CN112210768A - Epitaxial method of vertical beta gallium oxide nanowire array - Google Patents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/08—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of gallium, indium or thallium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/56—After-treatment
Abstract
The invention discloses an epitaxial method of a vertical beta gallium oxide nanowire array, which comprises the steps of introducing a Ga source and an O source, and epitaxially growing the nanowire array on the surface of a substrate by utilizing a Ga catalyst autocatalysis method, wherein the epitaxial growth temperature is 400-550 ℃. The preparation method realizes the preparation of the nanowire array with high crystallization quality vertical to the surface of the substrate by utilizing the Ga liquid drop autocatalysis technology, and avoids the unintentional doping pollution of other catalysts to epitaxial materials. The invention can realize beta-Ga at the low temperature of below 500 DEG C2O3The epitaxial preparation of the nano wire can effectively save energy consumption.
Description
Technical Field
The invention belongs to the technical field of semiconductor epitaxy, and particularly relates to an epitaxy method of a vertical beta gallium oxide nanowire array.
Background
In the prior art, the growth method of the beta gallium oxide nanowire array mainly comprises oblique array epitaxy, vertical array Au catalytic epitaxy and Ga-containing compound vertical nanowire array oxidation.
Inclined array epitaxy: up to now, the epitaxial beta gallium oxide nanowires reported in the literature all have a certain angle with the substrate, and the gallium oxide nanowires prepared by different subject groups have inconsistent orientation. Because the mesh planarization of the interweaving of the oblique arrays is difficult, the position control of functional junctions such as pn junctions and heterojunctions is difficult to control, and the preparation of the nanowire array device is limited due to the difficult implementation of a complex process. Currently based on Ga2O3The gas sensing device prepared by the nanowires is mostly prepared based on the nanowire array arranged in random orientation, and electronic and optoelectronic devices such as FET and a photodetector are mostly prepared based on a single nanowire or a parallel nanowire array arranged in a re-operated manner, so that the repeatability and uniformity of the performance of the device are poor, and the batch preparation is difficult.
Vertical array Au catalytic epitaxy: chang Ko-wei and Wu Jih-Jen of Taiwan successful university in China in 2004 published results on Advanced Materials, and Au catalytic vertical gallium oxide nanowire array epitaxy preparation is carried out by utilizing a single MO source, but generally, residue of Au catalyst in the nanowire out-process can cause unintended doping, and the photoelectric property of the material is seriously influenced.
Oxidizing the Ga-containing compound vertical nanowire array: preparation of Ga by GaN nanowire array oxidation2O3For example, nanowires are poor in surface morphology and crystallization quality due to large lattice mismatch and large difference of crystal structures in the conversion process, so that the carrier transport characteristics of the nanowires are greatly limited, and the application of devices is not facilitated.
How to prepare nanowire array Ga with uniform appearance vertical to substrate2O3Nanowire materials are an urgent problem to be solved.
Disclosure of Invention
An embodiment of the present invention provides an epitaxy method for a vertical beta-gallium oxide nanowire array, which is used to solve the problems of nanowire tilt, unintentional doping, lattice mismatch, etc. in the prior art, and includes:
in one embodiment, a method for epitaxy of vertical-type beta-gan nanowire arrays is provided, comprising: introducing Ga source and O source, epitaxially growing a nanowire array on the surface of the substrate by using a Ga catalyst autocatalysis method,
the epitaxial growth temperature is 400-550 ℃.
In one embodiment, a method for epitaxy of vertical-type beta-gan nanowire arrays is provided, comprising:
s1, introducing an oxygen source into the reaction cavity, and pretreating the substrate at 720-850 ℃;
in the technical scheme, the treatment temperature of the substrate is preferably 720 ℃, and the main purpose is to form a thin random mask layer in situ, and the thin random mask layer is mainly used for optimizing the epitaxial result of the random array.
s2, laying a medium on the surface of the substrate, opening holes, and depositing a catalyst in the holes at the temperature of 350-500 ℃;
in the technical scheme, the diameter of the catalyst is effectively controlled by combining an annealing technology, generally not higher than 500 ℃, and in order to ensure that the Ga source is effectively cracked, generally not lower than 350 ℃, and preferably 450 ℃.
s3, annealing the catalyst, wherein the annealing temperature is 500-800 ℃;
s4, introducing a Ga source and an O source, and epitaxially growing the nanowire array on the surface of the substrate by using a Ga catalyst autocatalysis method, wherein the epitaxial growth temperature is 400-550 ℃.
