CN111128687B - Preparation method of self-supporting gallium nitride layer - Google Patents
Preparation method of self-supporting gallium nitride layer Download PDFInfo
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- CN111128687B CN111128687B CN201911404413.5A CN201911404413A CN111128687B CN 111128687 B CN111128687 B CN 111128687B CN 201911404413 A CN201911404413 A CN 201911404413A CN 111128687 B CN111128687 B CN 111128687B
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
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Abstract
The invention relates to a preparation method of a self-supporting gallium nitride layer, which comprises the following steps: providing a substrate; forming a first gallium nitride layer on a substrate; providing oxygen-containing gas or oxygen-containing gas premixed gas to the first gallium nitride layer at a preset temperature so as to form a gallium oxide particle layer on the surface of the first gallium nitride layer; forming a second gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer; and cooling the obtained structure to strip the second gallium nitride layer so as to obtain the self-supporting gallium nitride layer. According to the invention, a gallium oxide particle layer with required diameter and density distribution can be formed as required; because the faying face of second gallium nitride layer and first gallium nitride layer has a lot of gallium oxide granules to block, lead to forming loose layer between the two, and then make the contact force greatly reduced of the two, there is thermal mismatch again between gallium nitride and the substrate at the cooling in-process, can peel off the gallium nitride layer automatically at the cooling in-process to form and peel off the gallium nitride layer certainly.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a preparation method of a self-supporting gallium nitride layer.
Background
The third generation semiconductor material is also called as a wide bandgap semiconductor because the energy bandgap is generally larger than 3.0 electron volts; compared with the traditional silicon-based and gallium arsenide-based semiconductor materials, wide-bandgap semiconductors (such as silicon carbide, gallium nitride, aluminum nitride, indium nitride and the like) have special bandgap range, excellent optical and electrical properties and excellent material performance, can meet the working requirements of high-power, high-temperature, high-frequency and high-speed semiconductor devices, and have very wide application prospects in the aspects of semiconductor devices working in the automobile and aviation industries, medical treatment, communication, military, common lighting and special conditions.
Gallium nitride has attracted attention as a typical third-generation semiconductor material having excellent properties such as a wide direct band gap and high thermal conductivity. Compared with the first generation and second generation semiconductor materials, gallium nitride has a wider forbidden band (the forbidden band width is 3.4eV at room temperature), can emit blue light with a shorter wavelength, and has the characteristics of high breakdown voltage, high electron mobility, stable chemical properties, high temperature resistance, corrosion resistance and the like. Gallium nitride is therefore well suited for the fabrication of radiation resistant, high frequency, high power and high density integrated electronic devices as well as blue, green and ultraviolet optoelectronic devices. Currently, the research and application of gallium nitride semiconductor materials have become the leading edge and hot spot of global semiconductor research.
However, the current gallium nitride single crystal growth is difficult and expensive, and large-scale homoepitaxial growth is not possible at present. At present, heteroepitaxy is still adopted for the growth of gallium nitride, and the selected heterogeneous substrates comprise a silicon substrate, a silicon carbide substrate and a sapphire substrate; the growth of gallium nitride on a foreign substrate can cause lattice mismatch and thermal mismatch, so that residual stress exists in the device to influence the performance of the device. In order to further improve device performance, it is necessary to strip gallium nitride from the foreign substrate to obtain a self-supporting gallium nitride layer.
The stripping process adopted at present mainly comprises laser stripping, self-stripping, mechanical stripping, chemical corrosion stripping and the like; however, the existing laser lift-off process, mechanical lift-off process and chemical corrosion process all need to perform an additional lift-off process after the gallium nitride growth process is completed, and process steps and process complexity are increased, so that the cost is increased, and meanwhile, the laser lift-off process, mechanical lift-off process and chemical corrosion lift-off process have strict requirements on a heterogeneous substrate, and the universality is poor; although the existing self-stripping process can realize the self-stripping of the foreign substrate and the gallium nitride, the quality of the gallium nitride is affected in the stripping process, and the yield is low.
