CN114203535B - High-quality aluminum nitride template and preparation method and application thereof - Google Patents
High-quality aluminum nitride template and preparation method and application thereof Download PDFInfo
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 327
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000005530 etching Methods 0.000 claims abstract description 100
- 239000000758 substrate Substances 0.000 claims abstract description 26
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 60
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 27
- 238000009616 inductively coupled plasma Methods 0.000 claims description 22
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 22
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 239000000460 chlorine Substances 0.000 claims description 20
- 229910052801 chlorine Inorganic materials 0.000 claims description 20
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- -1 aluminum nitrides Chemical class 0.000 claims description 10
- 230000005693 optoelectronics Effects 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 3
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005336 cracking Methods 0.000 abstract description 7
- 229910052594 sapphire Inorganic materials 0.000 description 18
- 239000010980 sapphire Substances 0.000 description 18
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 8
- 229910010271 silicon carbide Inorganic materials 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000001039 wet etching Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000001312 dry etching Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 208000012868 Overgrowth Diseases 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001657 homoepitaxy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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Abstract
The invention discloses a high-quality aluminum nitride template and a preparation method and application thereof. The preparation method comprises the following steps: growing and forming a first aluminum nitride layer on the surface of the foreign substrate; performing first etching on a first region of the first surface of the first aluminum nitride layer to form at least one first concave part; growing a second aluminum nitride layer on the first surface of the first aluminum nitride layer; performing second etching on a second region of the second surface of the second aluminum nitride layer to form at least one second concave part, wherein the second region and the first region have no overlapping region in the orthographic projection region on the surface of the heterogeneous substrate; and growing and forming a third aluminum nitride layer on the second surface of the second aluminum nitride layer. The preparation method of the high-quality aluminum nitride template provided by the embodiment of the invention solves the cracking problem of the AlN template and greatly reduces the density of threading dislocation in the AlN template.
Description
Technical Field
The invention relates to a preparation method of an aluminum nitride template, in particular to a high-quality aluminum nitride template and a preparation method and application thereof, belonging to the technical field of semiconductors.
Background
Hexagonal wurtzite aluminum nitride (AlN) has high thermal conductivity and high transmittance for waves of 210nm or more, and thus is suitable as a substrate material for Deep Ultraviolet (DUV) Light Emitting Diodes (LEDs) and Laser Diodes (LDs). In order to obtain a high-efficiency DUV-LED, the development of an AlN template with low dislocation density is very important, and an AlN thick film is generally grown on a sapphire substrate by adopting a Hydride Vapor Phase Epitaxy (HVPE) method and is used as a template of a DUV optoelectronic device. However, the large thermal and lattice mismatch between AlN and sapphire makes it difficult to obtain high quality and crack-free AlN thick film material.
Lateral epitaxial overgrowth (ELOG) of AlN templates on patterned AlN/sapphire substrates may alleviate the above-described problems, however, the patterned substrates in the prior art have been etched once to etch AlN, which avoids cracking of the AlN template by relieving internal stress, although this approach can reduce threading dislocation density to 10 a compared to AlN templates without a patterned substrate 8 cm -2 However, the base of residual dislocation density is still large and the dislocation distribution is very non-uniform, greatly affecting the luminous efficiency and stability of the DUV optoelectronic device.
Disclosure of Invention
The invention mainly aims to provide a high-quality aluminum nitride template and a preparation method and application thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a high-quality aluminum nitride template, which comprises the following steps:
forming a first aluminum nitride layer by epitaxial growth on the surface of the heterogeneous substrate by adopting an HVPE or MOCVD mode at 1400-1600 ℃ and under the condition of 10-50torr so as to form a first epitaxial structure;
transferring the first epitaxial structure into a potassium hydroxide aqueous solution, or transferring the first epitaxial structure into an inductively coupled plasma etching device, and introducing mixed gas containing boron trichloride and chlorine into the inductively coupled plasma etching device to perform first etching on the first surface of the first aluminum nitride layer, wherein the depth of the first etching is 1-10 μm, and the width of the first etching is 2-10 μm, so as to form a first pattern with a micrometer scale;
growing a second aluminum nitride layer on the first surface of the first aluminum nitride layer in an HVPE or MOCVD mode at 1400-1600 ℃ and 10-50torr to form a second epitaxial structure;
transferring the second epitaxial structure into a potassium hydroxide aqueous solution, or transferring the second epitaxial structure into inductively coupled plasma etching equipment, and introducing mixed gas containing boron trichloride and chlorine into the inductively coupled plasma etching equipment to perform second etching on the second surface of the second aluminum nitride layer, wherein the depth of the second etching is 5-10 mu m, and the width of the second etching is 2-10 mu m, so that a second pattern with a micrometer scale is formed;
and epitaxially growing a third aluminum nitride layer on the second surface of the second aluminum nitride layer by adopting an HVPE or MOCVD mode at 1400-1600 ℃ and under the condition of 10-50 torr.
