CN115369379B - Preparation method of GaN nanowire and GaN nanowire - Google Patents

Preparation method of GaN nanowire and GaN nanowire Download PDF

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CN115369379B
CN115369379B CN202110543134.8A CN202110543134A CN115369379B CN 115369379 B CN115369379 B CN 115369379B CN 202110543134 A CN202110543134 A CN 202110543134A CN 115369379 B CN115369379 B CN 115369379B
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CN115369379A (en
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刘志强
闫岩
张硕
伊晓燕
王军喜
李晋闽
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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Abstract

The invention discloses a preparation method of a GaN nanowire and the GaN nanowire, wherein the preparation method comprises the following steps: preparing a two-dimensional material layer on a substrate to obtain a composite growth template; preparing a metal film layer on the two-dimensional material layer of the composite growth template; and arranging the composite growth template with the metal film layer in growth equipment to grow the GaN nanowire.

Description

Preparation method of GaN nanowire and GaN nanowire
Technical Field
The invention relates to the technical field of nanowire preparation, in particular to a preparation method for a GaN nanowire grown by two-dimensional material assistance.
Background
The GaN material is a wide bandgap semiconductor material with a direct bandgap, and has the characteristics of high saturated electron drift speed, high breakdown voltage, excellent thermal stability and the like. The excellent physical properties lead the GaN material to have wide application prospect in various fields such as electronics, photoelectrons, piezoelectricity, thermoelectricity and the like.
GaN nanowires are used as low-dimensional semiconductor nanostructures, which possess unique dimensional characteristics and performance advantages due to their ability to strongly constrain two dimensions of electrons, holes, and photons. In addition, compared with a GaN film, the GaN nanowire has the advantages of no defect, low dimensional error and the like, so that the GaN nanowire has great potential application in the fields of light emitting diodes, field effect transistors and solar cells.
The growth mechanism of GaN nanowires can be divided into three types: gas-liquid-solid, gas-solid and gas-solid growth modes. The gas-liquid-solid growth mechanism has a faster growth rate than the other two growth mechanisms. However, in the gas-liquid-solid growth mechanism, the gas-solid growth mechanism is often carried out simultaneously, and the lateral growth of the nanowire is aggravated under the growth mechanism, so that the diameter of the nanowire is increased, the quality of the crystal is degraded, and the working performance of the device is further affected. In addition, large diameter nanowires are not beneficial to the performance of device integration process, and increase the process difficulty.
Disclosure of Invention
First, the technical problem to be solved
The invention discloses a preparation method of a GaN nanowire, which aims to at least partially solve the technical problems.
(II) technical scheme
In order to achieve the above object, an embodiment of the present invention provides a method for preparing a GaN nanowire, including: preparing a two-dimensional material layer on a substrate to obtain a composite growth template; preparing a metal film layer on the two-dimensional material layer of the composite growth template; and arranging the composite growth template with the metal film layer in growth equipment to grow the GaN nanowire.
According to an embodiment of the invention, the material of the substrate comprises Si, al 2O3, siC, gaN or GaAs.
According to an embodiment of the present invention, before the preparing the two-dimensional material layer on the substrate, further includes: cleaning the substrate by using a chemical solution, wherein the chemical solution comprises a mixed solution of concentrated sulfuric acid and hydrogen peroxide, or the chemical solution comprises an acetone and ethanol solution, and the ratio of the concentrated sulfuric acid to the hydrogen peroxide in the mixed solution is 1.5:1-4:1; in the case where the solution is acetone and ethanol, the acetone solution is used first, and then the ethanol solution is used.
According to the embodiment of the invention, the material of the two-dimensional material layer comprises at least one of graphene, molybdenum disulfide and tungsten disulfide.
According to an embodiment of the invention, the metal of the thin metal layer comprises at least one of Au, ni, pt, al, fe.
According to an embodiment of the invention, the thickness of the metal film layer is
According to an embodiment of the invention, the working temperature of the growth device is 500-1400 ℃.
According to an embodiment of the invention, the reaction gas in the growth apparatus comprises a first mixed component consisting of TMGa, TEGa, NH 3、N2 and H 2 or a second mixed component consisting of HCl, NH 3 and N 2; the reaction gas is introduced into the growth equipment for 2 to 10 minutes.
According to an embodiment of the present invention, further comprising: closing TMGa gas when the reaction gas is the first mixed component and the working temperature of the growth equipment is higher than 700 ℃, and closing NH 3 gas when the working temperature is lower than or equal to 700 ℃; and when the working temperature of the growth equipment is lower than or equal to 700 ℃, closing NH 3 gas.
The embodiment of the invention provides a GaN nanowire which is prepared based on any preparation method.
(III) beneficial effects
According to the preparation method of the GaN nanowire disclosed by the invention, the two-dimensional material/substrate composite growth template is utilized to promote the gas-liquid-solid growth, and the gas-solid growth is inhibited, so that the transverse growth of the nanowire is inhibited, the diameter of the nanowire is reduced, the crystal quality is further improved, the superfine GaN nanowire can be rapidly grown, and the performance of a subsequent device is improved; meanwhile, the process difficulty is reduced, and the production cost is greatly reduced.
Drawings
Fig. 1 schematically presents a flow chart of a GaN nanowire according to an embodiment of the invention;
FIG. 2 is a schematic diagram of a two-dimensional material/substrate composite growth template according to an embodiment of the invention;