Compared with the prior art, the invention has the advantages that:
1) the preparation of the nanowire array with high crystallization quality vertical to the surface of the substrate is realized by utilizing the Ga liquid drop autocatalysis technology, and the unintentional doping pollution of other catalysts to the epitaxial material is avoided;
2) compared with the technology for preparing the vertical nanowire array by oxidizing the Ga-containing nanowires, the method can flexibly control the doping of the nanowires by introducing a doping source in the growth process;
3) the realization of the vertical substrate nanowire array epitaxy does not depend on complete guided mode, namely, an implementation scheme for realizing ordered array epitaxy of nanowires by using a thin medium exists, but the existing epitaxy direction can be still maintained without change after the growth height of the nanowires exceeds the surface of a mask;
4) the invention can realize beta-Ga at the low temperature of below 500 DEG C2O3The epitaxial preparation of the nano wire can effectively save energy consumption.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a timing diagram illustrating the fabrication of vertical-type beta gallium oxide nanowire arrays according to a first embodiment of the present application;
FIG. 2 is a schematic structural diagram of a vertical-type beta gallium oxide nanowire array according to a first embodiment of the present application;
FIG. 3 is an SEM image of the structure of a vertical-type beta gallium oxide nanowire array in a first embodiment of the present application;
FIG. 4 is an SEM top view of a structure of a vertical beta gallium oxide nanowire array according to a first embodiment of the present application;
FIG. 5 is a schematic structural diagram of a vertical-type beta gallium oxide nanowire array according to a second embodiment of the present application;
fig. 6 is an SEM image of the structure of a vertical type β -ga nanowire array in the second embodiment of the present application.
Detailed Description
The present invention will be more fully understood from the following detailed description, which should be read in conjunction with the accompanying drawings. Detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which can be embodied in various forms. Therefore, specific functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed embodiment.
As shown in fig. 2, the present embodiment provides a vertical type β gallium oxide nanowire array, which includes a substrate 1, a β gallium oxide nanowire array 2 vertically grown on a surface of the substrate 1, and a Ga catalyst 3 located at a top end of the β gallium oxide nanowire array 2.
In one embodiment, the substrate 1 is preferably a sapphire or GaN substrate.
The embodiment also provides an epitaxial method of the vertical beta gallium oxide nanowire array, which ensures high-quality nanowire epitaxy, particularly the epitaxial temperature, by accurately controlling the epitaxial conditions of the nanowires, so as to realize the regulation and control of the orientation of the nanowires and obtain the gallium oxide nanowire array with the vertical proportion of more than 90%.
The method provided by the embodiment can be combined with the existing selective area epitaxy method to realize the positioned and ordered growth of the nanowires, and particularly provides an epitaxy structure for devices such as array nanowire detectors, LEDs, lasers and the like.
Specifically, the epitaxial method of the vertical beta gallium oxide nanowire array comprises the following steps:
1) and processing the substrate.
It is essential to perform the necessary cleaning to avoid contamination of the epitaxy equipment or introduction of unwanted impurities during the epitaxy process.
Optionally, in order to optimize the epitaxial effect, oxygen sources are introduced into a part of the process during the substrate treatment process.
2) And spreading a Ga catalyst.
The catalyst coating method includes, but is not limited to, deposition using a metal organic source, coating metal particles, sputtering or coating a metal film.
Generally, one or more times of annealing is carried out before and after the catalyst is paved so as to achieve the purposes of cleaning the substrate, promoting the catalyst to fuse, optimizing the distribution of catalytic particles/liquid drops and the like.
3) And annealing the catalyst.
The temperature of the catalyst anneal is preferably such that the substrate is not damaged, typically from about 500 c to about 800 c.
The size of the catalytic liquid drop can be adjusted by adjusting the annealing temperature of the catalyst by utilizing the change of the diffusion length of the catalyst atoms on the surface of the substrate along with the temperature, and finally the diameter of the nanowire is adjusted.