Disclosure of Invention
In view of the above, it is necessary to provide a method for preparing a self-supporting gallium nitride layer.
A preparation method of a self-supporting gallium nitride layer comprises the following steps:
providing a substrate;
forming a first gallium nitride layer on the substrate;
providing oxygen-containing gas or oxygen-containing gas premixed gas to the first gallium nitride layer at a preset temperature so as to form a gallium oxide particle layer on the surface of the first gallium nitride layer, wherein an opening pattern exposing the first gallium nitride layer is formed in the gallium oxide particle layer;
forming a second gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer;
and cooling the obtained structure to strip the second gallium nitride layer so as to obtain the self-supporting gallium nitride layer.
According to the preparation method of the self-supporting gallium nitride layer, the oxygen-containing gas or the oxygen-containing gas premixed gas is supplied to the first gallium nitride layer at the preset temperature, so that a gallium oxide particle layer with the required diameter and density distribution can be formed as required; because the faying face on second gallium nitride layer and first gallium nitride layer has a great deal of gallium oxide granule to block, lead to forming loose layer between the two, and then make the contact force greatly reduced of the two, there is thermal mismatch between gallium nitride and the substrate again at the in-process of cooling down, can peel off the gallium nitride layer automatically at the in-process of cooling down, in order to form and peel off the gallium nitride layer certainly, the required equipment input greatly reduced manufacturing cost is peeled off to laser after having removed the cooling down promptly and peeled off, the yield of product has been improved again.
In an optional embodiment, a plurality of gallium oxide protruding particles distributed at intervals are formed on the surface of the first gallium nitride layer as the gallium oxide particle layer.
In an optional embodiment, the step of providing the oxygen-containing gas or the oxygen-containing premixed gas to the first gallium nitride layer at a predetermined temperature to form the gallium oxide particle layer on the surface of the first gallium nitride layer includes:
placing the substrate with the first gallium nitride layer in a reaction furnace;
raising the temperature in the reaction furnace to the preset temperature;
and introducing the oxygen-containing gas or the oxygen-containing gas premixed gas into the reaction furnace.
In an optional embodiment, the oxygen-containing gas and the oxygen-containing gas premixed gas are introduced into the reaction furnace under the drive of a carrier gas; the method also comprises the following steps after the oxygen-containing gas is introduced into the reaction furnace:
stopping introducing the oxygen-containing gas or the oxygen-containing gas premixed gas into the reaction furnace;
and continuously introducing the carrier gas into the reaction furnace.
In the growth process of the second gallium nitride layer, the growth quality of the second gallium nitride layer can be reduced, the doping amount can be increased and corresponding accessories can be damaged even if the oxygen-containing gas exists; in the above embodiment, after the introduction of the oxygen-containing gas into the reaction furnace is stopped, the carrier gas is continuously introduced into the reaction furnace for a period of time to purge the remaining oxygen-containing gas, so that the oxygen-containing gas can be completely discharged from the reaction furnace before the second gallium nitride layer is formed, thereby avoiding the influence of the oxygen-containing gas on the second gallium nitride layer and ensuring the quality of the second gallium nitride layer.
In an alternative embodiment, the time for stopping the introduction of the oxygen-containing gas into the reaction furnace or continuing the introduction of the carrier gas into the reaction furnace thereafter includes 0 minute to 180 minutes.
In an alternative embodiment, the volume percentage of the oxygen-containing gas or the oxygen-containing gas premixed gas is 0.01-100%, and the flow rate of the oxygen-containing gas or the oxygen-containing gas premixed gas is 0.1-100 sccm.
In an alternative embodiment, the carrier gas comprises at least one of hydrogen, nitrogen, argon or helium.
In an alternative embodiment, the oxygen-containing gas premix comprises an oxygen-containing gas comprising at least one of oxygen or water vapor and a premix gas comprising at least one of hydrogen, nitrogen, or helium.