FIG. 3 is a scanning electron microscope image of metal pellets automatically generated from a metal thin film in a high temperature environment according to an embodiment of the present invention;
FIG. 4 is a low-magnification scanning electron microscope image of GaN nanowires grown with the assistance of two-dimensional material on C-plane sapphire Al 2O3 in accordance with an embodiment of the present invention;
FIG. 5 is a high-power scanning electron microscope image of GaN nanowires grown with the assistance of two-dimensional material on C-plane sapphire Al 2O3 in accordance with an embodiment of the present invention;
fig. 6 is a photoluminescence spectrum of a two-dimensional material layer-assisted grown GaN nanowire according to an embodiment of the invention.
Reference numerals:
1: a substrate; 2: a two-dimensional material layer; 3: a metal film layer.
Detailed Description
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
An embodiment of the present invention provides a method for preparing a GaN nanowire, including: preparing a two-dimensional material layer on a substrate to obtain a composite growth template; preparing a metal film layer on the two-dimensional material layer of the composite growth template; and arranging the composite growth template with the metal film layer in growth equipment to grow the GaN nanowire.
Fig. 1 schematically presents a flow chart of a GaN nanowire according to an embodiment of the invention.
As shown in fig. 1, the flow includes operations S101 to S103.
In operation S101, a two-dimensional material layer is prepared on a substrate to obtain a composite growth template.
According to an embodiment of the invention, the material of the substrate comprises Si, al 2O3, siC, gaN or GaAs.
In the embodiment of the present invention, the material of the substrate may be, for example, C-plane sapphire Al 2O3.
According to the embodiment of the invention, before the two-dimensional material layer is prepared on the substrate, the substrate is cleaned by using a chemical solution, wherein the chemical solution comprises a mixed solution of concentrated sulfuric acid and hydrogen peroxide, or the chemical solution comprises an acetone and ethanol solution, and the ratio of the concentrated sulfuric acid to the hydrogen peroxide in the mixed solution is 1.5:1-4:1; in the case where the solution is acetone and ethanol, the acetone solution is used first, and then the ethanol solution is used.
In the embodiment of the invention, the chemical solution may be, for example, a mixed solution of concentrated sulfuric acid and hydrogen peroxide, where the ratio of the concentrated sulfuric acid to the hydrogen peroxide may be, for example, 3:1; the substrate is put into the mixed solution to be cleaned for 10 minutes, so that organic pollution and impurity particles on the surface of the substrate can be removed; then washing with deionized water for 5 minutes; finally, the surface of the dry substrate is blown by N 2 to clean the substrate.
According to the embodiment of the invention, the material of the two-dimensional material layer comprises at least one of graphene, molybdenum disulfide and tungsten disulfide.
In an embodiment of the invention, the two-dimensional material layer may be transferred to the substrate by wet etching to obtain a composite growth template.
In the embodiment of the invention, the two-dimensional material layer can also be directly grown on the substrate to obtain the composite growth template.
In an embodiment of the present invention, a schematic diagram of a two-dimensional material/substrate composite growth template according to an embodiment of the present invention is shown in fig. 2. The two-dimensional material/substrate composite growth template as in fig. 2 comprises a substrate 1 and a two-dimensional material layer 2, and a metal film layer 3 is prepared on the two-dimensional material layer 2 of the composite growth template.
In operation S102, a metal thin film layer is prepared.
According to an embodiment of the invention, the metal of the thin metal layer comprises at least one of Au, ni, pt, al, fe; the thickness of the metal film layer is
In an embodiment of the present invention, the metal thin film layer may be evaporated on the two-dimensional material layer of the composite growth template using an electron beam evaporation apparatus, and the metal thin film layer may include, for example, an Au metal thin film layer and an Ni metal thin film layer. For example, an Au metal thin film layer may be deposited at a deposition rate of 0.05nm/s, and an Ni metal thin film layer may be deposited on the Au metal thin film layer at a deposition rate of 0.05 nm/s. The thickness of the metal film may be, for example
In embodiments of the invention, the evaporated metal may act as a catalyst to assist in nanowire growth. For example, the high temperature environment can automatically form metal pellets on the metal film layer in the subsequent growth process, and gas molecules react inside the pellets to grow GaN nanowires. The two-dimensional material layer can accelerate the adsorption and migration of gas molecules into the metal pellets, and promote the longitudinal growth of the nanowires, as shown in figure 3.
In operation S103, a GaN nanowire is grown.
According to an embodiment of the invention, the working temperature of the growth device is 500-1400 ℃.
According to an embodiment of the invention, the reaction gas in the growth apparatus comprises a first mixed component consisting of TMGa, TEGa, NH 3、N2 and H 2 or a second mixed component consisting of HCl, NH 3 and N 2; the reaction gas is introduced into the growth equipment for 2 to 10 minutes.
According to the embodiment of the invention, when the reaction gas is the first mixed component and the working temperature of the growth equipment is higher than 700 ℃, TMGa and TEGa gases are closed, and when the working temperature is lower than or equal to 700 ℃, NH 3 gas is closed again; and closing HCl gas under the condition that the reaction gas is the second mixed component and the working temperature of the growth equipment is higher than 700 ℃, and closing NH 3 gas under the condition that the working temperature is lower than or equal to 700 ℃.
