CN114232083B - Preparation method of two-dimensional gallium nitride crystal - Google Patents
Preparation method of two-dimensional gallium nitride crystal Download PDFInfo
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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Abstract
The invention discloses a preparation method of a two-dimensional gallium nitride crystal, which comprises the following steps: s1, providing a metal sheet and cleaning; s2, heating and melting gallium metal, and transferring molten gallium metal onto the metal sheet; s3, placing the metal sheet and molten gallium in a reaction chamber, and vacuumizing the reaction chamber; and S4, after the reaction chamber is heated to a constant temperature, introducing a nitrogen source into the reaction chamber, so that nitrogen atoms are transmitted to the surface of the gallium metal, and growing the two-dimensional gallium nitride crystal. The preparation method of the two-dimensional gallium nitride crystal can increase the transverse mobility, so that an ultrathin sp3 hybridization mode and an sp2 hybridization hexagonal phase are easier to obtain, and the high-quality two-dimensional gallium nitride single crystal material with high crystallinity and high flatness is obtained, and is expected to pave the way for preparing deep ultraviolet photoelectric and power electronic devices.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a preparation method of a two-dimensional gallium nitride crystal.
Background
Gallium nitride (GaN) is one of the third generation nitride semiconductors, and is a direct bandgap semiconductor having a forbidden band width of 3.4eV and excellent properties such as high electron mobility, high breakdown voltage, high thermal conductivity, and the like. When the gallium nitride material is reduced to a two-dimensional scale, two-dimensional electron gas, lattice constant increase, band gap blue shift and the like can occur.
The two-dimensional gallium nitride has ideal deep ultraviolet light emission, exciton effect and electric transport characteristics under the influence of quantum confinement effect. However, gallium nitride is susceptible to sp3 hybridized longitudinal bonding and is difficult to obtain by conventional vapor phase growth or mechanical exfoliation methods.
Accordingly, in view of the above-mentioned technical problems, there is a need to provide a method for preparing a two-dimensional gallium nitride crystal.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a two-dimensional gallium nitride crystal.
In order to achieve the above object, an embodiment of the present invention provides the following technical solution:
a method of preparing a two-dimensional gallium nitride crystal, the method comprising:
s1, providing a metal sheet and cleaning;
s2, heating and melting gallium metal, and transferring molten gallium metal onto the metal sheet;
s3, placing the metal sheet and molten gallium in a reaction chamber, and vacuumizing the reaction chamber;
and S4, after the reaction chamber is heated to a constant temperature, introducing a nitrogen source into the reaction chamber, so that nitrogen atoms are transmitted to the surface of the gallium metal, and growing the two-dimensional gallium nitride crystal.
In one embodiment, the metal sheet is a tungsten sheet.
In an embodiment, the surface of the metal sheet is covered with a noble metal film, the noble metal film is a gold film or a platinum film, and the thickness of the noble metal film is greater than or equal to 100nm.
In one embodiment, the step S1 specifically includes:
washing the metal sheet with deionized water, and then placing the metal sheet into a cleaned glass container;
firstly, ultrasonically cleaning the metal sheet by using ethanol, then ultrasonically cleaning the metal sheet by using deionized water, and finally, drying the metal sheet by using nitrogen.
In an embodiment, the step S1 further includes:
firstly, ultrasonically cleaning a glass container by deionized water, and then ultrasonically cleaning the glass container by acetone;
repeating the steps to finish the cleaning of the glass container.
In one embodiment, in the step S2, the heating temperature for heating and melting the gallium metal is 30 ℃ to 2000 ℃.
In one embodiment, in the step S4, the nitrogen source is nitrogen plasma, and the constant temperature is 600 ℃ to 1100 ℃; or, the nitrogen source is ammonia gas, and the constant temperature is more than or equal to 800 ℃.
In one embodiment, in the step S4, the introducing a nitrogen source into the reaction chamber is specifically:
introducing a nitrogen source into the reaction chamber, wherein the flow is 0.1-5 sccm, and the introducing time is 1-20 s;
closing the nitrogen source, wherein the closing time is longer than the introducing time;
the above steps are repeated at least twice.
In one embodiment, when the nitrogen source is nitrogen plasma, the thickness of the two-dimensional gallium nitride crystal is 1 nm-15 nm, and when the nitrogen source is ammonia, the thickness of the two-dimensional gallium nitride crystal is 1 nm-30 nm.
In an embodiment, the step S4 further includes:
and stripping the two-dimensional gallium nitride crystal from the metal sheet through a mechanical stripping process.