The embodiment of the invention provides an aluminum nitride template prepared by the preparation method.
The embodiment of the invention provides an optoelectronic device, which comprises an aluminum nitride template prepared by the preparation method or the aluminum nitride template.
Compared with the prior art, the invention has the advantages that:
1) The preparation method of the high-quality aluminum nitride template provided by the embodiment of the invention solves the cracking problem of the AlN template and greatly reduces the density of threading dislocation in the AlN template;
2) The preparation method of the high-quality aluminum nitride template provided by the embodiment of the invention is beneficial to greatly improving the performance of the DUV optoelectronic device.
Drawings
FIG. 1 is a schematic cross-sectional view of an unetched first layer of an AlN film/sapphire template in an exemplary embodiment of the present invention;
fig. 2a, 2b, 2c and 2d are schematic cross-sectional structures of first AlN film/sapphire templates etched to form strips, cylinders, blocks and hexagons, respectively, according to an exemplary embodiment of the present invention;
FIG. 3 is a schematic cross-sectional view of a first layer of an AlN film/sapphire template formed by etching in accordance with an exemplary embodiment of the present invention;
fig. 4 is a schematic cross-sectional structure of a second AlN film/first AlN film/sapphire template provided in an exemplary embodiment of the present invention;
FIG. 5 is a schematic cross-sectional view of a second AlN film/first AlN film/sapphire template formed by etching according to an exemplary embodiment of the present invention;
fig. 6 is a schematic cross-sectional view of a third AlN film/a second AlN film/a first AlN film/a sapphire template provided in an exemplary embodiment of the present invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The preparation method of the high-quality aluminum nitride template provided by the embodiment of the invention solves the cracking problem of the AlN template and greatly reduces the density of threading dislocation in the AlN template.
According to the preparation method of the secondary etched patterned AlN/sapphire template provided by the embodiment of the invention, the AlN film is grown on the secondary etched patterned AlN template, so that the cracking of the AlN template is avoided and the dislocation density is greatly reduced.
The embodiment of the invention provides a novel secondary etched graphical AlN substrate for growing an AlN template; the novel substrate provided by the embodiment of the invention not only can effectively solve the cracking problem of the AlN template, but also can reduce the threading dislocation density of the AlN template to 10 5 cm -2 And dislocation distribution is uniform, which is helpful to greatly improve the performance of the DUV photoelectronic device.
The embodiment of the invention provides a preparation method of a high-quality aluminum nitride template, which comprises the following steps:
forming a first aluminum nitride layer by epitaxial growth on the surface of the heterogeneous substrate by adopting an HVPE or MOCVD mode at 1400-1600 ℃ and under the condition of 10-50torr so as to form a first epitaxial structure;
transferring the first epitaxial structure into a potassium hydroxide aqueous solution, or transferring the first epitaxial structure into an inductively coupled plasma etching device, and introducing mixed gas containing boron trichloride and chlorine into the inductively coupled plasma etching device to perform first etching on the first surface of the first aluminum nitride layer, wherein the depth of the first etching is 1-10 μm, and the width of the first etching is 2-10 μm, so as to form a first pattern with a micrometer scale;
growing and epitaxially growing a second aluminum nitride layer on the first surface of the first aluminum nitride layer by adopting an HVPE or MOCVD mode at 1400-1600 ℃ and under the condition of 10-50torr so as to form a second epitaxial structure;
transferring the second epitaxial structure into a potassium hydroxide aqueous solution, or transferring the second epitaxial structure into inductively coupled plasma etching equipment, and introducing mixed gas containing boron trichloride and chlorine into the inductively coupled plasma etching equipment to perform second etching on the second surface of the second aluminum nitride layer, wherein the depth of the second etching is 5-10 mu m, and the width of the second etching is 2-10 mu m, so that a second pattern with a micrometer scale is formed;
and epitaxially growing a third aluminum nitride layer on the second surface of the second aluminum nitride layer by adopting an HVPE or MOCVD mode at 1400-1600 ℃ and under the condition of 10-50 torr.
In some more specific embodiments, the preparation method comprises: and transferring the first epitaxial structure into a potassium hydroxide aqueous solution or an inductively coupled plasma etching device, carrying out first etching on the first surface of the first aluminum nitride layer to remove all aluminum nitride in a first area of the first surface so as to form the first pattern, then transferring a second epitaxial structure into the potassium hydroxide aqueous solution or the inductively coupled plasma etching device, and carrying out second etching on the second surface of the second aluminum nitride layer so as to remove all aluminum nitride in a second area of the second surface so as to form the second pattern, wherein the second area and a forward projection area of the first area on the surface of the heterogeneous substrate have no overlapping area.
