CN113013020B - Growth method of large-area ultrathin two-dimensional nitride based on thickness etching - Google Patents
Growth method of large-area ultrathin two-dimensional nitride based on thickness etching Download PDFInfo
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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Abstract
The invention discloses a preparation method of an ultrathin two-dimensional nitride film, which comprises the following steps: the surface of the substrate is pretreated by an oxygen plasma cleaning machine, more active sites are provided for the adsorption of oxygen atoms, the bonding capability between the oxide film on the surface of the liquid metal and the substrate is obviously improved after the liquid metal is extruded, and the oxide film on the inner layer is poor in quality due to insufficient contact between the oxide film and the substrate and insufficient oxidation degree, so that the oxide film is etched in the subsequent nitrogen plasma chemical vapor deposition process, an ultrathin two-dimensional film is obtained, and the oxide film is nitrided at the same time, so that the ultrathin two-dimensional nitride film is obtained.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a method for growing large-area ultrathin two-dimensional nitride based on thickness etching.
Background
Nitride materials have been widely used in the field of optoelectronics as a new generation of semiconductor materials. With the rise of two-dimensional material research, there is also a great interest in two-dimensional nitride materials, and when the nitride reaches a single atomic layer thickness, the structure of the nitride becomes an in-plane two-dimensional structure similar to graphene. Compared with a parent material, the two-dimensional nitride material has the unique properties of ultra-wide band gap in a deep ultraviolet region, low thermal conductivity, strong mechanical strain capacity and the like, and the application of the nitride in the fields of deep ultraviolet, thermoelectric and flexible devices is widened. However, due to the wurtzite structure of the parent material, bonds are formed between the nitride layers, and the method of obtaining a few-layer two-dimensional material by mechanical stripping from top to bottom is difficult to realize. On the other hand, due to the lack of the influence of factors such as a proper epitaxial substrate, a great number of defects and dislocation exist in the thin film material obtained by the bottom-up epitaxial method, and the obtained two-dimensional nitride material often forms bonds with the substrate and cannot be independent, so that the further application of the two-dimensional nitride material is limited. Therefore, large-area blank exists in the preparation of the large-area ultrathin two-dimensional nitride material, and the preparation needs to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of a large-area ultrathin two-dimensional nitride material. The preparation method is simple and rapid, and nitride materials with single atomic layer thickness can be obtained.
The preparation method of the large-area ultrathin two-dimensional nitride material provided by the invention comprises the following steps:
1) Pretreating the substrate in the oxygen plasma environment to provide more active sites for oxygen atom adsorption;
2) Placing the two pretreated substrates in the step 1) on a heating table, placing metal on the surface of one substrate, covering and extruding liquid metal by the other substrate after the metal is melted, keeping the two substrates in a superposition state, standing, separating the two substrates, removing metal residues on the surface, and obtaining a metal oxide film on the surface of the substrate;
3) And 2) placing the substrate with the metal oxide film on the surface obtained in the step 2) into a plasma enhanced chemical vapor deposition system, introducing nitrogen plasma, and etching an area with an unstable surface of the oxide film while nitriding to obtain the ultrathin two-dimensional nitride film.
The method specifically comprises the following operations:
extruding metal liquid drops by using two substrates subjected to oxygen plasma pretreatment, leaving a metal oxide film on the surface of the substrate, putting the obtained oxide film into a nitrogen Plasma Enhanced Chemical Vapor Deposition (PECVD) system for nitriding to obtain nitride, and generating certain stripping and etching effects by plasma at the same time, so as to finally obtain the ultrathin large-area two-dimensional nitride film.
In the step 1) of the method, the substrate may be a silicon wafer, a silicon wafer with a silicon oxide layer, a quartz wafer, a silicon nitride wafer, a sapphire wafer, or the like. The thickness of the substrate may be 0.05 μm-2mm.
The thickness of the silicon oxide layer on the surface of the silicon oxide wafer in the silicon wafer with the silicon oxide layer can be 10nm-2000nm.