The invention has the following beneficial effects:
the preparation method of the two-dimensional gallium nitride crystal can increase the transverse mobility, so that an ultrathin sp3 hybridization mode and an sp2 hybridization hexagonal phase are easier to obtain, and the high-quality two-dimensional gallium nitride single crystal material with high crystallinity and high flatness is obtained, and is expected to pave the way for preparing deep ultraviolet photoelectric and power electronic devices.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method for preparing a two-dimensional gallium nitride crystal according to the invention;
FIG. 2a is a schematic structural view of a reaction furnace according to the present invention;
FIG. 2b is a schematic view of the reaction chamber according to the present invention;
FIG. 2c is a schematic diagram of the structure of the metal sheet and the molten metal gallium thereon according to the present invention;
FIG. 3 is a scanning electron microscope image of the surface morphology of a two-dimensional GaN crystal in example 1 of the invention;
FIG. 4 is an atomic force microscope image of the surface morphology of a two-dimensional GaN crystal of example 1 of the invention;
FIG. 5 is an X-ray energy spectrum of a two-dimensional GaN crystal of example 1 of the invention;
FIG. 6 is a graph showing the fluorescence spectrum of the cathode of the two-dimensional GaN crystal of example 1 of the invention;
FIG. 7 is a scanning electron microscope image of the surface morphology of a two-dimensional GaN crystal in example 2 of the invention;
FIG. 8 is an atomic force microscope image of the surface morphology of a two-dimensional GaN crystal in example 2 of the invention;
FIG. 9 is an X-ray energy spectrum of a two-dimensional GaN crystal in example 2 of the invention;
FIG. 10 is a graph showing the fluorescence spectrum of the cathode of the two-dimensional GaN crystal of example 2 of the invention.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Referring to fig. 1, the invention discloses a preparation method of a two-dimensional gallium nitride crystal, which comprises the following steps:
s1, providing a metal sheet, and cleaning.
Wherein, the metal sheet is selected from metals with stronger catalytic ability, such as tungsten sheet, etc. Further, the surface of the metal sheet is covered with a noble metal film as a catalyst, such as a gold film or a platinum film, and the thickness of the noble metal film is 100nm or more.
The cleaning step of the metal sheet comprises the following steps:
washing the metal sheet with deionized water, and then placing the metal sheet into a cleaned glass container;
firstly, ultrasonically cleaning the metal sheet by using ethanol, then ultrasonically cleaning the metal sheet by using deionized water, and finally, drying the metal sheet by using nitrogen.
Preferably, before step S1, the method further includes:
firstly, ultrasonically cleaning a glass container (such as a beaker) by using deionized water, and then ultrasonically cleaning the glass container by using acetone;
repeating the steps to finish the cleaning of the glass container.
S2, heating and melting gallium metal, and transferring molten gallium metal onto the metal sheet.
Wherein the heating temperature for heating and melting the gallium metal is higher than the melting point (29.76 ℃) of the gallium metal, and the temperature is 30-2000 ℃.
And S3, placing the metal sheet and molten gallium in a reaction chamber, and vacuumizing the reaction chamber.
And S4, after the reaction chamber is heated to a constant temperature, introducing a nitrogen source into the reaction chamber, so that nitrogen atoms are transmitted to the surface of the gallium metal, and growing the two-dimensional gallium nitride crystal.
The constant temperature is 600-1100 ℃ when the nitrogen source is nitrogen plasma or ammonia gas, and is more than or equal to 800 ℃ when the nitrogen source is ammonia gas.
Preferably, the nitrogen source is introduced by adopting an intermittent ventilation mode, specifically:
introducing a nitrogen source into the reaction chamber, wherein the flow is 0.1-5 sccm, and the introducing time is 1-20 s;
closing the nitrogen source for 5-30 s;
the above steps are repeated at least twice.
In the invention, when the nitrogen source is nitrogen plasma, the thickness of the two-dimensional gallium nitride crystal is 1 nm-15 nm, and when the nitrogen source is ammonia, the thickness of the two-dimensional gallium nitride crystal is 1 nm-30 nm.
Further, step S4 further includes:
and stripping the two-dimensional gallium nitride crystal from the metal sheet through a mechanical stripping process.
The invention is further illustrated below with reference to specific examples.
Example 1:
in the embodiment, gallium metal is used as a gallium source, alloy is formed with a metal tungsten sheet with strong catalytic capability, the alloy is placed in a reaction chamber, nitrogen plasma is introduced into the reaction chamber, so that nitrogen atoms can be transmitted to the surface of the gallium metal, and the growth of a two-dimensional gallium nitride crystal is realized.
Specifically, the preparation method of the two-dimensional gallium nitride crystal in the embodiment includes the following steps:
1. the glass container is cleaned.
In the embodiment, the glass container is a beaker, the beaker is firstly ultrasonically cleaned by deionized water, then the beaker is ultrasonically cleaned by acetone, and the cleaning is repeated for a plurality of times.