In some more specific embodiments, the first pattern includes a plurality of first aluminum nitrides spaced apart, the first aluminum nitrides have a diameter, length or width of 2-10 μm and a height of 1-10 μm, and a distance between two adjacent first aluminum nitrides is 2-10 μm.
In some more specific embodiments, the first aluminum nitride is an elongated, cylindrical, or prismatic structure.
In some more specific embodiments, the second pattern includes a plurality of spaced second aluminum nitrides, the second aluminum nitrides have a diameter, length, or width of 2-10 μm, a height of 5-10 μm, and a spacing between two adjacent second aluminum nitrides of 2-10 μm.
In some more specific embodiments, the second aluminum nitride comprises a second aluminum nitride layer, or the second aluminum nitride comprises a first aluminum nitride layer and a second aluminum nitride layer in a stacked arrangement.
In some more specific embodiments, the second aluminum nitride is an elongated, cylindrical, or prismatic structure.
In some specific embodiments, the concentration of the potassium hydroxide aqueous solution used in the first etching and the second etching is 4mol/L to 8mol/L, and the temperature is 50 ℃ to 80 ℃.
In some specific embodiments, during the first etching, the flow rates of boron trichloride and chlorine gas are respectively 25sccm and 10sccm, the pressure of the first etching is 5 to 15mTorr, the temperature is 20 to 50 ℃, during the second etching, the flow rates of boron trichloride and chlorine gas are respectively 25sccm and 10sccm, the pressure of the second etching is 5 to 15mTorr, and the temperature is 20 to 60 ℃.
In some more specific embodiments, the foreign substrate comprises a sapphire or silicon carbide substrate.
The embodiment of the invention provides an aluminum nitride template prepared by the preparation method.
In some specific embodiments, the aluminum nitride template includes a first aluminum nitride layer, a second aluminum nitride layer, and a third aluminum nitride layer, which are sequentially stacked, and a plurality of holes are formed in the aluminum nitride template.
In some more specific embodiments, the cross-sectional shape of the holes is generally triangular.
In some more specific embodiments, the first aluminum nitride layer, the second aluminum nitride layer, and the third aluminum nitride layer are all aluminum nitride crystal layers grown by HVPE or MOCVD.
In some more specific embodiments, the first aluminum nitride layer and the second aluminum nitride layer, and the third aluminum nitride layer and the second aluminum nitride layer have step surfaces therebetween.
In some more specific embodiments, the first aluminum nitride layer has a thickness of 1-10 μm.
In some more specific embodiments, the second aluminum nitride layer has a thickness of 5 to 10 μm.
In some more specific embodiments, the third aluminum nitride layer has a thickness of 10-15 μm.
The embodiment of the invention provides an optoelectronic device, which comprises an aluminum nitride template prepared by the preparation method or the aluminum nitride template.
For example, the optoelectronic device may be a deep ultraviolet light emitting diode (DUV-LED) or a Laser Diode (LD), the aluminum nitride template may be used as a substrate of the optoelectronic device, and other epitaxial structures of the optoelectronic device may be known to those skilled in the art and are not limited thereto.
The technical solution, the implementation process and the principle thereof will be further explained with reference to the drawings and the specific embodiments, unless otherwise specified, the epitaxial growth equipment used in the embodiments of the present invention may be equipment known to those skilled in the art, and other epitaxial structures of the optoelectronic device grown in the embodiments may also be epitaxial structures known to those skilled in the art, and are not specifically limited herein.