According to one embodiment of the invention, the thickness of the silicon wafer with the silicon oxide layer is 0.5mm, and the thickness of the silicon oxide layer is 90nm; the specification of the substrate may be specifically 1cm by 1cm.
The substrate is also required to be ultrasonically cleaned before being used, and the cleaning method is as follows, taking a silicon wafer with a silicon oxide layer as an example: and ultrasonically cleaning the silicon wafer with the silicon oxide layer by using acetone, isopropanol and deionized water for 5-10 minutes (specifically, 5 minutes).
In the above method step 1), the pretreatment is performed in an oxygen plasma cleaning machine. The conditions are as follows: controlling the pressure of the introduced oxygen to be 100-240Pa and cleaning for 2-20 minutes, specifically comprising the following steps: the pressure of the introduced oxygen was controlled to be 110Pa and the mixture was purged for 3 minutes.
In the above method step 2), the metal may be a low melting point metal (e.g. indium, tin, gallium) or an alloy (e.g. gallium indium alloy, indium tin alloy, aluminum gallium alloy) having a melting point below 500 ℃. The low melting point metal or alloy may be solid or liquid.
The metal is solid low-melting point metal or alloy, and after the low-melting point metal or alloy is melted, another substrate is used for covering and extruding the liquid metal or alloy. The metal is solid low-melting point metal or alloy, and the temperature of the heating table is 50-500 ℃ (particularly 50 ℃, 75 ℃ and 100 ℃) according to the melting point of the metal or alloy.
The metal is a liquid low melting point metal or alloy, and can be directly covered with another piece of substrate and extruded. The metal is liquid low-melting point metal or alloy, and the temperature of the heating table is 50-200deg.C (such as 50deg.C, 75deg.C, 100deg.C).
In the above method step 2), the time of the standing may be 0.1 to 60 minutes (specifically, 2 minutes).
In the above method step 2), the two substrates cannot slide laterally during the separation process.
In the above method step 3), the specific method is as follows: placing the oxide film surface of the substrate with the metal oxide film on a quartz tile boat with the surface being equal to the size of the substrate in a face-down mode, pushing the quartz tile to the center of a reaction area of a plasma enhanced tube furnace, pumping the quartz tile to the air pressure of less than 1Pa in the quartz tube by a mechanical pump, introducing 5-30sccm argon gas at the moment, heating the reaction area to 400-800 ℃ at the heating rate of 5-30 ℃/min when the air pressure in the quartz tube is 10-35Pa, stopping introducing the argon gas after reaching the target temperature, introducing 1-30sccm nitrogen gas at the same time, turning on a power supply of a plasma module, setting the plasma power to 10-80W (particularly 10W) and starting the plasma power, closing a plasma switch after reacting for 5-90 minutes (particularly 20 minutes), rapidly cooling the temperature of the furnace body to room temperature within twenty minutes, and keeping the atmosphere in the reaction chamber unchanged by the nitrogen gas during the twenty minutes.
Compared with the prior art, the invention has the following advantages:
after the substrate is pre-treated by utilizing oxygen plasma, the bonding force between the oxide formed on the surface of the liquid metal and the substrate can be obviously increased, the upper unstable oxide is etched by utilizing a nitrogen plasma enhanced chemical vapor deposition system, and meanwhile, the oxide is nitrided, and finally, the large-area ultrathin two-dimensional nitride film is obtained. The obtained nitride film can be as low as 0.8nm, and is single-layer or double-layer. The prepared nitride film can be deposited on different substrates, and can be transferred to any other target substrate, and the characteristic of independence from the substrate enables the two-dimensional nitride film to have wider application prospect.
Drawings
FIG. 1 is a growth flow chart of the present invention; firstly, processing a substrate by an oxygen plasma cleaner, then extruding metal liquid drops by two substrates, obtaining a uniform oxide film after simple cleaning, putting the obtained oxide film into a nitrogen plasma enhanced chemical vapor deposition system for nitriding, and finally obtaining a large-area ultrathin nitride film.
FIG. 2 is an optical micrograph of a gallium oxide film of example 1 of the present invention before and after nitridation; the metal oxide film before nitriding is shown as a, and the nitride film after nitriding is shown as b.