In an optional embodiment, the forming the second gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer includes the following steps:
forming a buffer gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer;
and forming a target gallium nitride layer on the surface of the buffer gallium nitride layer.
In an optional embodiment, the growth rate of the buffer gallium nitride layer is lower than the growth rate of the target gallium nitride layer, or the growth temperature of the buffer gallium nitride layer is lower than the growth temperature of the target gallium nitride layer, or the growth pressure of the buffer gallium nitride layer is lower than the growth pressure of the target gallium nitride layer.
Drawings
FIG. 1 is a flow chart of a method for fabricating a self-supporting gallium nitride layer provided in one embodiment of the present invention;
fig. 2 is a schematic cross-sectional structure view of a structure obtained after a substrate is provided in the method for manufacturing a self-supporting gallium nitride layer provided in one embodiment of the present invention;
fig. 3 is a schematic cross-sectional structure of a structure obtained after an aluminum nitride layer is formed on a surface of a substrate in a method for preparing a self-supporting gallium nitride layer according to an embodiment of the present invention;
fig. 4 is a schematic cross-sectional structure view of a structure obtained after a first gallium nitride layer is formed on a substrate in the method for manufacturing a self-supporting gallium nitride layer according to an embodiment of the present invention;
fig. 5 is a schematic top-view structural view of a structure obtained after a gallium oxide particle layer is formed in the method for producing a self-supporting gallium nitride layer according to an embodiment of the present invention;
fig. 6 is a schematic cross-sectional structure view of a structure obtained after a gallium oxide particle layer is formed in the method for producing a self-supporting gallium nitride layer according to an embodiment of the present invention;
fig. 7 is a schematic cross-sectional structure diagram of a structure obtained after a buffer gallium nitride layer is formed in the method for preparing a self-supporting gallium nitride layer according to an embodiment of the present invention;
fig. 8 is a schematic cross-sectional structure view of a structure obtained after a target gallium nitride layer is formed in the method for producing a self-supporting gallium nitride layer according to an embodiment of the present invention;
fig. 9 is a schematic cross-sectional structure diagram of a structure obtained after a temperature reduction treatment is performed on the self-supporting gallium nitride layer in the preparation method of the self-supporting gallium nitride layer according to an embodiment of the present invention.
Description of reference numerals:
10 substrate
11 first gallium nitride layer
12 patterned gallium layer
121 gallium oxide raised particles
122 opening pattern
13 second gallium nitride layer
131 buffer gallium nitride layer
132 target gallium nitride layer
14 self-supporting gallium nitride layer
15 AlN layer
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on methods or positional relationships shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In one embodiment, as shown in fig. 1, there is provided a method for preparing a self-supporting gallium nitride layer, comprising the steps of:
s10: providing a substrate;
s11: forming a first gallium nitride layer on the substrate;
s12: providing oxygen-containing gas or oxygen-containing gas premixed gas to the first gallium nitride layer at a preset temperature so as to form a gallium oxide particle layer on the surface of the first gallium nitride layer, wherein an opening pattern exposing the first gallium nitride layer is formed in the gallium oxide particle layer;
s13: forming a second gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer;
s14: and cooling the obtained structure to strip the second gallium nitride layer so as to obtain the self-supporting gallium nitride layer.
In the preparation method of the self-supporting gallium nitride layer in the embodiment, the oxygen-containing gas or the oxygen-containing gas premixed gas is provided for the first gallium nitride layer at the preset temperature, so that the gallium oxide particle layer with the required diameter and density distribution can be formed as required; because the faying face on second gallium nitride layer and first gallium nitride layer has a great deal of gallium oxide granule to block, lead to forming loose layer between the two, and then make contact force and area greatly reduced of the two, there is the thermal mismatch between gallium nitride and the substrate again at the in-process of cooling down, can peel off the gallium nitride layer automatically at the in-process of cooling down, in order to form from peeling off the gallium nitride layer, the required equipment input greatly reduced manufacturing cost is peeled off to laser after having removed cooling down promptly and laser, the yield of product has been improved again.