2. A metal sheet is provided and cleaned.
In this embodiment, the metal sheet is a tungsten sheet, and a gold film with a thickness of 100nm is covered on the surface of the tungsten sheet as a catalyst, and in other embodiments, a platinum film may be used as a catalyst.
The cleaning steps of the tungsten sheet are as follows:
after the tungsten sheet is washed by deionized water, putting the tungsten sheet into a well-washed beaker;
firstly, ultrasonically cleaning the tungsten sheet by using ethanol, then ultrasonically cleaning by using deionized water, and finally, drying the tungsten sheet by using nitrogen.
3. The gallium metal is heated and melted, and the molten gallium metal is transferred to the tungsten plate.
The heating temperature is greater than the melting point of gallium metal (29.76 ℃), in this example 700 ℃.
4. Fixing the sample (tungsten sheet and molten metal gallium) on a tray, then integrally placing the tray in a reaction chamber, and vacuumizing the reaction chamber to a vacuum degree of 10 -5 Torr。
Referring to fig. 2a, fig. 2b, fig. 2c, and fig. 2c, respectively, are schematic diagrams of a reaction chamber in the present embodiment and a metal sheet and molten gallium thereon in the present embodiment.
5. And after the reaction chamber is heated to a constant temperature, introducing a nitrogen source into the reaction chamber, so that nitrogen atoms are transmitted to the surface of the gallium metal, and the growth of the two-dimensional gallium nitride crystal is carried out.
In this embodiment, the nitrogen source is nitrogen plasma, and the constant temperature of the reaction chamber after heating is 700 ℃.
After the reaction chamber reaches a constant temperature, nitrogen sources are introduced by adopting an intermittent ventilation mode, so that enough relaxation time is ensured in the growth process of the two-dimensional gallium nitride crystal.
In the embodiment, firstly, a nitrogen source is introduced into a reaction chamber, the flow is 0.5sccm, and the introduction time is 10s; closing the nitrogen source for 5min; repeating the above steps for 6 times until the two-dimensional gallium nitride crystal is grown, wherein the thickness of the two-dimensional gallium nitride crystal is about 8 nm.
Finally, the tray is moved out of the reaction chamber.
Further, the two-dimensional gallium nitride crystal can be peeled from the tungsten sheet by a mechanical peeling process.
Example 2:
in the embodiment, gallium metal is used as a gallium source, alloy is formed with a metal tungsten sheet with strong catalytic capability, the alloy is placed in a reaction chamber, ammonia gas is introduced into the reaction chamber, nitrogen atoms are obtained through heating and decomposition, and the nitrogen atoms can be transmitted to the surface of the gallium metal, so that the growth of the two-dimensional gallium nitride crystal is realized.
Specifically, the preparation method of the two-dimensional gallium nitride crystal in the embodiment includes the following steps:
1. the glass container is cleaned.
In the embodiment, the glass container is a beaker, the beaker is firstly ultrasonically cleaned by deionized water, then the beaker is ultrasonically cleaned by acetone, and the cleaning is repeated for a plurality of times.
2. A metal sheet is provided and cleaned.
In this embodiment, the metal sheet is a tungsten sheet, and a gold film with a thickness of 100nm is covered on the surface of the tungsten sheet as a catalyst, and in other embodiments, a platinum film may be used as a catalyst.
The cleaning steps of the tungsten sheet are as follows:
after the tungsten sheet is washed by deionized water, putting the tungsten sheet into a well-washed beaker;
firstly, ultrasonically cleaning the tungsten sheet by using ethanol, then ultrasonically cleaning by using deionized water, and finally, drying the tungsten sheet by using nitrogen.
3. The gallium metal is heated and melted, and the molten gallium metal is transferred to the tungsten plate.
The heating temperature is greater than the melting point of gallium metal (29.76 ℃), in this example 900 ℃.
4. Fixing the sample (tungsten sheet and molten metal gallium) on a tray, then integrally placing the tray in a reaction chamber, and vacuumizing the reaction chamber to a vacuum degree of 10 -5 Torr。
Referring to fig. 2a, fig. 2b, fig. 2c, and fig. 2c, respectively, are schematic diagrams of a reaction chamber in the present embodiment and a metal sheet and molten gallium thereon in the present embodiment.
5. And after the reaction chamber is heated to a constant temperature, introducing a nitrogen source into the reaction chamber, so that nitrogen atoms are transmitted to the surface of the gallium metal, and the growth of the two-dimensional gallium nitride crystal is carried out.
In this example, the nitrogen source is ammonia gas, and the constant temperature of the reaction chamber after heating is 900 ℃.