Fig. 3 is Atomic Force Microscope (AFM) data of a gallium oxide thin film prepared in example 1 of the present invention.
Fig. 4 is Atomic Force Microscope (AFM) data of a two-dimensional gallium nitride film prepared in example 1 of the present invention.
FIG. 5 is X-ray photoelectron spectroscopy (XPS) data of a two-dimensional gallium nitride film prepared in example 1 of the present invention; wherein a is the fine-swept spectrum of the N1s orbit, and b is the fine-swept spectrum of the Ga2p orbit.
FIG. 6 is X-ray photoelectron spectroscopy (XPS) data of a two-dimensional indium nitride film prepared in example 2 of the present invention.
FIG. 7 shows Atomic Force Microscope (AFM) data for gallium nitride films obtained by 10 minutes of reaction at 100W power.
Fig. 8 is an optical microscope photograph of a gallium oxide thin film deposited on the surface of a silicon oxide wafer without plasma pretreatment.
Detailed Description
The invention will be further illustrated with reference to the following specific examples, but the invention is not limited to the following examples. The methods are conventional methods unless otherwise specified. The starting materials are available from published commercial sources unless otherwise specified.
Example 1 preparation of ultra-thin gallium nitride Using silicon wafer with silicon oxide layer and liquid gallium Metal
According to the flow chart in fig. 1, the method for preparing ultrathin gallium nitride specifically comprises the following steps:
(1) Cutting a silicon wafer with a silicon oxide layer (the thickness is 0.5mm, wherein the thickness of the silicon oxide layer is 90 nm) into 1cm by using a diamond knife, cleaning the silicon wafer for 10 minutes by using acetone, isopropanol and deionized water in sequence, putting the cleaned silicon oxide wafer into an oxygen plasma cleaner, controlling the air pressure of the introduced oxygen to be 110Pa, and cleaning the silicon oxide wafer for 3 minutes.
(2) The silicon oxide layers of the two treated silicon oxide wafers were placed on a heating table with a temperature of 50 c, one drop (about 5 mg) of metallic gallium stored in isopropyl alcohol was taken out with a rubber head dropper, placed on one of the silicon oxide wafers, and the other silicon oxide wafer was picked up with tweezers and the metallic drop was squeezed to spread on the silicon oxide wafer.
(3) Placing the two extruded silicon oxide wafers on a heating table, standing for two minutes, separating the two silicon oxide wafers by using tweezers, wherein transverse sliding cannot exist between the two silicon oxide wafers in the process, placing the separated silicon oxide wafers into isopropanol, and using a cotton swab to simply clean the silicon oxide wafers, so as to clean metal residues on the surfaces of the silicon oxide wafers, and obtaining a clean and uniform oxide film.
(4) Placing the prepared oxide film on a heating table, placing the front surface of the silicon oxide wafer with the metal oxide film on a quartz tile downwards after the organic solvent on the surface of the silicon oxide wafer volatilizes, sending the silicon oxide wafer into a reaction zone of a plasma enhanced chemical vapor deposition system, pumping the silicon oxide wafer to the air pressure of less than 1Pa by using a mechanical pump, introducing 20sccm of argon, and heating the silicon oxide wafer to 800 ℃ at the speed of 30 ℃/min.
(5) After the temperature rises to 800 ℃, stopping introducing argon, introducing 5-30sccm of nitrogen, turning on a switch of the plasma module, setting the power to 10W, and starting.
(6) After 20 minutes of reaction, the plasma was turned off and the furnace temperature was rapidly lowered to room temperature, during which time the atmosphere in the reaction chamber remained unchanged.
(7) Taking out the nitrided sample, observing the morphology of the sample by using an optical microscope and a Scanning Electron Microscope (SEM), determining the uniformity and the size of the thin film, determining the material element composition by using X-ray photoelectron spectroscopy (XPS), and determining the thickness and the surface uniformity of the sample by using an Atomic Force Microscope (AFM).