In one example, as shown in fig. 2, the substrate 10 provided in step S10 may include, but is not limited to, any one of a silicon substrate, a sapphire substrate, a glass substrate, a silicon carbide substrate, a gallium nitride substrate, or a gallium arsenide substrate, etc.
In one example, as shown in fig. 3, step S10 is followed by a step of forming an aluminum nitride layer 15 on the surface of the substrate 10, that is, a step of forming an aluminum nitride layer 15 on the surface of the substrate 10 is further included before forming the first gallium nitride layer on the substrate 10.
In one example, the first gallium nitride layer 11 may be formed using any one of a physical vapor deposition process, a chemical vapor deposition process, a Molecular Beam Epitaxy (MBE) process, a magnetron sputtering process, a Hydride Vapor Phase Epitaxy (HVPE) process, Metal Organic Chemical Vapor Deposition (MOCVD), or an ammonothermal method, or the like; when the aluminum nitride layer 15 is formed on the surface of the substrate 10, the first gallium nitride layer 11 is formed on the surface of the aluminum nitride layer 15, as shown in fig. 4.
In one example, the thickness of the first gallium nitride layer 11 may be selected according to actual needs, preferably, the thickness of the first gallium nitride layer 11 may be 50nm to 10 μm, and specifically, the thickness of the first gallium nitride layer 11 may be 50nm, 100nm, 200nm, 300nm, 400nm, 500nm, 1 μm, 2 μm, 3 μm, 4 μm or 5 μm.
In one example, the surface roughness of the first gallium nitride layer 11 is 5nm or less, preferably, the surface roughness of the first gallium nitride layer 11 is 3nm or less, and more preferably, the surface roughness of the first gallium nitride layer 11 is 1nm or less.
In an example, in step S12, a plurality of gallium oxide raised particles 121 distributed at intervals may be formed on the surface of the first gallium nitride layer 11 as the gallium oxide particle layer 12, as shown in fig. 5 and 6.
The size and distribution of gallium oxide particles can be controlled by controlling the introduction amount of oxygen-containing gas or oxygen-containing gas premixed gas, and the invention preferably controls the distance between gallium oxide particles in a nanometer to micrometer scale.
In step S12, the gallium oxide convex particles 121 may be formed directly on the surface of the first gallium oxide layer 11; the plurality of gallium oxide raised particles 121 may be randomly arranged, for example, the plurality of gallium oxide raised particles 121 may be arranged in an array or randomly arranged; the gaps between adjacent gallium oxide raised particles 121 are the opening patterns 122.
In one example, step S12 may include the steps of:
s121: placing the substrate 10 on which the first gallium nitride layer 11 is formed in a reaction furnace;
s122: raising the temperature in the reaction furnace to a preset temperature;
s123: introducing oxygen-containing gas or oxygen-containing gas premixed gas into the reaction furnace.
Specifically, the reaction furnace in step S121 may be a reaction furnace in which the first gallium nitride layer 11 is formed, that is, after step S11 is completed, the obtained structure is not required to be taken out of the reaction furnace, and after the temperature in the reaction furnace is raised to a preset temperature, an oxygen-containing gas or an oxygen-containing gas premixed gas is introduced into the reaction furnace. It is not necessary to use a reaction furnace for forming the first gallium nitride layer 11.
In one example, the oxygen-containing gas premix may include an oxygen-containing gas and a premix gas, and the oxygen-containing gas may include, but is not limited to, at least one of oxygen and water vapor, that is, the oxygen-containing gas may be oxygen, water vapor, or a mixture of oxygen and water vapor; the premix gas may include at least one of hydrogen, nitrogen, helium, or argon.
In one example, the preset temperature may be 800 ℃ to 1100 ℃; specifically, the preset temperature may be 800 ℃, 900 ℃, 100 ℃ or 1100 ℃.
