CN114804082A - Step-regulated graphene sapphire wafer and preparation method thereof - Google Patents
Step-regulated graphene sapphire wafer and preparation method thereof Download PDFInfo
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Abstract
The invention provides a step-regulated graphene sapphire wafer and a preparation method thereof. The preparation method comprises the following steps: pretreating the sapphire wafer; placing the pretreated sapphire wafer substrate in a graphite disc, heating by electromagnetic induction, pumping the pressure to 10Pa, and setting the growth pressure, the growth temperature and the growth time; when the temperature rises to 200-500 ℃, introducing argon, and when the temperature continues to rise to 600-800 ℃, introducing hydrogen; when the temperature is raised to the growth temperature, introducing growth gas; and after the growth is finished, stopping introducing growth gas, cooling in an argon and hydrogen environment, stopping introducing hydrogen when the temperature is lower than 500 ℃, stopping introducing argon when the temperature is lower than 100 ℃, and performing vacuum breaking treatment to obtain the graphene sapphire wafer. The high-quality graphene sapphire wafer can be prepared by the method.
Description
Technical Field
The invention relates to a preparation method of graphene, in particular to a preparation method of a step-regulated graphene sapphire wafer, and belongs to the technical field of graphene preparation.
Background
The graphene is sp 2 Hybrid bonded carbonsA honeycomb-shaped two-dimensional atomic crystal composed of atoms. In 2004, Geim et al, university of Manchester, UK, successfully separated graphene from graphite for the first time by a micromechanical stripping method, and performed a series of characterization and electrical property measurements on the graphene material, and found the unique field effect characteristic of the graphene material. The proposal of the simple stripping method and the discovery of excellent properties of graphene have triggered a global hot tide in graphene research. Graphene has ultra-high carrier mobility (-105 cm) 2 V -1 s -1 ) Ultra high thermal conductivity (-5300W m) -1 K -1 ) Good mechanical strength (1.0 TPa), high light transmittance (2.3% per layer), and the like. The graphene has extremely high chemical stability, is easy to prepare in a large scale, and has wide application prospects in the fields of materials science, micro-nano processing, transparent conductive films, flexible batteries, super capacitors, optical devices, biomedicine, field effect transistors, integrated circuits and the like.
At present, the main preparation methods of graphene include a mechanical exfoliation method, a liquid phase exfoliation method, a redox method, a silicon carbide epitaxy method, an organic synthesis method, a CVD method, and the like. The CVD method has the advantages of high graphene preparation quality, good controllability, high release capacity and the like, and thus becomes a mainstream preparation method for large-scale production of high-quality graphene films. At present, the CVD preparation of large-area and high-quality graphene films is mainly realized on metal substrates, and the reaction principle is very clear. However, in order to meet the potential application requirements of graphene electronic devices, the graphene thin film is often required to be transferred from a metal substrate to an insulating substrate, such as silicon dioxide/silicon, quartz, sapphire and the like. It should be noted that, the existing transfer technology is complex in process, time-consuming and tedious, and most importantly, the graphene film is inevitably damaged, especially for the transfer of the large-area wafer-level graphene film, the integrity of the transferred graphene is usually low, the damage rate is high, and the subsequent device processing is undoubtedly seriously affected. If the graphene can be directly grown on the insulating substrate, the problems of pollution, damage and the like caused by the transfer process are avoided, and the industrial preparation and application of the graphene can be further promoted.
There are many kinds of insulating substrates, and they are classified into a single crystal substrate (e.g., sapphire, silicon carbide, single crystal silicon), a polycrystalline substrate (e.g., polycrystalline silicon), and an amorphous substrate (e.g., amorphous silicon dioxide) according to their lattice structures. Among them, sapphire is an alumina crystal material, which is advantageous from both the preparation and application aspects of analysis. Firstly, the sapphire production and preparation process is mature in technology, can be produced in batch, and is high in stability, the melting point is 1700 ℃, and the sapphire can bear high growth temperature. And the price is cheap, and currently, the 2-inch single-throw substrate is about 25 RMB, and the 4-inch substrate is about 100 RMB. Secondly, the sapphire has excellent optical property, thermal property and chemical stability, and is widely applied to many fields of scientific research, national defense and military and production life. Window materials for infrared devices, high intensity lasers; substrate materials for semiconductor light emitting diodes, large scale integrated circuits, and the like; the glass can be used in the fields of mobile phone cover plate glass, camera lens and the like.