As shown in FIG. 2, the optical microscope photographs before and after nitriding of the gallium oxide film prepared in the example show that the contrast on the silicon oxide wafer of the film sample after nitriding by the plasma is obviously reduced, which shows the ultra-thin property of the film, the color of the film is uniform, and the thickness of the film prepared by the reaction is uniform.
The Atomic Force Microscope (AFM) data of the gallium oxide film prepared in this example are shown in FIG. 3, and it can be seen from FIG. 3 that the thickness of the gallium oxide film is 3nm.
As shown in fig. 4, the Atomic Force Microscope (AFM) data of the two-dimensional gallium nitride thin film prepared in this example shows that the thickness of two-dimensional gallium nitride is as low as 0.8nm, which is a monolayer. In contrast to fig. 3, the thickness of gallium nitride after nitridation is significantly thinner than the thickness of gallium oxide film before nitridation due to the etching action of nitrogen plasma.
The X-ray photoelectron spectroscopy (XPS) data of the two-dimensional gallium nitride film prepared in this example are shown in fig. 5, and as can be seen from fig. 5, the fine scanning spectrum of the N1s and Ga2p orbitals indicates that Ga atoms and N atoms are bonded to form bonds, and a gallium nitride material is obtained.
Example 2 preparation of ultra-thin InGaN Using silicon oxide wafer and GaInalloy
(1) Cutting a silicon wafer with a silicon oxide layer (the thickness is 0.5mm, wherein the thickness of the silicon oxide layer is 90 nm) into 1cm by using a diamond knife, cleaning the silicon wafer for 10 minutes by using acetone, isopropanol and deionized water in sequence, putting the cleaned silicon oxide wafer into an oxygen plasma cleaner, controlling the air pressure of the introduced oxygen to be 110Pa, and cleaning the silicon oxide wafer for 3 minutes.
(2) In a glove box, metal indium and metal gallium are mixed according to a mass ratio of 1:1 is placed in a beaker for heating and stirring, the temperature of a heating table is set to 75 ℃, and the mixture is placed in isopropanol solution for standby after being fully and uniformly stirred.
(3) The two silicon oxide wafers after treatment are placed on a heating table with the temperature of 100 ℃ upwards, prepared gallium indium alloy (about 10 mg) is placed on one silicon oxide wafer, after the gallium indium alloy is melted, the other silicon oxide wafer is picked up by tweezers and molten metal is extruded, so that the metal is spread on the silicon oxide wafer.
(4) And placing the two extruded silicon oxide wafers on a heating table, standing for two minutes, separating the two silicon oxide wafers by using tweezers, wherein transverse sliding cannot exist between the two silicon oxide wafers in the process, and wiping off metal residues on the surfaces by using PDMS (polydimethylsiloxane) to obtain a clean and uniform oxide film.
(5) Placing the prepared oxide film on a heating table, placing the front surface of the silicon oxide wafer with the sample on a quartz tile downwards after the organic solvent on the surface of the silicon oxide wafer volatilizes, sending the silicon oxide wafer into a reaction zone of a plasma enhanced chemical vapor deposition system, pumping the silicon oxide wafer to the air pressure of less than 1Pa by using a mechanical pump, introducing 20sccm argon, and heating the silicon oxide wafer to 500 ℃ at the speed of 20 ℃/min.
(6) After the temperature rises to 500 ℃, stopping introducing argon, introducing 5-30sccm of nitrogen, turning on a switch of the plasma module, setting the power to 10W, and starting.
(7) After 20 minutes of reaction, the plasma was turned off and the furnace temperature was rapidly lowered to room temperature, during which time the atmosphere in the reaction chamber remained unchanged.
(8) Taking out the nitrided sample, observing the morphology of the sample by using an optical microscope and a Scanning Electron Microscope (SEM), determining the uniformity of the thin film, determining the material element composition by using X-ray photoelectron spectroscopy (XPS), and determining the thickness and the surface uniformity of the sample by using an Atomic Force Microscope (AFM).