In an embodiment of the present invention, the process of growing GaN nanowires by disposing the above composite growth template with the metal thin film layer in the growth apparatus may be represented, for example: first, the growth apparatus is warmed up from room temperature to an operating temperature, which may be 900 ℃, for example, at a warming rate of 10 ℃/min. And secondly, introducing the above reaction gas, for example, the reaction gas may be TMGa, TEGa, NH 3、N2 and H 2, the time for introducing the reaction gas may be 4 minutes, wherein the flow rate of introducing the TMGa gas may be 4sccm, the flow rate of introducing the TEGa gas may be 4sccm, the flow rate of introducing the NH 3 gas may be 100sccm, the flow rate of introducing the N 2 gas may be 2slm, the flow rate of introducing the H 2 gas may be 2slm, and the reaction gas flow may be diluted by introducing the N 2 and H 2 gases while helping the reaction gas smoothly enter the growth apparatus. And finally, closing the introduction of TMGa and TEGa gas when the introduction time reaches 4 minutes, then performing cooling operation on the growth equipment, and closing the introduction of NH 3 gas after the working temperature is equal to 700 ℃. And finally, the working temperature is reduced to room temperature, and the preparation of the GaN nanowire is completed. The NH 3 gas is introduced when the working temperature is reduced to 700 ℃, because GaN material is stable under NH 3 gas at high temperature and is prevented from decomposing in high temperature environment.
In an embodiment of the present invention, the process of growing GaN nanowires by disposing the composite growth template with the metal thin film layer in the growth apparatus may be represented as: first, the growth apparatus is warmed up from room temperature to an operating temperature, which may be 600 ℃ for example, at a warming rate of 10 ℃/min. And secondly, introducing the above reaction gas, for example, the reaction gas may be TMGa, TEGa, NH 3、N2 and H 2, the time of introducing the reaction gas may be 4 minutes, wherein the flow rate of introducing the TMGa gas may be 4sccm, the flow rate of introducing the TEGa gas may be 4sccm, the flow rate of introducing the NH 3 gas may be 100sccm, the flow rate of introducing the N 2 gas may be 2slm, the flow rate of introducing the N 2 gas may be 2slm, and the reaction gas may be assisted in smoothly entering the growth apparatus while diluting the reaction gas flow by introducing the N 2 and H 2 gases. And finally, when the access time reaches 4 minutes, closing the reaction gas flow, and cooling the growth equipment to room temperature to finish the preparation of the GaN nanowire grown by the two-dimensional material.
In an embodiment of the present invention, the process of growing GaN nanowires by disposing the composite growth template with the metal thin film layer in the growth apparatus may be represented as: first, the growth apparatus is warmed up from room temperature to an operating temperature, which may be 800 ℃, for example, at a warming rate of 10 ℃/min. Secondly, the above-mentioned reaction gas, for example, the reaction gas may be HCl, NH 3 and N 2, the time for introducing the reaction gas may be 4 minutes, wherein the flow rate of introducing the HCl gas may be 8sccm, the flow rate of introducing the NH 3 gas may be 100sccm, the flow rate of introducing the N 2 gas may be 4slm, and the effect of introducing the N 2 gas is to dilute the reaction gas flow and simultaneously help the reaction gas smoothly enter the growth apparatus. And finally, when the inlet time reaches 4 minutes, closing the inlet of HCl gas, then cooling the growth equipment, closing the inlet of NH 3 gas after the working temperature is equal to 700 ℃, and finally cooling the working temperature to room temperature to finish the preparation of the GaN nanowire. The NH 3 gas is introduced when the working temperature is reduced to 700 ℃, because GaN material is stable under NH 3 gas at high temperature and is prevented from decomposing in high temperature environment.
In an embodiment of the present invention, the process of growing GaN nanowires by disposing the composite growth template with the metal thin film layer in the growth apparatus may be represented as: first, the growth apparatus is warmed up from room temperature to an operating temperature, which may be 600 ℃ for example, at a warming rate of 10 ℃/min. Secondly, the above-mentioned reaction gas, for example, the reaction gas may be HCl, NH 3 and N 2, the time for introducing the reaction gas may be 4 minutes, wherein the flow rate of introducing the HCl gas may be 8sccm, the flow rate of introducing the NH 3 gas may be 100sccm, the flow rate of introducing the N 2 gas may be 4slm, and the effect of introducing the N 2 gas is to dilute the reaction gas flow and simultaneously help the reaction gas smoothly enter the growth apparatus. And finally, when the feeding time reaches 4 minutes, closing the flow of the reaction gas, and cooling the temperature of the growth equipment to the room temperature to finish the preparation of the GaN nanowire grown by the two-dimensional material.
Another embodiment of the present invention provides a GaN nanowire, which may be prepared based on the preparation method described in any one of the above embodiments.
In an embodiment of the present invention, fig. 4 is a low-power scanning electron microscope image of the GaN nanowire grown with the assistance of the two-dimensional material layer on the C-plane sapphire Al 2O3 according to an embodiment of the present invention, and fig. 5 is a high-power scanning electron microscope image of the GaN nanowire grown with the assistance of the two-dimensional material layer on the C-plane sapphire Al 2O3 according to an embodiment of the present invention, the GaN nanowire grown by the assistance of the two-dimensional material layer may have a lower diameter as observed by a scanning electron microscope, wherein the diameter of the GaN nanowire may be 20nm to 40nm.
In an embodiment of the present invention, fig. 6 is a photoluminescence spectrum of the GaN nanowire grown with the assistance of the two-dimensional material layer according to an embodiment of the present invention, through which no distinct yellow band can be seen, indicating that the quality of the grown GaN nanowire is superior.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the invention thereto, but to limit the invention thereto, and any modifications, equivalents, improvements and equivalents thereof may be made without departing from the spirit and principles of the invention.

