches saturation, carbon is precipitated from the surface of the metal nano-catalytic particles 200, thereby growing the graphene nano-ribbons 300, as shown in fig. 3. In this embodiment, the same tube furnace 10 may be used for the second heating as the first heating, and the gas 30 in the furnace tube 20 may further include the continuously introduced hydrogen gas in addition to the introduced carbon source gas during the high temperature heating, so as to reduce some carbon-containing impurities generated by the carbon source gas at high temperature through the hydrogen gas. The flow ratio of the hydrogen gas to the carbon source gas may be 1:5, for example, the flow of the hydrogen gas may be 40SCCM, the flow of the carbon source gas may be 200SCCM, and the specific flow may be set according to the requirement, which is not excessively limited herein.
As an example, the length of the graphene nanoribbons 300 formed may include a micrometer scale.
Specifically, referring to fig. 3, the graphene nanoribbon 300 is prepared based on a catalytic chemical vapor deposition method in the embodiment, and the graphene nanoribbon 300 with a micrometer-sized length and a neat edge structure can be prepared, and the method is simple to operate, low in cost and capable of mass production.
Then, the carbon source gas is turned off, and the temperature is lowered to room temperature under the action of the protective gas.
As an example, the shielding gas may include one or a combination of hydrogen, nitrogen, or an inert gas.
Specifically, in this embodiment, the hydrogen gas is used as the shielding gas to avoid the influence of the external gas on the cooling process of the graphene nanoribbon 300 caused by the tightness of the tube furnace 10 after the carbon source gas is closed, so as to prepare the graphene nanoribbon 300 with high quality, but the kind of the shielding gas is not limited thereto.
The preparation of the graphene nanoribbons according to the present invention is further described below by way of specific examples, including:
example 1
1) A silicon wafer having an oxide layer 300nm thick on the surface thereof was taken and cut into 1cm X1 cm pieces.
2) Hexagonal Boron Nitride (HBN) flakes were prepared on the above silicon wafer by a mechanical lift-off method as a base material for growth.
3) Vapor plating on the substrate material by electron beam vapor platingA nickel metal film of a thickness to act as a catalyst for growth.
4) The above substrate plated with the catalyst was placed in a tube furnace, and while two gases of hydrogen (flow 40 SCCM) and argon (flow 20 SCCM) were introduced, the temperature was gradually raised from room temperature to 800 ℃, the temperature was raised for about 15 minutes, and the air pressure was maintained at 1 standard atmospheric pressure during the temperature raising.
5) After the temperature reaches 800 ℃, stopping introducing argon, and on the basis that the original hydrogen flow, namely the flow rate is 40SCCM, introducing methane gas of 200SCCM as growth gas, and growing at 800 ℃ for 30min, wherein the air pressure is kept at 1 standard atmosphere in the growth process.
6) And after the growth is finished, closing methane gas, naturally cooling to room temperature, and taking out the sample to obtain the graphene nanoribbon.
Example two
1) A piece of highly oriented pyrolytic graphite was taken, with dimensions of about 1cm. Times.1 cm.
2) Vapor plating on the substrate material by electron beam vapor platingIron metal thin film of thickness, acting as a catalyst for growth.
3) The above substrate plated with the catalyst was placed in a tube furnace, and gradually heated from room temperature to 800 ℃ in an atmosphere of two protective gases of hydrogen (flow 40 SCCM) and argon (flow 20 SCCM), the temperature was raised for about 15 minutes, and the air pressure was maintained at 1 standard atmospheric pressure during the temperature raising.
4) After the temperature reaches 800 ℃, stopping introducing argon, and on the basis that the original hydrogen flow, namely the flow rate is 40SCCM, introducing methane gas of 200SCCM as growth gas, and growing at 800 ℃ for 30min, wherein the air pressure is kept at 1 standard atmosphere in the growth process.
5) And after the growth is finished, closing methane gas, naturally cooling to room temperature, and taking out the sample to obtain the graphene nanoribbon.
In summary, the invention provides a preparation method of graphene nanoribbons, which is based on a catalytic chemical vapor deposition method for preparing the graphene nanoribbons, wherein the method adopts a crystal material with an atomic-level planeness surface as a growth substrate, adopts metal nanoparticles as a growth catalyst, and adopts carbon source gas containing carbon atoms as a growth gas, so that the graphene nanoribbons with micron-level length and orderly edge structures can be obtained.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (7)
1. The preparation method of the graphene nanoribbon is characterized by comprising the following steps of:
providing a substrate with atomic level flatness;
forming a metal nano catalyst film on the substrate;
heating the substrate with the metal nano catalyst film in a heating furnace to enable the metal nano catalyst film to be agglomerated to form metal nano catalyst particles, and introducing carbon source gas, wherein the carbon source gas is cracked under the action of the metal nano catalyst particles to form carbon atoms, and the carbon atoms are separated out of the metal nano catalyst particles to grow so as to form graphene nano belts on the substrate; wherein the heating temperature is 600-1000 ℃; the metal nano catalyst particles comprise one of iron metal nano catalyst particles, cobalt metal nano catalyst particles and nickel metal nano catalyst particles;
and closing the carbon source gas, and cooling to room temperature under the action of the protective gas.
2. The method for preparing the graphene nanoribbon according to claim 1, wherein: the substrate comprises a hexagonal boron nitride substrate or a graphite substrate.
3. The method for preparing the graphene nanoribbon according to claim 1, wherein: the carbon source gas comprises one of methane, acetylene and ethanol.
4. The method of preparing a graphene nanoribbon according to claim 1, wherein the step of forming the graphene nanoribbon on the substrate comprises:
providing a tube furnace, and introducing hydrogen and carbon source gas into the tube furnace;
heating under the condition of 1 standard atmospheric pressure and the heat preservation time of 20-40 min.
5. The method for preparing the graphene nanoribbon according to claim 4, wherein: the flow ratio of the hydrogen to the carbon source gas is 1:5.
6. The method for preparing the graphene nanoribbon according to claim 1, wherein: the shielding gas comprises one or a combination of hydrogen, nitrogen or inert gases.
7. The method for preparing the graphene nanoribbon according to claim 1, wherein: the length of the graphene nanoribbons formed includes a micrometer scale.
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