CN113013020A - Large-area ultrathin two-dimensional nitride growth method based on thickness etching - Google Patents
Large-area ultrathin two-dimensional nitride growth method based on thickness etching Download PDFInfo
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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 cleaner, more active sites are provided for the adsorption of oxygen atoms, the bonding capacity between an 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 of the inner layer is not fully contacted with the substrate, so that the quality is poor due to insufficient oxidation degree, the oxide film of the layer can be etched in the subsequent nitrogen plasma chemical vapor deposition process, the ultrathin two-dimensional film is obtained, and meanwhile, the oxide film is nitrided, and 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 research on two-dimensional materials, people have generated a great interest in two-dimensional nitride materials, and when the nitride reaches the thickness of a single atomic layer, the structure of the nitride can be changed into a graphene-like in-plane two-dimensional structure. Compared with a parent material, the two-dimensional nitride material has the unique properties of ultra-wide band gap, low thermal conductivity, strong mechanical strain capacity and the like in a deep ultraviolet region, and widens the application of the nitride in the fields of deep ultraviolet, thermoelectricity and flexible devices. However, due to the wurtzite structure of the parent material, the nitride layer and the layer form a bond, and the method for obtaining the two-dimensional material with few layers by mechanical stripping from top to bottom is difficult to realize. On the other hand, due to the influence of factors such as lack of a proper epitaxial substrate, a film material obtained by a bottom-up epitaxial method has a large number of defects and dislocations, and the obtained two-dimensional nitride material is often bonded with the substrate and cannot be separated out, so that the further application of the two-dimensional nitride material is limited. Therefore, the preparation of large-area ultrathin two-dimensional nitride materials has a large-area blank and needs to be solved urgently.
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 quick, and the nitride material with the thickness of a single atomic layer can be obtained.
The preparation method of the large-area ultrathin two-dimensional nitride material provided by the invention comprises the following steps of:
1) the method comprises the following steps of pretreating a substrate in an oxygen plasma environment to provide more active sites for adsorption of oxygen atoms;
2) placing the two pretreated substrates in the step 1) on a heating table, placing metal on the surface of one substrate, covering the other substrate after the metal is molten and extruding liquid metal to enable the two substrates to be kept in a superposed state and stand, then separating the two substrates, removing metal residues on the surfaces, and obtaining a metal oxide film on the surface of the substrate;
3) and (3) putting 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, etching the unstable area of the surface of the oxide film while nitriding, and finally obtaining the ultrathin two-dimensional nitride film.
The method specifically comprises the following operations:
two pieces of substrate pretreated by oxygen plasma are used for extruding metal liquid drops, a metal oxide film is left on the surface of the substrate, the obtained oxide film is placed into a nitrogen plasma enhanced chemical vapor deposition system (PECVD) for nitridation, the plasma generates a certain stripping and etching effect while the nitride is obtained, and finally the ultrathin large-area two-dimensional nitride film is obtained.
In step 1), the substrate may be a silicon wafer, a silicon wafer with a silicon oxide layer, a quartz wafer, silicon nitride, a sapphire wafer, or the like. The substrate may have a thickness of 0.05 μm-2 mm.
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-2000 nm.
According to one embodiment of the invention, the silicon wafer with the silicon oxide layer is 0.5mm thick, and the thickness of the silicon oxide layer is 90 nm; the substrate may specifically have a dimension of 1cm by 1 cm.
The substrate is required to be subjected to ultrasonic cleaning before use, and taking a silicon wafer with a silicon oxide layer as an example, the cleaning method comprises the following steps: and ultrasonically cleaning the silicon wafer with the silicon oxide layer for 5-10 minutes (specifically 5 minutes) by using acetone, isopropanol and deionized water in sequence.
In step 1) of the above method, 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 as follows: the pressure of the introduced oxygen was controlled to 110Pa and the purging was carried out for 3 minutes.
In 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) with a melting point lower than 500 ℃. The low melting point metal or alloy may be in a solid or liquid state.
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 metal or alloy, and the temperature of the heating stage is 50-500 deg.C (such as 50 deg.C, 75 deg.C, and 100 deg.C) according to the melting point of the metal or alloy.
The metal is a liquid low-melting-point metal or alloy, and the liquid metal can be directly covered and extruded by another substrate. The metal is liquid low-melting point metal or alloy, and the temperature of the heating stage is 50-200 deg.C (such as 50 deg.C, 75 deg.C, and 100 deg.C).
In the step 2) of the above method, the standing time may be 0.1 to 60 minutes (specifically, 2 minutes).