Example 1
A preparation method of a high-quality aluminum nitride template can comprise the following steps:
1) Growing a first layer of AlN film on the sapphire or silicon carbide substrate by adopting an HVPE (hydride vapor phase epitaxy) or MOCVD (metal organic chemical vapor deposition) process; the first AlN film layer has a growth temperature of 1400-1600 deg.C, a growth pressure of 10-50torr, a thickness of 1-10 μm, and a dislocation density of about 10 9 -10 10 cm -2 ；
2) Transferring the epitaxial structure obtained in the step 1) into an Inductively Coupled Plasma (ICP) etching device, introducing mixed gas of boron trichloride and chlorine, wherein the introduction flow rates of the boron trichloride and the chlorine are respectively 25sccm and 10sccm, performing first etching on the first AlN film, the pressure of the first etching is 5-15mTorr, the temperature is 20-50 ℃, the depth of the first etching is 1-10 mu m, so as to remove all AlN corresponding to a first area on the first surface of the first AlN film, and form a first micrometer-scale pattern, wherein the first pattern comprises a plurality of long-strip, cylindrical, square-shaped or hexagonal-shaped first AlN (as shown in figures 2 a-2 d) which are distributed at intervals, the pattern size (diameter, width or length) of the first AlN is 2-10 mu m, the intervals of the plurality of first AlN are 2-10 mu m, and the cross section of the etched epitaxial structure is shown in figure 3;
3) Transferring the epitaxial structure subjected to the first etching in the step 2) into HVPE or MOCVD equipment, continuously growing a second AlN film, wherein the growth temperature of the second AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 5-10 μm, the second AlN film and the first AlN film are combined by a lateral epitaxial growth method, the combined epitaxial structure is as shown in FIG. 4, in the AlN film formed by growth and combination, a step-shaped growth interface is formed between the second AlN film and the first AlN film, high-density threading dislocations are formed above the steps, and in the gaps of the steps, the dislocations are stopped at the holes, so that the threading dislocation density in the gaps of the steps is far lower than that of the rest of the first AlN film;
4) Transferring the epitaxial structure obtained in the step 3) into Inductively Coupled Plasma (ICP) etching equipment, and introducing mixed gas of boron trichloride and chlorine, wherein the introduction flow rates of the boron trichloride and the chlorine are 25sccm and 10sccm respectively; performing a second etching at room temperature, wherein the pressure of the second etching is 5-15mTorr, the temperature is 20-50 ℃, and the depth of the second etching is 5-10 μm, so as to remove AlN corresponding to a second region on the second surface of the second AlN film layer, thereby forming a second micrometer-scale pattern, the second pattern comprises a plurality of spaced-apart second AlN strips, columns, squares or hexagons (the structure can be seen in FIGS. 2 a-2 d), the pattern size (diameter, width or length) of the second AlN strips is 2-10 μm, the spacing of the second AlN strips is 2-10 μm, and the cross section of the epitaxial structure after etching is shown in FIG. 5;
5) Transferring the epitaxial structure etched for the second time in the step 4) into HVPE or MOCVD equipment, continuously growing a third layer of AlN film, wherein the growth temperature of the third layer of AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 10-15 mu m, and combining the third layer of AlN film with the second layer of AlN film and the first layer of AlN film by a lateral epitaxial growth method, thereby obtaining the final productAn AlN template having a cross-sectional structure as shown in FIG. 6 was formed, a step-like growth interface was also formed between the third AlN film and the second AlN film, and the dislocation density of the finally formed AlN template was 10 5 cm -2 。
In the AlN template after the merged growth in this example, since homoepitaxy is performed on AlN with a low dislocation density, there is no threading dislocation above the steps, and only a small amount of dislocations in the step gaps end up at the holes, so that the dislocation densities above and in the step gaps are simultaneously reduced, thereby obtaining an AlN template with a low dislocation density. In addition, due to the existence of the holes in the step gaps, the residual stress of the AlN is released, so that the AlN template cannot crack.
It should be noted that, in this embodiment, the growth temperature and pressure conditions of the first AlN film, the second AlN film, and the third AlN film are all the same, and the substrate needs to be exposed in both the first etching and the second etching, so that all the AlN grown before is removed, and if the substrate is not etched, the remaining AlN still contains higher-density dislocations, and the crystal quality of the finally obtained AlN may be reduced.