The growth of graphene on sapphire wafers still presents some problems. Since the growth of graphene on sapphire substrates is completely different from that of metal substrates. Sapphire has low growth catalytic activity on graphene, so that carbon source cracking is difficult during graphene preparation, and the migration barrier of active species is high, which causes poor quality of the grown graphene. In order to solve this problem, high temperature CVD method, plasma enhanced chemical vapor deposition method, metal-assisted method, and gas-assisted method have been proposed in succession. However, the quality of the graphene prepared by the method can not be comparable to that of the graphene prepared on the metal substrate. This is due to the fact that at high temperatures the sapphire surface will produce certain cleavage products, which are different from the cleavage products of graphene grown on metal substrates. And thus do not have a high catalytic effect. It is still highly desirable to explore the high quality growth of graphene on sapphire wafers.
In conclusion, a direct preparation method of the high-quality graphene sapphire wafer is developed, the growth mechanism of the high-quality graphene is further and deeply explored, and the key core problem of the sapphire wafer material in the application process is solved.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a one-step preparation method of a graphene sapphire wafer with step control.
In order to achieve the technical purpose, the invention firstly provides a preparation method of a step-regulated graphene sapphire wafer, which comprises the following steps:
pretreating the sapphire wafer;
placing the pretreated sapphire substrate in a graphite disc, heating by electromagnetic induction, pumping the pressure to 10Pa, and setting the growth pressure, the growth temperature and the growth time;
when the temperature rises to 200-500 ℃, introducing argon, and when the temperature continues to rise to 600-800 ℃, introducing hydrogen;
when the temperature is raised to the growth temperature, introducing growth gas;
and after the growth is finished, stopping introducing growth gas, cooling in an argon and hydrogen environment, closing hydrogen when the temperature is lower than 500 ℃, closing argon when the temperature is lower than 100 ℃, and performing vacuum breaking treatment to obtain the graphene sapphire wafer.
The preparation method of the step-regulated graphene sapphire wafer is a direct preparation method of a high-quality graphene sapphire wafer, and the step has a regulating effect on the growth of high-quality graphene under a very high temperature condition. The very high temperature is slightly higher than the ordinary temperature, and generally refers to 1200-1500 ℃. The sapphire wafers used are C-plane sapphire wafers, wafer sizes include, but are not limited to, two inches, four inches, six inches, eight inches, and the like.
In one embodiment of the invention, the growth pressure is 2000Pa to 5000 Pa; preferably the growth pressure is 2000Pa, 3000Pa or 5000 Pa; more preferably, the growth pressure is 3000 Pa.
In one embodiment of the invention, the growth temperature is 1275 ℃ to 1400 ℃; preferably the growth temperature is 1275 ℃, 1300 ℃, 1325 ℃, 1350 ℃, 1375 ℃ or 1400 ℃. More preferably, the growth temperature is 1350 ℃.
In one embodiment of the invention, the growth time is 20min to 60 min; preferably, the growth time is 20min, 30min or 60 min; more preferably, the growth time is 30 min.
In one embodiment of the present invention, the flow rate of argon gas is 500sccm to 1000 sccm. The flow rate of the hydrogen gas is 300sccm to 500 sccm.
In one embodiment of the invention, the growth gas is methane. Wherein the flow rate of the growth gas is 120sccm-200 sccm.
In one embodiment of the present invention, the pretreatment comprises the steps of:
and (3) respectively washing the sapphire wafer in alcohol/acetone and water for three times, and drying the sapphire wafer by using a nitrogen gun for later use.