The X-ray photoelectron spectroscopy (XPS) data of the two-dimensional indium gallium nitride film prepared In this example are shown In fig. 6, and as can be seen from fig. 6, global scan 6a shows that the obtained alloy film contains Ga element and In element, and fine scan spectra of N1s track 6b and In3d track 6c show that the two-dimensional indium gallium nitride alloy film is successfully prepared.
EXAMPLE 3 Effect of Nitrogen plasma on film thickness uniformity
In example 1, the reactive plasma power was increased, and it was found that too high a power would damage the surface morphology of the thin film, as shown in fig. 7, the nitrogen plasma power was increased to 100w at the time of the reaction, and the surface roughness of the thin film measured by afm was significantly increased, so that it was necessary to maintain the plasma power at a moderate level for uniform synthesis of two-dimensional ultra-thin nitride.
EXAMPLE 4 Effect of oxygen plasma on pretreatment of substrates
In example 1, the removal of the oxygen plasma pretreatment step performed on the substrate significantly reduced the adhesion of the metal oxide to the substrate, and the simple stripping of the residual metal with a cotton swab resulted in significant damage to the metal oxide film, as shown in fig. 8. The metal oxide film after being pretreated by oxygen plasma is tightly combined with the substrate, the film is not damaged in the process of stripping residual metal, and the finally prepared nitride film is more uniform.
Claims (9)
1. The preparation method of the large-area ultrathin two-dimensional nitride material comprises the following steps:
1) Pretreating the substrate in the oxygen plasma environment to provide more active sites for oxygen atom adsorption;
2) Placing the two pretreated substrates in the step 1) on a heating table, placing metal on the surface of one substrate, covering and extruding liquid metal by the other substrate after the metal is melted, keeping the two substrates in a superposition state, standing, separating the two substrates, removing metal residues on the surface, and obtaining a metal oxide film on the surface of the substrate;
3) And (3) placing the substrate with the oxide film on the surface into a plasma enhanced chemical vapor deposition system, introducing nitrogen plasma, and etching the unstable surface area of the oxide film while nitriding to finally obtain the ultrathin two-dimensional nitride film.
2. The method according to claim 1, characterized in that: in the step 1), the substrate is a silicon wafer, a silicon wafer with a silicon oxide layer, a quartz wafer, sapphire or silicon nitride.
3. The method according to claim 1, characterized in that: in the step 1), the pretreatment is carried out in an oxygen plasma cleaning machine, the pressure of the introduced oxygen is controlled to be 100-240Pa, and the oxygen is cleaned for 2-30 minutes.
4. The method according to claim 1, characterized in that: in the step 2), the metal is a low-melting-point metal or alloy with a melting point lower than 500 ℃; the low-melting point metal or alloy is solid or liquid.
5. The method according to claim 4, wherein:
the metal is solid low-melting-point metal or alloy, and after the low-melting-point metal or alloy is melted, another substrate is used for covering and extruding the liquid metal or alloy; the metal is solid low-melting-point metal or alloy, and the temperature of the heating table is 50-500 ℃.
6. The method according to claim 4, wherein: the metal is liquid low-melting-point metal or alloy, and can be directly covered by another substrate and extruded; the metal is liquid low-melting-point metal or alloy, and the temperature of the heating table is 50-200 ℃.
7. The method according to claim 1, characterized in that: in the step 2), the standing time is 2-120 minutes.
8. The method according to claim 1, characterized in that: in the step 3), the specific method is as follows: placing the oxide film surface of the substrate with the oxide film on a quartz tile face down, sending the substrate into a reaction area of a plasma enhanced chemical vapor deposition system, pumping the substrate to the air pressure of less than 1Pa by using a mechanical pump, introducing argon gas of 5-30sccm, heating the substrate to 400-800 ℃ at the speed of 5-30 ℃/min, stopping introducing the argon gas, introducing nitrogen of 5-30sccm, opening a switch of a plasma module, setting the power to 10-80W, starting the plasma module, closing plasma after reacting for 5-90 min, rapidly cooling the temperature of a furnace body to room temperature, and keeping the atmosphere in the reaction chamber unchanged during the period.
9. The large-area ultrathin two-dimensional nitride material prepared by the method of any one of claims 1-8.
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