Example 2
A preparation method of a high-quality aluminum nitride template can comprise the following steps:
1) Growing a first layer of AlN film on the sapphire or silicon carbide substrate by adopting an HVPE (hydride vapor phase epitaxy) or MOCVD (metal organic chemical vapor deposition) process; the first AlN film layer has a growth temperature of 1400-1600 deg.c, a growth pressure of 10-50torr and a thickness of 1-10 microns and has a dislocation density of about 10 9 -10 10 cm -2 ；
2) Transferring the epitaxial structure obtained in the step 1) into Inductively Coupled Plasma (ICP) etching equipment, and introducing mixed gas of boron trichloride and chlorine, wherein the introduction flow rates of the boron trichloride and the chlorine are respectively 25sccm and 10sccm; carrying out first etching on the first AlN film, wherein the pressure of the first etching is 5-15mTorr, the temperature is 20-50 ℃, and the depth of the first etching is 1-10 mu m, so as to remove a part of AlN corresponding to a first area on the first surface of the first AlN film, and form a first pattern with a micrometer scale, wherein the first pattern comprises a plurality of first AlN with strip shapes, column shapes, square shapes or hexagonal shapes which are distributed at intervals, the pattern size (diameter, width or length) of the first AlN is 2-10 mu m, and the intervals of the first AlN are 2-10 mu m;
3) Transferring the epitaxial structure etched for the first time in the step 2) into HVPE or MOCVD equipment, continuously growing a second AlN film, wherein the growth temperature of the second AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 5-10 μm, and the second AlN film is combined with the first AlN film by a lateral epitaxial growth method, and in the AlN film formed after growth and combination, high-density threading dislocations are arranged above the steps, and in the gaps of the steps, the dislocations are stopped at the holes, so that the threading dislocation density in the gaps of the steps is far lower than that of the remaining first AlN film;
4) Transferring the epitaxial structure in the step 3) into Inductively Coupled Plasma (ICP) etching equipment, and introducing mixed gas of boron trichloride and chlorine, wherein the introduction flow rates of the boron trichloride and the chlorine are respectively 25sccm and 10sccm; performing a second etching at room temperature, wherein the pressure of the second etching is 5-15mTorr, the temperature is 20-50 ℃, and the depth of the second etching is 5-10 μm, so as to remove a part of AlN corresponding to a second region on the second surface of the second AlN film layer to form a second micrometer-scale pattern, the second pattern comprises a plurality of second AlN strips, columns, squares or hexagons which are distributed at intervals, the pattern size (diameter, width or length) of the second AlN strips is 2-10 μm, and the intervals of the second AlN strips are 2-10 μm;
5) Transferring the epitaxial structure etched for the second time in the step 4) into HVPE or MOCVD equipment, continuously growing a third layer of AlN film, wherein the growth temperature of the third layer of AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 10-15 mu m, merging the third layer of AlN film with the second layer of AlN film and the first layer of AlN film through a lateral epitaxial growth method to form an AlN template, and the dislocation density of the finally formed AlN template is 10 5 cm -2 。
In this embodiment, the growth temperature and pressure conditions of the first AlN film, the second AlN film, and the third AlN film are the same.
Example 3
A preparation method of a high-quality aluminum nitride template can comprise the following steps:
1) Growing a first layer of AlN film on the sapphire or silicon carbide substrate by adopting an HVPE (hydride vapor phase epitaxy) or MOCVD (metal organic chemical vapor deposition) process; the first AlN film layer has a growth temperature of 1400-1600 deg.C, a growth pressure of 10-50torr, a thickness of 1-10 μm, and a dislocation density of about 10 9 -10 10 cm -2 ；
2) Transferring the epitaxial structure obtained in the step 1) into a potassium hydroxide aqueous solution, wherein the concentration of the potassium hydroxide aqueous solution is 4-8 mol/L, the temperature is 50-80 ℃, so as to perform first wet etching on the first surface of the first AlN film, the etching depth is 1-10 mu m, the etching width is 2-10 mu m, so as to remove all AlN corresponding to the first region of the first surface of the first AlN film, and form a micron-scale first pattern, wherein the first pattern comprises a plurality of first AlN with long strips, columns, squares or hexagonal shapes distributed at intervals, the pattern size (diameter, width or length) of the first AlN is 2-10 mu m, and the intervals of the plurality of first AlN are 2-10 mu m;
3) Transferring the epitaxial structure subjected to the first etching in the step 2) into HVPE or MOCVD equipment, continuously growing a second AlN film, wherein the growth temperature of the second AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 5-10 μm, the second AlN film and the first AlN film are combined by a lateral epitaxial growth method, the combined epitaxial structure is as shown in FIG. 4, in the AlN film formed by growth and combination, a step-shaped growth interface is formed between the second AlN film and the first AlN film, high-density threading dislocations are formed above the steps, and in the gaps of the steps, the dislocations are stopped at the holes, so that the threading dislocation density in the gaps of the steps is far lower than that of the rest of the first AlN film;
4) Transferring the epitaxial structure obtained in the step 3) into a potassium hydroxide aqueous solution, wherein the concentration of the potassium hydroxide aqueous solution is 4-8 mol/L, the temperature is 50-80 ℃, so as to perform second wet etching on the second surface of the second layer of AlN film, the etching depth is 1-10 μm, the etching width is 2-10 μm, so as to remove AlN corresponding to a second region on the second surface of the second layer of AlN film, and form a micron-scale second pattern, the second pattern comprises a plurality of spaced long-strip, cylindrical, square-shaped or hexagonal-shaped second AlN (the structure of the second pattern can be seen in FIGS. 2 a-2 d), the pattern size (diameter, width or length) of the second AlN is 2-10 μm, and the spacing of the plurality of second AlN is 2-10 μm;
5) Transferring the epitaxial structure etched for the second time in the step 4) into HVPE or MOCVD equipment, continuously growing a third layer of AlN film, wherein the growth temperature of the third layer of AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 10-15 mu m, combining the third layer of AlN film with a second layer of AlN film and a first layer of AlN film through a lateral epitaxial growth method to form an AlN template, the cross-sectional structure of the AlN template is shown in figure 6, a step-shaped growth interface is also formed between the third layer of AlN film and the second layer of AlN film, and the dislocation density of the finally formed AlN template is 10 5 cm -2 。
In this embodiment, the growth temperature and pressure conditions of the first AlN film, the second AlN film, and the third AlN film are the same.