After the reaction chamber reaches a constant temperature, nitrogen sources are introduced by adopting an intermittent ventilation mode, so that enough relaxation time is ensured in the growth process of the two-dimensional gallium nitride crystal.
In the embodiment, firstly, a nitrogen source is introduced into a reaction chamber, the flow is 0.5sccm, and the introduction time is 10s; closing the nitrogen source for 5min; repeating the above steps for 6 times until the two-dimensional gallium nitride crystal is grown, wherein the thickness of the two-dimensional gallium nitride crystal is about 8 nm.
Finally, the tray is moved out of the reaction chamber.
Further, the two-dimensional gallium nitride crystal can be peeled from the tungsten sheet by a mechanical peeling process.
The crystals prepared in example 1 and example 2 were sealed in a vacuum bag and the quality of the crystals was characterized as follows:
a. FIGS. 3 and 7 are scanning electron microscope images of the surface morphology of the two-dimensional gallium nitride crystal in example 1 and example 2, respectively;
b. FIGS. 4 and 8 are atomic force microscope views of the surface morphologies of the two-dimensional gallium nitride crystals of examples 1 and 2, respectively;
c. FIGS. 5 and 9 are X-ray energy spectra of two-dimensional gallium nitride crystals of example 1 and example 2, respectively;
d. FIGS. 6 and 10 are respectively the cathode fluorescence spectra of two-dimensional gallium nitride crystals in example 1 and example 2.
The grown material can be judged to be a two-dimensional gallium nitride crystal through a scanning electron microscope image, an X-ray energy spectrogram and a cathode fluorescence spectrogram.
The thickness of the grown two-dimensional gallium nitride crystal was measured by atomic force microscopy, and the maximum thickness of the two-dimensional gallium nitride crystal grown using nitrogen plasma as a nitrogen source in example 1 was about 15nm, and the maximum thickness of the two-dimensional gallium nitride crystal grown using ammonia gas as a nitrogen source in example 2 was about 30nm.
As can be seen from the technical scheme, the invention has the following advantages:
the preparation method of the two-dimensional gallium nitride crystal can increase the transverse mobility, so that an ultrathin sp3 hybridization mode and an sp2 hybridization hexagonal phase are easier to obtain, and the high-quality two-dimensional gallium nitride single crystal material with high crystallinity and high flatness is obtained, and is expected to pave the way for preparing deep ultraviolet photoelectric and power electronic devices.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (6)
1. A method for preparing a two-dimensional gallium nitride crystal, comprising:
s1, providing a metal sheet and cleaning; the surface of the metal sheet is covered with a noble metal film, the noble metal film is a gold film or a platinum film, and the thickness of the noble metal film is more than or equal to 100nm;
s2, heating and melting gallium metal, and transferring molten gallium metal onto the metal sheet;
s3, placing the metal sheet and molten gallium in a reaction chamber, and vacuumizing the reaction chamber;
s4, after the reaction chamber is heated to a constant temperature, introducing a nitrogen source into the reaction chamber, so that nitrogen atoms are transmitted to the surface of the gallium metal, and growing a two-dimensional gallium nitride crystal; the nitrogen source is nitrogen plasma, and the constant temperature is 600-1100 ℃; or, the nitrogen source is ammonia gas, and the constant temperature is more than or equal to 800 ℃;
in the step S4, the step of introducing a nitrogen source into the reaction chamber specifically includes:
introducing a nitrogen source into the reaction chamber, wherein the flow is 0.1-5 sccm, and the introducing time is 1-20 s;
closing the nitrogen source, wherein the closing time is longer than the introducing time;
repeating the above steps at least twice;
the step S4 further includes:
and stripping the two-dimensional gallium nitride crystal from the metal sheet through a mechanical stripping process.
2. The method of claim 1, wherein the metal sheet is a tungsten sheet.
3. The preparation method according to claim 1, wherein the step S1 specifically comprises:
washing the metal sheet with deionized water, and then placing the metal sheet into a cleaned glass container;
firstly, ultrasonically cleaning the metal sheet by using ethanol, then ultrasonically cleaning the metal sheet by using deionized water, and finally, drying the metal sheet by using nitrogen.
4. The method according to claim 3, wherein the step S1 is preceded by:
firstly, ultrasonically cleaning a glass container by deionized water, and then ultrasonically cleaning the glass container by acetone;
repeating the steps to finish the cleaning of the glass container.
5. The method according to claim 1, wherein in the step S2, the heating temperature for heating the molten gallium metal is 30 ℃ to 2000 ℃.
6. The method according to claim 1, wherein the thickness of the two-dimensional gallium nitride crystal is 1nm to 15nm when the nitrogen source is nitrogen plasma, and 1nm to 30nm when the nitrogen source is ammonia gas.
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