Specifically, the preparation method of the step-regulated graphene sapphire wafer comprises the following specific preparation steps:
(1) and preprocessing the purchased sapphire wafer. Respectively washing for three times under the conditions of alcohol/acetone and deionized water, and blow-drying by a nitrogen gun for later use;
(2) placing the graphite disc in cold wall electromagnetic induction heating equipment, opening the heating furnace, taking out the graphite disc, placing the cleaned sapphire substrate to be used in the graphite disc, loading the graphite disc into a tray, lifting the graphite disc to the center of an induction coil, and closing a cabin door to enable the system to be in a closed state;
(3) and opening a vacuum pump, pumping the pressure of the heating furnace system to 10Pa, setting an European land surface after the vacuum index is stable, and determining the growth pressure required by the reaction. After the vacuum reading again stabilized.
(4) Opening a temperature control system, and setting the growth temperature and the growth time required by the reaction;
(5) and opening the mass flow controller to introduce argon when the temperature rises to 500 ℃, and opening the mass flow controller to introduce hydrogen when the temperature continues to rise to 800 ℃. The argon and hydrogen flow rates were set according to the parameters in the examples;
(6) when the temperature rises to the set growth temperature, opening the mass flow controller and introducing growth gas methane, wherein the methane flow is set according to the parameters in the example;
(7) after the growth is finished, the mass flow controller is closed to turn off methane, the temperature is reduced in the argon and hydrogen environment, when the temperature is lower than 500 ℃, the mass flow controller is closed to turn off hydrogen, and the graphite plate can be lowered to the cabin door.
(8) When the temperature is lower than 100 ℃. And closing the mass flow controller, closing the argon, closing the vacuum pump, performing vacuum breaking treatment, and taking out the graphite disc to obtain the graphene sapphire wafer.
The invention also provides a graphene sapphire wafer, and the graphene sapphire wafer is prepared by the preparation method of the step-regulated graphene sapphire wafer.
The invention utilizes the electromagnetic induction coil to heat the graphite plate (for example, a special cold wall electromagnetic induction heating device, such as the prior application of the applicant, or the existing conventional method, as long as the heating of the graphite plate can be realized), alternating current generated by an induction heating power supply generates an alternating magnetic field through the electromagnetic induction coil, the graphite plate is arranged in the alternating magnetic field to cut alternating magnetic lines, so that alternating current (namely eddy current) is generated in the graphite plate, the eddy current enables atoms in an object to move randomly at a high speed, and the atoms collide and rub with each other to generate heat energy, thereby achieving the effect of heating the object.
The sapphire wafers used in the method for preparing the step-regulated graphene sapphire wafer include, but are not limited to, two inches, four inches and six inches. The design experiment result is suitable for all C-plane sapphire wafers.
The Raman result of the (four-inch) graphene sapphire crystal prepared by the preparation method of the step-regulated graphene sapphire wafer shows that I is D /I G Is less than 0.1, and I 2D /I G The value of (A) is close to 2, indicating that the grown graphene is good in quality and is a single layer. Under the condition of very high temperature, a step is generated on the surface of the sapphire, and according to a cross section TEM representation result, the sapphire surface is terminated by Al, so that certain promotion is realized on the growth of grapheneAnd (6) acting.
The average value of the sheet resistance of the (four-inch) graphene sapphire wafer prepared by the preparation method of the step-regulated graphene sapphire wafer is 565 omega/sq, the standard deviation of the whole sample is about 50 omega/sq, and the uniformity is good. Compared with other substrates, the result shows that the conductivity of the graphene film prepared by the method is equivalent to the quality of graphene obtained on a metal substrate, and the quality of the graphene film is far higher than that of graphene prepared on an insulating substrate at the present stage.
Drawings
FIG. 1 is an AMF graph of the surface topography of sapphire prepared in example 1 at various temperatures.