Example 4
A preparation method of a high-quality aluminum nitride template can comprise the following steps:
1) Growing a first layer of AlN film on the sapphire or silicon carbide substrate by adopting an HVPE (hydride vapor phase epitaxy) or MOCVD (metal organic chemical vapor deposition) process; the first AlN film layer has a growth temperature of 1400-1600 deg.c, a growth pressure of 10-50torr and a thickness of 1-10 microns and has a dislocation density of about 10 9 -10 10 cm -2 ；
Transferring the epitaxial structure obtained in the step 1) into a potassium hydroxide aqueous solution, wherein the concentration of the potassium hydroxide aqueous solution is 4-8 mol/L, the temperature is 50-80 ℃, so as to perform wet etching on the first surface of the first AlN film, the etching depth is 1-10 mu m, and the etching width is 2-10 mu m, so as to remove all AlN corresponding to the first area of the first surface of the first AlN film, thereby forming a first micron-scale pattern, wherein the first pattern comprises a plurality of first AlN with strip, cylinder, square or hexagonal shape distributed at intervals, the pattern size (diameter, width or length) of the first AlN is 2-10 mu m, and the intervals of the first AlN are 2-10 mu m;
3) Transferring the epitaxial structure etched for the first time in the step 2) into HVPE or MOCVD equipment, continuously growing a second AlN film, wherein the growth temperature of the second AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 5-10 μm, and the second AlN film is combined with the first AlN film by a lateral epitaxial growth method, and in the AlN film formed after growth and combination, high-density threading dislocations are arranged above the steps, and in the gaps of the steps, the dislocations are stopped at the holes, so that the threading dislocation density in the gaps of the steps is far lower than that of the remaining first AlN film;
4) Transferring the epitaxial structure in the step 3) into Inductively Coupled Plasma (ICP) etching equipment, and introducing mixed gas of boron trichloride and chlorine, wherein the introduction flow rates of the boron trichloride and the chlorine are respectively 25sccm and 10sccm; performing dry etching at room temperature, wherein the pressure of the dry etching is 5-15mTorr, the temperature is 20-50 ℃, and the depth of the second etching is 5-10 mu m, so as to remove a part of AlN corresponding to a second area on the second surface of the second AlN film layer to form a second micrometer-scale pattern, wherein the second pattern comprises a plurality of second AlN with long strips, columns, squares or hexagonal shapes which are distributed at intervals, the pattern size (diameter, width or length) of the second AlN is 2-10 mu m, and the intervals of the second AlN are 2-10 mu m;
5) Transferring the epitaxial structure after the second etching in the step 4) into HVPE or MOCVD equipment, continuously growing a third AlN film, wherein the growth temperature of the third AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 10-15 mu m, and combining the third AlN film, the second AlN film and the first AlN film through a lateral epitaxial growth method to form an AlN template, wherein the dislocation density of the finally formed AlN template is 10 5 cm -2 。
In this embodiment, the growth temperature and pressure conditions of the first AlN film, the second AlN film, and the third AlN film are the same.
Comparative example 1
A method for preparing an aluminum nitride template comprises directly growing an AlN template on a sapphire or silicon carbide substrate by HVPE (hydride vapor phase epitaxy) or MOCVD (metal organic chemical vapor deposition) process; the AlN template has a growth temperature of 1400-1600 deg.c, a growth pressure of 10-50torr and a thickness of 15-30 microns and has a dislocation density of about 10 9 -10 10 cm -2 。
Tests have shown that if an AlN template is grown directly without etching, the AlN template may crack when its thickness exceeds 30 μm.