Claims (8)

1. A method of fabricating a GaN nanowire, comprising:
Preparing a two-dimensional material layer on a substrate to obtain a composite growth template;
preparing a metal film layer on the two-dimensional material layer of the composite growth template;
setting the composite growth template with the metal film layer in growth equipment to grow GaN nanowires;
The reaction gas in the growth device comprises a first mixed component consisting of TMGa, TEGa, NH 3、N2 and H 2 or a second mixed component consisting of HCl, NH 3 and N 2;
The working temperature of the growth equipment is 500-1400 ℃, so that the metal film layer automatically forms metal pellets, and the two-dimensional material layer accelerates the reaction gas to be adsorbed and migrated into the metal pellets;
the material of the two-dimensional material layer comprises at least one of graphene, molybdenum disulfide and tungsten disulfide.
2. The method of manufacturing according to claim 1, wherein the material of the substrate comprises Si, al 2O3, siC, gaN, or GaAs.
3. The method of manufacturing of claim 1, wherein prior to preparing the two-dimensional material layer on the substrate, further comprising:
Cleaning the substrate by using a chemical solution, wherein the chemical solution comprises a mixed solution of concentrated sulfuric acid and hydrogen peroxide, or the chemical solution comprises an acetone and ethanol solution, and the ratio of the concentrated sulfuric acid to the hydrogen peroxide in the mixed solution is 1.5:1-4:1; in the case where the solutions are acetone and ethanol, the acetone solution is used first, and then the ethanol solution is used.
4. The method of manufacturing of claim 1, wherein the metal of the metal film layer comprises at least one of Au, ni, pt, al, fe.
5. The production method according to claim 1, wherein the thickness of the metal thin film layer is
6. The production method according to claim 1, wherein the reaction gas is introduced into the growth apparatus for a period of 2 to 10 minutes.
7. The preparation method according to claim 6, further comprising:
Closing TMGa and TEGa gases when the reaction gas is the first mixed component and the working temperature of the growth equipment is higher than 700 ℃, and closing NH 3 gas when the working temperature is lower than or equal to 700 ℃;
And closing HCl gas under the condition that the reaction gas is the second mixed component and the working temperature of the growth equipment is higher than 700 ℃, and closing NH 3 gas under the condition that the working temperature is lower than or equal to 700 ℃.
8. A GaN nanowire, wherein the GaN nanowire is prepared based on the preparation method of any one of claims 1 to 7.
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