In one example, the time for passing the oxygen-containing gas may be 3min (minutes) to 20min, and specifically, the time for passing the oxygen-containing gas may be 3min, 4min, 5min, 6min, 7min, 8min, 9min, 10min, 15min, or 20 min.
In an optional example, a carrier gas can be introduced into the reaction furnace while introducing the oxygen-containing gas into the reaction furnace, and the oxygen-containing gas is introduced into the reaction furnace under the driving of the carrier gas; at this time, step S123 may be followed by the following steps:
s124: stopping introducing the oxygen-containing gas into the reaction furnace;
s125: and continuously introducing carrier gas into the reaction furnace.
In another optional example, the oxygen-containing gas premixed gas can be introduced into the reaction furnace under the drive of the carrier gas; at this time, step S123 may be followed by the following steps:
s124: stopping introducing oxygen-containing gas premixed gas into the reaction furnace;
s125: and continuously introducing carrier gas into the reaction furnace.
During the growth of the second gallium nitride layer 13, the existence of the oxygen-containing gas can reduce the growth quality of the second gallium nitride layer 13, increase the doping amount and even damage the corresponding fittings; in order to avoid the reduction of the epitaxial quality of the second gallium nitride layer 13 caused by the oxygen-containing gas, the amount of the oxygen-containing gas in the growth environment of the second gallium nitride layer 13 needs to be strictly controlled, in the above embodiment, after the oxygen-containing gas is stopped being introduced into the reaction furnace, the carrier gas is continuously introduced into the reaction furnace for a period of time to purge the residual oxygen-containing gas, so that the oxygen-containing gas can be completely discharged out of the reaction furnace before the second gallium nitride layer 13 is formed, thereby avoiding the influence of the oxygen-containing gas on the second gallium nitride layer 13 and ensuring the quality of the second gallium nitride layer 13.
In one example, the carrier gas may include at least one of hydrogen, nitrogen, helium, and argon.
In one example, the time for continuously introducing the carrier gas into the reaction furnace in step S125 may be 0 minute to 180 minutes, and specifically, may be 1 minute, 50 minutes, 100 minutes, 150 minutes, and 180 minutes.
In one example, when the carrier gas and the oxygen-containing gas are simultaneously introduced into the reaction furnace, the volume percentage of the oxygen-containing gas in the mixed gas of the oxygen-containing gas and the carrier gas may be 0.01% to 100%, and specifically, the volume percentage of the oxygen-containing gas in the mixed gas of the oxygen-containing gas and the carrier gas may be 0.01%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or 100%; preferably, the volume percentage of the oxygen-containing gas in the mixed gas of the oxygen-containing gas and the carrier gas may be 0.05% to 20%.
In one example, when the oxygen-containing gas premixed gas and the carrier gas are simultaneously introduced into the reaction furnace, the volume percentage of the oxygen-containing gas premixed gas in the mixed gas of the oxygen-containing gas premixed gas and the carrier gas can be 0.01-100%; specifically, the volume percentage of the oxygen-containing gas premixed gas in the mixed gas of the oxygen-containing gas premixed gas and the carrier gas may be 0.01%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90% or 100%; preferably, the volume percentage of the oxygen-containing gas premixed gas in the mixed gas of the oxygen-containing gas premixed gas and the carrier gas can be 0.05-20%.
In one example, the flow rate of the oxygen-containing gas premixed gas can be 1sccm (standard milliliters per minute) to 100sccm, specifically, the flow rate of the oxygen-containing gas premixed gas can be 1sccm, 10sccm, 20sccm, 30sccm, 40sccm, 50sccm, 60sccm, 70sccm, 80sccm, 90sccm, or 100 sccm; preferably, the flow rate of the oxygen-containing gas premixed gas may be 2sccm to 20 sccm.
In one example, the reaction furnace may include a hydride vapor phase epitaxy reaction furnace including a gallium boat region and a substrate region, and the substrate 10 formed with the first gallium nitride layer 11 is placed in the substrate region. In step S13, hydrogen chloride gas or chlorine gas is introduced into the gallium boat region, and ammonia gas is introduced into the substrate region to form the second gallium nitride layer 13.