4) And (5) extending the nanowire.
For sapphire or GaN substrates, the epitaxy temperature is about 400-550 DEG C
In the epitaxial process, Ga source and oxygen source are simultaneously introduced in proper proportion, and for sapphire or GaN substrate, the O/Ga ratio is generally not higher than 300. The pressure in the reaction chamber generally does not exceed one atmosphere.
O source is not limited to N2O, also includes H2O、O2And other oxygen-containing sources.
The Ga source is not limited to the TEGa source, and other Ga-containing or pure metal sources such as TMGa are also included.
The epitaxial equipment is not only suitable for MOCVD epitaxial equipment, but also can realize the epitaxy of vertical nanowires on other types of CVD equipment or MBE through reasonable parameter setting.
The diameter of the catalytic liquid drop can be adjusted by adjusting the O/Ga ratio during growth, and the diameter of the nanowire can be adjusted in real time, so that the morphological characteristics of the nanowire can be controlled.
The doping type and the doping concentration of the nanowire can be adjusted by introducing a doping source and adjusting the flow.
After the growth is finished, the existence of the catalyst can be maintained by simultaneously stopping the supply of the Ga source and the O source, and the introduction of the O source and the introduction of the Ga source can be maintained to eliminate the consumption of the catalyst.
Example 1
As shown in fig. 2, in this embodiment, the obtained vertical type β gallium oxide nanowire array includes a substrate 1, a β gallium oxide nanowire array 2 vertically grown on the surface of the substrate 1, and a Ga catalyst 3 located at the top end of the β gallium oxide nanowire array 2.
Referring to fig. 1, the process for manufacturing a vertical beta-gan nanowire array includes:
1) substrate processing
a) The substrate is cleaned as necessary to avoid pollution to epitaxial equipment or unnecessary impurity introduction in the epitaxial process;
b) and introducing an oxygen source in the substrate processing process, and keeping the substrate processing temperature at about 720 ℃.
2) Ga catalyst deposition
a) And preparing the Ga catalyst on the surface of the substrate by using metal organic sources for deposition, metal particle coating, sputtering or metal film coating and the like, wherein the deposition temperature of the catalyst is kept at about 450 ℃.
3) Annealing of catalyst
a) The annealing temperature of the catalyst is preferably controlled to be about 650 ℃ so as not to damage the substrate;
b) the size of the catalytic liquid drop can be adjusted by adjusting the annealing temperature of the catalyst by utilizing the change of the diffusion length of catalyst atoms on the surface of the substrate/medium along with the temperature, and finally the diameter of the nanowire is adjusted.
4) Nanowire epitaxy
a) Adjusting the temperature of the reaction chamber to an epitaxial temperature, wherein the epitaxial temperature is controlled to be about 485 ℃;
b) simultaneously introducing a Ga source and an oxygen source, wherein the Ga source adopts TEGa, and the oxygen source adopts N2O, the O/Ga ratio is about 25;
c) the pressure in the reaction chamber was set at 20 KPa.
The SEM images of the prepared vertical nanowire arrays are shown in FIGS. 3 and 4, and the obtained beta-Ga2O3The nanowire array has
The normal direction.
Example 2
Referring to fig. 5, in this embodiment, the obtained vertical type β gallium oxide nanowire array includes a substrate 1, a mask 4 laid on the surface of the substrate, through holes 41 with the mask 4 distributed thereon, a β gallium oxide nanowire array 2 vertically grown on the surface of the substrate 1 from inside the through holes 41, and a Ga catalyst 3 located at the top end of the β gallium oxide nanowire array 2.
The process for manufacturing the vertical beta gallium oxide nanowire array comprises the following steps:
1) substrate processing
a) Depositing a mask on the surface of the substrate, wherein the mask is Al2O3A mask, LP-SiNx mask or AlN mask;
b) the mask 4 is provided with through holes 41 distributed in an array.
c) The substrate is cleaned as necessary to avoid pollution to epitaxial equipment or unnecessary impurity introduction in the epitaxial process;
d) introducing an oxygen source in the substrate processing process, and keeping the substrate processing temperature at about 720 ℃;
2) ga catalyst deposition and annealing
And depositing Ga catalyst on the surface of the mask, wherein the deposition temperature is kept at about 450 ℃ and the deposition amount is reduced.