In the step 2) of the method, the two substrates cannot slide transversely in the process of separating the two substrates.
In step 3), the specific method is as follows: putting the substrate with metal oxide film on the surface of the substrate with the oxide film facing downwards on a quartz tile boat with the size equal to that of the substrate, pushing the quartz tile to the center of a reaction area of a plasma enhanced tube furnace, pumping the quartz tile to the pressure in the quartz tube less than 1Pa by using a mechanical pump, introducing argon gas of 5-30sccm at the moment, wherein the pressure in the quartz tube is 10-35Pa at the moment, heating the reaction zone to 400-800 ℃ at the heating rate of 5-30 ℃/min, stopping introducing argon after the target temperature is reached, simultaneously introducing nitrogen of 1-30sccm, turning on the power supply of the plasma module, setting the plasma power to 10-80W (specifically 10W) and starting, reacting for 5-90 min (specifically 20 min), and closing the plasma switch, and rapidly cooling the furnace body to room temperature within twenty minutes, wherein the atmosphere in the reaction chamber is kept unchanged by nitrogen.
Compared with the prior art, the invention has the following advantages:
after the substrate is treated by the oxygen plasma in the early stage, the bonding force between the oxide formed on the surface of the liquid metal and the substrate can be obviously increased, the unstable oxide on the upper layer is etched by a nitrogen plasma enhanced chemical vapor deposition system, and the oxide is nitrided at the same time, so that the large-area ultrathin two-dimensional nitride film is finally obtained. The prepared nitride film can be as low as 0.8nm and is a single layer or a double layer. The prepared nitride film can be deposited on different substrates and can also be transferred to any other target substrate, and the characteristic of independence of the substrate enables the two-dimensional nitride film to have wider application prospect.
Drawings
FIG. 1 is a flow chart of the growth of the present invention; firstly, processing a substrate by using an oxygen plasma cleaning machine, then extruding metal liquid drops by using two substrates, obtaining a uniform oxidation film after simple cleaning, putting the obtained oxidation 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 thin film before and after nitridation in example 1 of the present invention; 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 thin film prepared in example 1 of the present invention.
FIG. 5 is X-ray photoelectron spectroscopy (XPS) data of a two-dimensional gallium nitride thin film prepared according to example 1 of the present invention; wherein, a is the fine scanning spectrum of the N1s orbit, and b is the fine scanning spectrum of the Ga2p orbit.
FIG. 6 shows X-ray photoelectron spectroscopy (XPS) data of a two-dimensional indium nitride thin film prepared in example 2 of the present invention.
FIG. 7 shows Atomic Force Microscope (AFM) data of a gallium nitride thin film obtained by a reaction for 10 minutes at a power of 100W.
FIG. 8 is an optical microscope photograph of a gallium oxide film deposited on the surface of a silicon oxide wafer without plasma pretreatment.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1 preparation of ultra-thin gallium nitride Using silicon wafer with silicon oxide layer and liquid Metal gallium
According to the process in fig. 1, the method for preparing ultrathin gallium nitride specifically comprises the following steps:
(1) cutting a silicon wafer (with the thickness of 0.5mm, wherein the thickness of the silicon oxide layer is 90nm) with a diamond knife into the size of 1cm x 1cm, sequentially cleaning the silicon wafer with acetone, isopropanol and deionized water for 10 minutes, putting the cleaned silicon oxide wafer into an oxygen plasma cleaning machine, controlling the pressure of introduced oxygen to be 110Pa, and cleaning for 3 minutes.
(2) The silicon oxide layers of the two treated silicon oxide wafers face upward and are placed on a heating table at the temperature of 50 ℃, a drop (about 5mg) of metal gallium stored in isopropanol is taken out by a rubber head dropper and is placed on one of the silicon oxide wafers, and the other silicon oxide wafer is taken up by tweezers and the metal drop is extruded to be 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 the two silicon oxide wafers cannot slide transversely in the process, placing the separated silicon oxide wafers into isopropanol, simply cleaning the silicon oxide wafers by using cotton swabs, and cleaning off metal residues on the surfaces to obtain clean and uniform oxide films.
(4) Placing the prepared oxide film on a heating table, placing the silicon oxide wafer with the metal oxide film with the front surface facing downwards on a quartz tile after the organic solvent on the surface of the silicon oxide wafer is volatilized, sending the silicon oxide wafer into a reaction area of a plasma enhanced chemical vapor deposition system, pumping the silicon oxide wafer with the metal oxide film with the front surface facing downwards to the pressure of less than 1Pa by using a mechanical pump, introducing 20sccm argon, and heating the silicon oxide wafer to 800 ℃ at the speed of 30 ℃/min.