Specifically, hydrogen chloride gas or chlorine gas can be introduced into the gallium boat region, and then ammonia gas can be introduced into the substrate region; or introducing ammonia gas into the substrate region for a certain time, and introducing hydrogen chloride gas or chlorine gas into the gallium boat region while maintaining the ammonia gas introduced into the substrate region; specifically, ammonia gas can be introduced into the substrate region for 3min (min) to 180min, and then hydrogen chloride gas or chlorine gas can be introduced into the gallium boat region while ammonia gas is introduced into the substrate region.
In one example, step S13 may include the steps of:
s131: forming a buffer gallium nitride layer 131 in the opening pattern 122 and on the surface of the gallium oxide particle layer 12, as shown in fig. 7;
s132: a target gallium nitride layer 132 is formed on the surface of the buffer gallium nitride layer 131, as shown in fig. 8.
In one example, the growth rate of the buffer gallium nitride layer 131 formed in step S131 may be lower than the growth rate of the target gallium nitride layer 132 formed in step S132; specifically, the growth rate of the buffer gallium nitride layer 131 can be controlled by controlling the flow rate of the hydrogen chloride gas or the chlorine gas in step S131, preferably, the flow rate of the hydrogen chloride gas or the chlorine gas is less than or equal to 200 seem in step S131, and more preferably, the flow rate of the hydrogen chloride gas or the chlorine gas is less than or equal to 150 seem in the present embodiment, such as 150 seem, 100 seem, 50 seem, 40 seem, 30 seem, 20 seem, 10 seem, or the like in step S131.
In another example, the growth temperature of the buffer gallium nitride layer 131 formed in step S131 may be lower than the growth temperature of the target gallium nitride layer 132 formed in step S132, i.e., the buffer gallium nitride layer 131 formed in step S131 is a low-temperature gallium nitride layer in this example; specifically, the growth temperature of the buffer gallium nitride layer 131 may be 700 ℃ to 1080 ℃, preferably, the growth temperature of the buffer gallium nitride layer 131 may be 750 ℃ to 1000 ℃, more preferably, the growth temperature of the buffer gallium nitride layer 131 may be 780 ℃ to 900 ℃, and more preferably, the growth temperature of the buffer gallium nitride layer 131 may be 800 ℃ to 850 ℃.
In yet another example, the growth pressure of the buffer gallium nitride layer 131 formed in step S131 is lower than the growth pressure of the target gallium nitride layer 132 in step S132, i.e., the buffer gallium nitride layer 131 formed in step S131 is a low-pressure gallium nitride layer in this example; specifically, the growth pressure of the buffer gallium nitride layer 131 may be lower than the normal pressure, preferably, the growth pressure of the buffer gallium nitride layer 131 may be 1torr (torr) to 600torr, and specifically, the growth pressure of the buffer gallium nitride layer 131 may be 1torr, 50torr, 100torr, 150torr, 200torr, 250torr, 300torr, 350torr, 400torr, 500torr, 600torr, or the like.
Specifically, in step S131, when the growth of the buffer gallium nitride layer 131 is started, since the buffer gallium nitride layer 131 cannot grow on the gallium oxide bump particles 121, and only grows in the opening patterns 122, after the growth height exceeds the height of the gallium nitride bumps 121, the buffer gallium nitride layers 131 that continue to grow are combined into a whole by a lateral epitaxial growth method, so that the buffer gallium nitride layer 131 grows into a whole for the subsequent growth of the target gallium nitride layer 132.