Fig. 2 is EBSD characterization of the sapphire surface before (a) and after (b) annealing prepared in example 1.
Fig. 3 shows AFM images of graphene/sapphire substrates obtained at different temperatures prepared in example 2.
Fig. 4 shows raman spectra of graphene obtained at different temperatures according to example 2.
Fig. 5 shows raman spectra of graphene obtained in example 3 under different pressures.
Fig. 6 shows raman spectra of graphene obtained in example 4 at different growth times.
FIG. 7 shows a single graphene domain I prepared in example 5 D /I G (a),I 2D /I G (b) Raman Mapping of (a).
Fig. 8 is a cross-sectional TEM image of the graphene/sapphire interface prepared in example 5.
Fig. 9 is a high-resolution TEM image of the graphene/sapphire interface structure prepared in example 5.
Fig. 10 is a graph representing the sheet resistance of the graphene/sapphire wafer prepared in example 5.
Detailed Description
Example 1
The embodiment provides a graphene sapphire wafer, and a preparation method thereof comprises the following steps:
(1) firstly, pretreating a sapphire wafer, respectively cleaning for three times under the conditions of alcohol/acetone and deionized water, and blow-drying by using a nitrogen gun for later use;
(2) opening the heating furnace, taking out the graphite disc, placing the cleaned sapphire substrate to be used in the graphite disc, loading the graphite disc into a tray, ascending to the center of the induction coil, and closing the cabin door to enable the system to be in a closed state;
(3) and opening a vacuum pump, pumping the pressure of the heating furnace system to 10Pa, setting an Otoland table after the vacuum index is stable, and determining the pressure required by the reaction. After the vacuum reading again stabilized.
(4) Opening a temperature control system, and setting the required temperature of the reaction at 1200 ℃, 1250 ℃, 1275 ℃, 1300 ℃, 1325 ℃, 1350 ℃, 1375 ℃ and 1400 ℃; the growth pressure is 3000Pa, and the growth time is 30 min;
(5) when the temperature rises to 500 ℃, 1000sccm argon and 500sccm hydrogen are introduced;
(6) stabilizing for 5min after the temperature is raised to the target temperature;
(7) after the temperature is stable, keeping the flow of hydrogen and argon unchanged, keeping the temperature unchanged, and carrying out annealing treatment on the sapphire substrate for 30 min;
(8) and after the annealing time is finished, stopping heating, and naturally cooling to room temperature under the protection of hydrogen and argon.
Fig. 1 is a result of Atomic Force Microscope (AFM) characterization of the sapphire substrate after the treatment of example 1, and the result shows that steps are generated on the sapphire surface after the treatment of the low-pressure reducing atmosphere, and the height of the steps becomes larger as the temperature rises. When the temperature is less than 1250 ℃, the surface appearance of the sapphire is not obviously changed, the roughness is less than 1nm, and the surface of the sapphire does not generate steps under the condition. As the temperature further increased from 1275 ℃ to 1300 ℃, the density of surface steps also began to grow larger, and the steps became larger and wider. When the temperature is further increased to 1350 ℃, steps with more uniform and regular surfaces appear, the height of the steps is about 2-5nm, and the width is about 200nm-1000 nm; the temperature then continues to rise to 1400 deg.C, with the step becoming significantly larger in height and wider in width.
Fig. 2 is a back scattered electron diffraction (EBSD) characterization result of the processed sapphire substrate for determining crystal form change of the sapphire surface before and after return. The results show that the sapphire surface is a (0001) plane before and after annealing, and no crystal form change is observed.
Example 2
The embodiment provides a graphene sapphire wafer, and a preparation method thereof comprises the following steps:
(1) firstly, pretreating a sapphire wafer, respectively cleaning for three times under the conditions of alcohol/acetone and deionized water, and blow-drying by using a nitrogen gun for later use;
(2) opening the heating furnace, taking out the graphite disc, placing the cleaned sapphire substrate to be used in the graphite disc, loading the graphite disc into a tray, ascending to the center of the induction coil, and closing the cabin door to enable the system to be in a closed state;
(3) and opening a vacuum pump, pumping the pressure of the heating furnace system to 10Pa, setting an Otoland table after the vacuum index is stable, and determining the pressure required by the reaction. After the vacuum reading again stabilized.