Comparative example 2
A preparation method of an aluminum nitride template comprises the following steps:
1) Growing a first layer of AlN film on the sapphire or silicon carbide substrate by adopting an HVPE (hydride vapor phase epitaxy) or MOCVD (metal organic chemical vapor deposition) process; the first AlN film layer has a growth temperature of 1400-1600 deg.C, a growth pressure of 10-50torr, a thickness of 1-10 μm, and a dislocation density of about 10 9 -10 10 cm -2 ；
2) And 2) carrying out wet etching or dry etching on the epitaxial structure obtained in the step 1). Wet etching: and transferring the first epitaxial structure into a potassium hydroxide aqueous solution, wherein the concentration of the solution is 4-8 mol/L, the temperature is 50-80 ℃, so as to carry out first etching on the first surface of the first aluminum nitride layer, the etching depth is 1-10 mu m, and the etching width is 2-10 mu m, thereby forming a first pattern with a micron scale. Dry etching: transferring the first epitaxial structure into an Inductively Coupled Plasma (ICP) etching device, introducing mixed gas of boron trichloride and chlorine, wherein the introduction flow rates of the boron trichloride and the chlorine are respectively 25sccm and 10sccm, performing first etching on the first AlN film, the pressure of the first etching is 5-15mTorr, the temperature is 20-50 ℃, the depth of the first etching is 1-10 mu m, so as to remove AlN corresponding to a first area on the first surface of the first AlN film to form a first micrometer-sized pattern, wherein the first pattern comprises a plurality of first AlN (shown in figures 2 a-2 d) which are long strips, cylinders, squares or hexagons and are distributed at intervals, the pattern size (diameter, width or length) of the first AlN is 2-10 mu m, the interval of the first AlN is 2-10 mu m, and the cross section of the etched epitaxial structure is shown in figure 3;
3) Transferring the epitaxial structure after the first etching in the step 2) into HVPE or MOCVD equipment, continuously growing a second AlN film layer, wherein the growth temperature of the second AlN film layer is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 10-20 mu m, and combining the second AlN film layer with the first AlN film layer through a lateral epitaxial growth method to form an AlN template, wherein the dislocation density of the finally formed AlN template is 10 8 cm -2 。
Comparative example 3
A preparation method of an aluminum nitride template comprises the following steps:
1) Growing a first layer of AlN film on the sapphire or silicon carbide substrate by adopting an HVPE (hydride vapor phase epitaxy) or MOCVD (metal organic chemical vapor deposition) process; the first AlN film layer has a growth temperature of 1400-1600 deg.C, a growth pressure of 10-50torr, a thickness of 1-10 μm, and a dislocation density of about 10 9 -10 10 cm -2 ；
2) Transferring the epitaxial structure obtained in the step 1) into a potassium hydroxide aqueous solution, wherein the solution concentration is 4-8 mol/L, the temperature is 50-80 ℃, so as to perform wet etching on the first surface of the first aluminum nitride layer, the etching depth is 1-10 μm, and the etching width is 2-10 μm, so as to form a first micrometer-scale pattern, the first pattern comprises a plurality of first long-strip, cylindrical, square-block or hexagonal-shaped AlN (as shown in figures 2 a-2 d), the pattern size (diameter, width or length) of the first AlN is 2-10 μm, the interval of the first AlN is 2-10 μm, and the cross section of the epitaxial structure after etching is shown in figure 3;
3) After the first etching in the step 2)The epitaxial structure is transferred into HVPE or MOCVD equipment, a second layer of AlN film is continuously grown, the growth temperature of the second layer of AlN film is 1400-1600 ℃, the growth pressure is 10-50torr, the growth thickness is 10-20 mu m, the second layer of AlN film is combined with the first layer of AlN film through a lateral epitaxial growth method, an AlN template is formed, and the dislocation density of the finally formed AlN template is 10 8 cm -2 。
The patterned first AlN layer and the patterned second AlN layer are in strip shapes, cylindrical shapes, square shapes or hexagonal shapes, and the like, and the holes above the patterns effectively release the residual stress of the AlN template, so that the cracking problem of the AlN template is avoided.