In one example, in step S14, the structure obtained in step S13 may be cooled to room temperature by natural cooling; the structure obtained in step S13 may also be cooled to room temperature at a predetermined cooling rate, for example, the structure obtained in step S13 may be cooled to room temperature at a cooling rate of 5 ℃/min (celsius per minute) to 30 ℃/min; the structure obtained in step S13 may also be cooled to room temperature by a cooling method combining natural cooling and a preset cooling rate, for example, the structure obtained in step S13 may be cooled to a preset temperature at a preset cooling rate, and then naturally cooled to room temperature, and so on; the preset temperature can be set according to actual needs, for example, the preset temperature can be 600 ℃ to 800 ℃, and the like. The resulting freestanding gallium nitride layer 14 after the temperature reduction process is shown in fig. 9.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a self-supporting gallium nitride layer is characterized by comprising the following steps:
providing a substrate;
forming a first gallium nitride layer on the substrate;
providing oxygen-containing gas or oxygen-containing gas premixed gas to the first gallium nitride layer at a preset temperature so as to form a gallium oxide particle layer on the surface of the first gallium nitride layer, wherein an opening exposing the first gallium nitride layer is formed in the gallium oxide particle layer;
forming a second gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer;
and cooling the obtained structure to strip the second gallium nitride layer so as to obtain the self-supporting gallium nitride layer.
2. The method of fabricating a self-supporting gallium nitride layer according to claim 1, wherein: forming a plurality of gallium oxide protruding particles distributed at intervals on the surface of the first gallium nitride layer to serve as the gallium oxide particle layer.
3. The method according to claim 1, wherein the step of providing the oxygen-containing gas or the oxygen-containing gas premixed gas to the first gallium nitride layer at a predetermined temperature to form the gallium oxide particle layer on the surface of the first gallium nitride layer comprises:
placing the substrate with the first gallium nitride layer in a reaction furnace;
raising the temperature in the reaction furnace to the preset temperature;
and introducing the oxygen-containing gas or the oxygen-containing gas premixed gas into the reaction furnace.
4. A method of fabricating a self-supporting gallium nitride layer according to claim 3, characterized in that: introducing the oxygen-containing gas and the oxygen-containing gas premixed gas into the reaction furnace under the drive of a carrier gas; the method also comprises the following steps after the oxygen-containing gas or the oxygen-containing gas premixed gas is introduced into the reaction furnace:
stopping introducing the oxygen-containing gas or the oxygen-containing gas premixed gas into the reaction furnace;
and continuously introducing the carrier gas into the reaction furnace.
5. The method of fabricating a self-supporting gallium nitride layer according to claim 4, wherein: the time for continuously introducing the carrier gas into the reaction furnace after the introduction of the oxygen-containing gas or the oxygen-containing gas premixed gas into the reaction furnace is stopped comprises 0-180 minutes.
6. The method of fabricating a self-supporting gallium nitride layer according to claim 4, wherein: the volume percentage of the oxygen-containing gas or the oxygen-containing gas premixed gas is 0.01-100%, and the flow rate of the oxygen-containing gas or the oxygen-containing gas premixed gas is 1-100 sccm.
7. The method of fabricating a self-supporting gallium nitride layer according to claim 4, wherein: the carrier gas comprises at least one of hydrogen, nitrogen, argon or helium.
8. The method of fabricating a self-supporting gallium nitride layer according to claim 1, wherein: the oxygen-containing gas premix comprises an oxygen-containing gas and a premix gas, wherein the oxygen-containing gas comprises at least one of oxygen or water vapor, and the premix gas comprises at least one of hydrogen, nitrogen, helium or argon.
9. Method for the preparation of a self-supporting gallium nitride layer according to any one of claims 1to 8, characterized in that: forming the second gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer comprises the following steps:
forming a buffer gallium nitride layer in the opening pattern and on the surface of the gallium oxide particle layer;
and forming a target gallium nitride layer on the surface of the buffer gallium nitride layer.
10. The method of fabricating a self-supporting gallium nitride layer according to claim 9, wherein: the growth speed of the buffer gallium nitride layer is lower than that of the target gallium nitride layer, or the growth temperature of the buffer gallium nitride layer is lower than that of the target gallium nitride layer, or the growth pressure of the buffer gallium nitride layer is lower than that of the target gallium nitride layer.
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