(4) Opening a temperature control system, and setting the required temperature of the reaction at 1200 ℃, 1250 ℃, 1275 ℃, 1300 ℃, 1325 ℃, 1350 ℃, 1375 ℃ and 1400 ℃; the growth pressure is 3000Pa, and the growth time is 30 min;
(5) when the temperature rises to 500 ℃, 1000sccm argon and 500sccm hydrogen are introduced;
(6) stabilizing for 5min after the temperature is raised to the target temperature;
(7) after the program is stable, introducing 200sccm methane, and keeping the temperature for 30 min;
(8) and after the constant temperature time is finished, stopping heating, closing methane, and naturally cooling to room temperature under the protection of hydrogen and argon.
Fig. 3 is an AFM profile representation of graphene grown at different temperatures in example 2, and the result shows that after graphene is grown, the surface profile of sapphire still maintains the same step as that during annealing, which indicates that methane introduced during graphene growth does not affect the substrate. Meanwhile, the formation of graphene wrinkles can be observed, mainly because the graphene and the sapphire have larger difference of thermal expansion coefficients, and the wrinkles cannot be generated in the cooling process.
FIG. 4 shows Raman characterization results of graphene at different temperatures, and the results show that when the temperature is 1350 ℃, I D /I G The ratio is the lowest, which indicates that the growth quality of the graphene is the highest at the moment.
Example 3
The embodiment provides a graphene sapphire wafer, and a preparation method thereof comprises the following steps:
setting the three steps as described in example 1, setting the reaction pressures to 2000Pa, 3000Pa and 5000Pa, opening the temperature control system after the indicated numbers are stable, setting the temperature required by the reaction to 1350 ℃, introducing 1000sccm argon and 500sccm hydrogen when the temperature is increased to 500 ℃, stabilizing for 5min, introducing 200sccm methane after the temperature is increased to the target temperature, and keeping the temperature constant for 30 min. And after the constant temperature time is finished, stopping heating, closing methane, and naturally cooling to room temperature under the protection of hydrogen and argon.
FIG. 5 shows Raman characterization results of graphene under different pressures, and the results show that I is measured at 3000Pa D /I G The ratio is the lowest, which indicates that the growth quality of the graphene is the highest at the moment.
Example 4
The embodiment provides a graphene sapphire wafer, and a preparation method thereof comprises the following steps:
the first three steps are carried out according to the steps described in the embodiment 1, the reaction pressure is set to be 3000Pa, the temperature control system is opened after the indicated number is stable, the temperature required by the reaction is set to be 1350 ℃, 1000sccm argon and 500sccm hydrogen are introduced when the temperature is increased to 500 ℃, 200sccm methane is introduced after the temperature is increased to the target temperature stably for 5min, and the constant temperature time is 20min, 30min and 60min respectively. And after the constant temperature time is finished, stopping heating, closing methane, and naturally cooling to room temperature under the protection of hydrogen and argon.
Fig. 6 is a raman characterization result of graphene under different growth times, and the result shows that when the growth time is 30min, the growth quality of graphene is the best.
Example 5
The embodiment provides a graphene sapphire wafer, and a preparation method thereof comprises the following steps:
and determining the optimal growth conditions of the graphene sapphire wafer. Setting the three steps as described in embodiment 1, setting the reaction pressure to be 3000Pa, opening the temperature control system after the indicated number is stable, setting the temperature required by the reaction to be 1350 ℃, introducing 1000sccm argon and 500sccm hydrogen when the temperature is increased to 500 ℃, stably introducing 200sccm methane for 5min after the temperature is increased to the target temperature, and keeping the temperature for 30 min. And after the constant temperature time is finished, stopping heating, closing methane, and naturally cooling to room temperature under the protection of hydrogen and argon.