According to the preparation method of the high-quality aluminum nitride template provided by the embodiment of the invention, when AlN grows on the first patterned AlN layer based on the first etching, dislocation in the gaps of the patterns is stopped at the holes, and threading dislocation above the patterns cannot disappear; based on the patterned template etched for the second time, dislocations above the pattern and in the pattern gaps can further disappear, and thus the AlN template with uniformly distributed dislocations and low density is obtained; the preparation method of the high-quality aluminum nitride template provided by the embodiment of the invention greatly reduces the threading dislocation density in the AlN template and is beneficial to greatly improving the performance of the DUV photoelectronic device.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (16)
1. A preparation method of a high-quality aluminum nitride template is characterized by comprising the following steps:
epitaxially growing a first aluminum nitride layer on the surface of the foreign substrate by adopting an HVPE or MOCVD mode at 1400-1600 ℃ under the condition of 10-50torr to form a first epitaxial structure;
transferring the first epitaxial structure into a potassium hydroxide aqueous solution, or transferring the first epitaxial structure into an inductively coupled plasma etching device, introducing a mixed gas containing boron trichloride and chlorine into the inductively coupled plasma etching device, and performing first etching on the first surface of the first aluminum nitride layer to remove all aluminum nitride in a first area of the first surface, wherein the depth of the first etching is 1-10 μm, and the width of the first etching is 2-10 μm, so that a first micrometer-scale pattern is formed, and the first pattern comprises a plurality of first aluminum nitrides distributed at intervals;
epitaxially growing a second aluminum nitride layer on the first surface of the first aluminum nitride layer by adopting an HVPE or MOCVD mode at 1400-1600 ℃ and 10-50torr so as to form a second epitaxial structure;
transferring the second epitaxial structure into a potassium hydroxide aqueous solution, or transferring the second epitaxial structure into an inductively coupled plasma etching device, introducing a mixed gas containing boron trichloride and chlorine into the inductively coupled plasma etching device, and performing second etching on the second surface of the second aluminum nitride layer to remove all aluminum nitride in a second area of the second surface, wherein the depth of the second etching is 5-10 μm, the width of the second etching is 2-10 μm, so as to form a second micrometer-scale pattern, the second pattern comprises a plurality of second aluminum nitrides distributed at intervals, and the orthographic projection areas of the second area and the first area on the surface of the heterogeneous substrate are not overlapped;
and epitaxially growing a third aluminum nitride layer on the second surface of the second aluminum nitride layer by adopting an HVPE or MOCVD mode at 1400-1600 ℃ and under the condition of 10-50 torr.
2. The method of claim 1, wherein: the diameter, length or width of the first aluminum nitride is 2-10 μm, the height is 1-10 μm, and the distance between two adjacent first aluminum nitrides is 2-10 μm.
3. The method of claim 2, wherein: the first aluminum nitride is in a strip, cylindrical or prismatic structure.
4. The method of claim 1, wherein: the diameter, the length or the width of the second aluminum nitride is 2-10 mu m, the height is 5-10 mu m, and the distance between two adjacent second aluminum nitrides is 2-10 mu m.
5. The method of claim 4, wherein: the second aluminum nitride includes a second aluminum nitride layer, or the second aluminum nitride includes a first aluminum nitride layer and a second aluminum nitride layer that are arranged in a stack.
6. The method of claim 4, wherein: the second aluminum nitride is of a strip-shaped, cylindrical or prismatic structure.
7. The method of claim 1, wherein: and transferring the first epitaxial structure into a potassium hydroxide aqueous solution, performing first etching on the first surface of the first aluminum nitride layer, transferring the second epitaxial structure into the potassium hydroxide aqueous solution, and performing second etching on the second surface of the second aluminum nitride layer, wherein the potassium hydroxide aqueous solution adopted in the first etching and the second etching has the concentration of 4-8 mol/L and the temperature of 50-80 ℃.
8. The method of claim 1, wherein: transferring the first epitaxial structure into inductively coupled plasma etching equipment, and performing first etching on the first surface of the first aluminum nitride layer, wherein during the first etching, the introduction flow rates of boron trichloride and chlorine are respectively 25sccm and 10sccm, the pressure of the first etching is 5-15mTorr, and the temperature is 20-50 ℃;
and transferring the second epitaxial structure into inductively coupled plasma etching equipment, and performing second etching on the second surface of the second aluminum nitride layer, wherein during the second etching, the introduction flow rates of boron trichloride and chlorine are respectively 25sccm and 10sccm, the pressure of the second etching is 5-15mTorr, and the temperature is 20-60 ℃.
9. An aluminum nitride template produced by the production method according to any one of claims 1 to 8.
10. The aluminum nitride template according to claim 9, comprising a first aluminum nitride layer, a second aluminum nitride layer and a third aluminum nitride layer which are sequentially stacked, wherein a plurality of holes are formed in the aluminum nitride template.
11. The aluminum nitride template of claim 10, wherein: the first aluminum nitride layer, the second aluminum nitride layer and the third aluminum nitride layer are all aluminum nitride crystal layers grown by HVPE or MOCVD.
12. The aluminum nitride template of claim 10, wherein: step surfaces are arranged between the first aluminum nitride layer and the second aluminum nitride layer and between the third aluminum nitride layer and the second aluminum nitride layer.
13. The aluminum nitride template of claim 10, wherein: the thickness of the first aluminum nitride layer is 1-10 μm.
14. The aluminum nitride template of claim 10, wherein: the thickness of the second aluminum nitride layer is 5-10 μm.
15. The aluminum nitride template of claim 10, wherein: the thickness of the third aluminum nitride layer is 10-15 mu m.
16. An optoelectronic device, characterized by comprising the aluminum nitride template prepared by the preparation method of any one of claims 1 to 8 or the aluminum nitride template of any one of claims 9 to 15.
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