(5) And after the temperature rises to 800 ℃, stopping introducing the argon gas, introducing 5-30sccm nitrogen gas, opening a switch of the plasma module, setting the power to 10W and starting.
(6) After the reaction is carried out for 20 minutes, the plasma is closed, the temperature of the furnace body is rapidly reduced to room temperature, and the atmosphere in the reaction chamber is kept unchanged during the period.
(7) Taking out the nitrided sample, observing the appearance of the nitrided sample by using an optical microscope and a Scanning Electron Microscope (SEM), determining the uniformity and the size of the film, determining the element composition of the material by using X-ray photoelectron spectroscopy (XPS), and determining the thickness and the surface uniformity of the nitrided sample by using an Atomic Force Microscope (AFM).
The optical microscope photographs before and after nitridation of the gallium oxide film prepared in the example are shown in fig. 2, and as can be seen from fig. 2, the contrast of the film sample subjected to plasma nitridation on the silicon oxide wafer is obviously reduced, which shows the ultrathin property of the film, the color of the film is uniform, and the thickness of the film prepared by reaction is uniform.
The Atomic Force Microscope (AFM) data of the gallium oxide thin 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 thin film is 3 nm.
The Atomic Force Microscope (AFM) data of the two-dimensional gallium nitride thin film prepared in this example are shown in fig. 4, and it can be seen from fig. 4 that the thickness of the two-dimensional gallium nitride is as low as 0.8nm and is a monolayer. Comparing with fig. 3, the thickness of the gallium nitride after nitridation is obviously thinner than that of the gallium oxide film before nitridation due to the etching effect of the nitrogen plasma.
The X-ray photoelectron spectroscopy (XPS) data of the two-dimensional gallium nitride thin film prepared in this example is shown in fig. 5, and it can be seen from fig. 5 that the fine scanning spectra of orbitals of N1s and Ga2p show that Ga atoms and N atoms are bonded to each other to obtain a gallium nitride material.
Example 2 preparation of ultra-thin indium gallium nitride Using silicon oxide wafer and gallium indium alloy
(1) Cutting a silicon wafer (with the thickness of 0.5mm, wherein the thickness of the silicon oxide layer is 90nm) with a diamond knife into the size of 1cm x 1cm, sequentially cleaning the silicon wafer with acetone, isopropanol and deionized water for 10 minutes, putting the cleaned silicon oxide wafer into an oxygen plasma cleaning machine, controlling the pressure of introduced oxygen to be 110Pa, and cleaning for 3 minutes.
(2) In a glove box, adding indium and gallium in a mass ratio of 1: 1, placing the mixture in a beaker, heating and stirring the mixture, setting the temperature of a heating table to be 75 ℃, and placing the mixture in an isopropanol solution for standby after fully and uniformly stirring the mixture.
(3) Placing two processed silicon oxide wafers on a heating table at the temperature of 100 ℃ with the silicon oxide layers facing upwards, placing the prepared gallium-indium alloy (about 10mg) on one silicon oxide wafer, taking the other silicon oxide wafer by using tweezers after the gallium-indium alloy is molten, and extruding the molten metal to spread the metal on the silicon oxide wafer.
(4) 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 the two silicon oxide wafers cannot slide transversely 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 silicon oxide wafer with the sample on a quartz tile with the front surface facing downwards after the organic solvent on the surface of the silicon oxide film is volatilized, sending the silicon oxide wafer into a reaction zone of a plasma enhanced chemical vapor deposition system, pumping the silicon oxide wafer with the sample until the air pressure is less than 1Pa by using a mechanical pump, introducing 20sccm argon, and heating the silicon oxide film to 500 ℃ at the speed of 20 ℃/min.
(6) And after the temperature rises to 500 ℃, stopping introducing the argon, introducing 5-30sccm nitrogen, opening a switch of the plasma module, setting the power to 10W and starting.
(7) After the reaction is carried out for 20 minutes, the plasma is closed, the temperature of the furnace body is rapidly reduced to room temperature, and the atmosphere in the reaction chamber is kept unchanged during the period.
(8) Taking out the nitrided sample, observing the appearance of the nitrided sample by using an optical microscope and a Scanning Electron Microscope (SEM), determining the uniformity of the film, determining the elemental composition of the material by using X-ray photoelectron spectroscopy (XPS), and determining the thickness and the surface uniformity of the nitrided sample by using an Atomic Force Microscope (AFM).