FIG. 7 is a Raman mapping characterization of graphene sapphire (25 μm x 25 μm region size was selected) under optimal conditions to further evaluate overall quality and uniformity, FIG. 7a is I D /I G mapping characterization results show that the whole graphene film has high crystallization quality, I in fig. 7b 2D /I G mapping characterization results further show that the graphene film is a uniform single layer, the number of layers is controllable, and the uniformity is high.
Fig. 8 is TEM representation of a graphene/sapphire interface section under an optimal condition, and a graphene growth result at a substrate platform shown in fig. 8a shows that graphene and a sapphire substrate are perfectly attached. The growth of the graphene at the step is further characterized, as shown in fig. 8b, the step presents a gentle slope (13.3 °), and since the graphene itself has flexibility, the curvature radius of the graphene crossing the step is estimated according to the height and the slope of the step, and the curvature radius of the graphene at this time is 1.38nm, which indicates that the graphene can complete the cross-step growth.
Fig. 9 is a high-resolution TEM characterization result of a graphene sapphire interface under an optimal condition, in which a graphene carbon layer can be clearly observed, Al atoms and O atoms can be respectively observed to be distributed in a staggered manner below the carbon layer, at this time, sapphire is an Al terminated surface, and the Al atoms are bonded to C atoms. The result shows that when the sapphire surface is subjected to O desorption and changed into an Al-rich surface under the condition of very high temperature, the catalyst has a catalytic effect on the cracking of a carbon source and the growth of graphene, so that the growth quality of the graphene is further improved.
Fig. 10 is a four-probe sheet resistance result of a graphene sapphire wafer prepared from graphene under the optimal condition, the average value of the sheet resistance of the graphene sapphire wafer is 565 Ω/sq, and the standard deviation of the whole sample is about 50 Ω/sq, which proves that the graphene sapphire wafer has good uniformity.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A preparation method of a step-regulated graphene sapphire wafer comprises the following steps:
pretreating the sapphire wafer;
placing the pretreated sapphire substrate in a graphite disc, heating by electromagnetic induction, pumping the pressure to 10Pa, and setting the growth pressure, the growth temperature and the growth time;
when the temperature rises to 200-500 ℃, introducing argon, and when the temperature continues to rise to 600-800 ℃, introducing hydrogen;
when the temperature is raised to the growth temperature, introducing growth gas;
and after the growth is finished, stopping introducing growth gas, cooling in an argon and hydrogen environment, stopping introducing hydrogen when the temperature is lower than 500 ℃, stopping introducing argon when the temperature is lower than 100 ℃, and performing vacuum breaking treatment to obtain the graphene sapphire wafer.
2. The production method according to claim 1, wherein the growth pressure is 2000Pa to 5000 Pa;
preferably, the growth pressure is 3000 Pa.
3. The preparation method according to claim 1, wherein the growth temperature is 1275 ℃ to 1400 ℃;
preferably, the growth temperature is 1350 ℃.
4. The method of claim 1, wherein the growth time is 20min to 60 min;
preferably, the growth time is 30 min.
5. The production method according to claim 1, wherein the flow rate of argon gas is 500sccm to 1000 sccm.
6. The production method according to claim 1, wherein the flow rate of the hydrogen gas is 300sccm to 500 sccm.
7. The method of claim 1, wherein the growth gas is methane.
8. The production method according to claim 1 or 7, wherein a flow rate of the growth gas is 120sccm to 200 sccm.
9. The production method according to claim 1, wherein the pretreatment comprises the steps of:
and respectively cleaning the sapphire wafer in alcohol/acetone and water for three times, and drying the sapphire wafer by using a nitrogen gun for later use.
10. A graphene sapphire wafer prepared by the step-regulated graphene sapphire wafer preparation method of any one of claims 1-9.
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