3) Annealing of catalyst
a) Diffusing the catalyst into the pre-opening hole by annealing by utilizing the crystallization state difference of the mask and the substrate, and adjusting the hole filling rate and the filling amount by combining the pre-deposition amount of the catalyst and the annealing temperature;
b) the annealing temperature of the catalyst is controlled to be about 550 ℃ for the purpose of improving the filling rate;
4) nanowire epitaxy
a) Adjusting the temperature of the reaction chamber to an epitaxial temperature, wherein the epitaxial temperature is controlled to be about 485 ℃;
b) simultaneously introducing a Ga source and an oxygen source, wherein the Ga source adopts TEGa, and the oxygen source adopts N2O, the O/Ga ratio is about 25;
c) the pressure in the reaction chamber was set at 20 KPa.
The SEM image of the prepared vertical nanowire array is shown in fig. 6.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the invention; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this disclosure, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the compositions taught by the present invention also consist essentially of, or consist of, the recited components, and that the processes taught by the present invention also consist essentially of, or consist of, the recited process steps.
Unless specifically stated otherwise, use of the terms "comprising", "including", "having" or "having" is generally to be understood as open-ended and not limiting.
The use of the singular herein includes the plural (and vice versa) unless specifically stated otherwise. Furthermore, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. In addition, where the term "about" is used before a quantity, the present teachings also include the particular quantity itself unless specifically stated otherwise.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (10)
1. An epitaxial method of a vertical beta gallium oxide nanowire array is characterized in that a Ga source and an O source are introduced, the nanowire array is epitaxially grown on the surface of a substrate by utilizing a Ga catalyst autocatalysis method, wherein,
the epitaxial growth temperature is 400-550 ℃.
2. The method of epitaxy of vertical arrays of beta-gallium oxide nanowires of claim 1, wherein: the temperature of epitaxial growth was 485 ℃.
3. The method of epitaxy of vertical arrays of beta-gallium oxide nanowires of claim 1, wherein: the Ga source is selected from TEGa or TMGa,
the O source is selected from N2O、H2O or O2。
4. The method of epitaxy of vertical arrays of beta-gallium oxide nanowires of claim 1, wherein: the ratio of the Ga source to the O source is more than 0 and less than or equal to 300.
5. The method of epitaxy of vertical arrays of beta-gallium oxide nanowires of claim 4, wherein: the ratio of the Ga source to the O source is 25.
6. The method of epitaxy of vertical arrays of beta-gallium oxide nanowires of claim 1, wherein: and introducing a doping source in the epitaxial growth process.
7. The method for the epitaxy of vertical arrays of beta-gallium oxide nanowires of claim 1, wherein the Ga catalyst is prepared by a process comprising:
laying a mask on the surface of the substrate;
forming a through hole on the mask;
and manufacturing Ga catalyst in the through hole.
8. The method of claim 1, wherein the size of the droplets is controlled by the annealing temperature during the Ga catalyst preparation process.
9. The method of epitaxy of vertical arrays of beta-gallium oxide nanowires of claim 1, wherein: in the process of growing the nanowire, the diameter of the nanowire is adjusted by controlling the ratio of the Ga source to the O source.
10. An epitaxial method of a vertical beta gallium oxide nanowire array is characterized by comprising the following steps:
s1, introducing an oxygen source into the reaction cavity, and pretreating the substrate at 720-850 ℃;
s2, laying a medium on the surface of the substrate, opening holes, and depositing a catalyst in the holes at the temperature of 350-500 ℃;
s3, annealing the catalyst, wherein the annealing temperature is 500-800 ℃;
s4, introducing a Ga source and an O source, and epitaxially growing the nanowire array on the surface of the substrate by using a Ga catalyst autocatalysis method, wherein the epitaxial growth temperature is 400-550 ℃.
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Cited By (2)
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| CN113517172A (en) * | 2021-06-07 | 2021-10-19 | 西安电子科技大学 | beta-Ga2O3Film and preparation method thereof |
| CN113643960A (en) * | 2021-06-07 | 2021-11-12 | 西安电子科技大学 | beta-Ga based on pulse method2O3Film and preparation method thereof |
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