The X-ray photoelectron spectroscopy (XPS) data of the two-dimensional indium gallium nitride thin film prepared In this example is shown In fig. 6, and as can be seen from fig. 6, global scanning 6a indicates that the obtained alloy thin film contains Ga element and In element, and fine scanning spectra of N1s orbital 6b and In3d orbital 6c indicate that the two-dimensional indium gallium nitride alloy thin film is successfully prepared.
EXAMPLE 3 Effect of Nitrogen plasma on film thickness uniformity
In example 1, the reaction plasma power was increased, and it was found that the surface morphology of the thin film was damaged by too high power, as shown in fig. 7, the nitrogen plasma power was increased to 100W during the reaction, and the surface roughness of the thin film measured by AFM was significantly increased, and therefore, it was necessary to maintain the plasma power at a moderate level for the uniform synthesis of two-dimensional ultra-thin nitride.
EXAMPLE 4 Effect of oxygen plasma on substrate pretreatment
In example 1, the oxygen plasma pretreatment step was performed to remove the metal oxide from the substrate, and the adhesion of the metal oxide to the substrate was significantly reduced, and the metal oxide film was significantly damaged by a simple process of peeling off the residual metal with a cotton swab, as shown in fig. 8. The metal oxide film pretreated by the oxygen plasma is more tightly combined with the substrate, the film cannot be damaged in the process of stripping residual metal, and the finally prepared nitride film is more uniform.
Claims (9)
1. A preparation method of a large-area ultrathin two-dimensional nitride material comprises the following steps:
1) the method comprises the following steps of pretreating a substrate in an oxygen plasma environment to provide more active sites for adsorption of oxygen atoms;
2) placing the two pretreated substrates in the step 1) on a heating table, placing metal on the surface of one substrate, covering the other substrate after the metal is molten and extruding liquid metal to enable the two substrates to be kept in a superposed state and stand, then separating the two substrates, removing metal residues on the surfaces, and obtaining a metal oxide film on the surface of the substrate;
3) and (3) putting the substrate with the oxide film on the surface into a plasma enhanced chemical vapor deposition system, introducing nitrogen plasma, and etching the unstable area on the surface of the oxide film while nitriding the oxide film to finally obtain the ultrathin two-dimensional nitride film.
2. The method of claim 1, wherein: 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 or 2, characterized in that: in the step 1), the pretreatment is performed in an oxygen plasma cleaning machine, and the pressure of the introduced oxygen is controlled to be 100-240Pa and the cleaning is performed for 2-30 minutes.
4. The method according to any one of claims 1-3, wherein: 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 in a solid or liquid state.
5. The method of 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 of claim 4, wherein: the metal is liquid low-melting-point metal or alloy, and can be directly covered by another substrate and extruded with the liquid metal; 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 any one of claims 1-6, wherein: in the step 2), the standing time is 2-120 minutes.
8. The method according to any one of claims 1-7, wherein: in the step 3), the specific method is as follows: placing an oxide film surface of a substrate with an oxide film on the surface downwards on a quartz tile, sending the substrate into a reaction area of a plasma enhanced chemical vapor deposition system, pumping the substrate to the pressure of less than 1Pa by using a mechanical pump, introducing 5-30sccm argon, heating to 400-800 ℃ at the speed of 5-30 ℃/min, stopping introducing the argon, introducing 5-30sccm nitrogen, opening a switch of a plasma module, setting the power to 10-80W and starting, after reacting for 5-90 min, closing the plasma, rapidly cooling the temperature of a furnace body to room temperature, and keeping the atmosphere in the reaction chamber unchanged during the period.
9. A large-area ultra-thin two-dimensional nitride material prepared by the method of any one of claims 1 to 8.
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| CN116288276A (en) * | 2023-03-22 | 2023-06-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing monoatomic layer two-dimensional nitride |
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| 蒋百灵,张先锋,朱静: "铝、镁合金微弧氧化技术研究现状和产业化前景", 金属热处理, no. 01 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113549898A (en) * | 2021-08-13 | 2021-10-26 | 安徽泽众安全科技有限公司 | Two-dimensional gallium nitride film domain-limited template preparation method and prepared two-dimensional gallium nitride film |
| CN113549898B (en) * | 2021-08-13 | 2023-07-25 | 安徽泽众安全科技有限公司 | Preparation method of two-dimensional gallium nitride film finite field template and prepared two-dimensional gallium nitride film |
| CN116288276A (en) * | 2023-03-22 | 2023-06-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing monoatomic layer two-dimensional nitride |
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| CN113013020B (en) | 2023-06-27 |
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