CN109103070B - Method for preparing high-quality thick film AlN based on nano-pattern silicon substrate - Google Patents
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Abstract
The invention discloses a method for preparing high-quality thick-film AlN based on a nano-pattern silicon substrate, wherein the layered stacked AlN material obtained by the method sequentially comprises the following steps from bottom to top: the nano-pattern silicon substrate, the nano-pattern AlN nucleating layer, the high-temperature AlN transverse growth layer and the high-temperature AlN longitudinal growth layer are provided with air gaps which are periodically distributed, the depth of the air gaps in the Si substrate is 10 nm-1 mu m, the maximum width of the cross section of the air gaps is 50 nm-1 mu m, and the period of the air gaps is 100 nm-2 mu m. Compared with the existing method for growing thick-film AlN, the method has low cost, can be applied in large-scale industrialization, greatly reduces the defect density of AlN on a silicon substrate, improves the crystal quality of the subsequent device structure material, and has wide application prospect in the fields of manufacturing of UV-LED devices with vertical structures, micro-electro-mechanical systems, light emitting diodes, radio frequency filters, surface acoustic wave devices, high-frequency broadband communication and the like.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a substrate preparation process for obtaining high-quality thick-film AlN on a nano-pattern Si substrate and an epitaxial method thereof.
Background
Group III nitrides, including AlN, GaN and InN, as well as ternary and quaternary alloys thereof, have been widely used in Light Emitting Diodes (LEDs), Lasers (LDs), detectors (PDs) and the like due to their excellent optical and electrical properties, particularly their ternary alloys with a continuously tunable forbidden bandwidth from 6.1eV for AlN to 0.64eV for InN and corresponding band-edge emission wavelength coverage from 200nm for deep ultraviolet to 1.8 μm for infrared.
In the nitride heterostructure material taking sapphire, silicon carbide and silicon as substrate materials, the silicon-on-nitride heterostructure material and the device thereof have obvious advantages in the aspects of large size, low cost, compatibility with the existing Si process and the like. For example, high quality AlN thin films on silicon substrates are considered the preferred structure for fabrication of GHz-level Surface Acoustic Wave (SAW), bulk acoustic wave devices (BAW), and the use of silicon as a substrate allows for the direct utilization of existing processes, equipment and base structures of mainstream IC manufacturers, compatible with existing Si processes. And secondly, the AlGaN-based UV-LED on the silicon substrate greatly improves the light-emitting efficiency of the AlGaN-based UV-LED by manufacturing the AlGaN-based UV-LED with a vertical structure and light-emitting from the back surface by utilizing the characteristic that Si is easy to strip by a chemical corrosion method, so that the AlGaN-based UV-LED on the silicon substrate becomes one of the hot spots of international research in the nitride field.
Among group III nitrides, aluminum nitride has received attention from modern researchers due to its excellent physical properties. The aluminum nitride has physical characteristics of high hardness, high breakdown field strength, high thermal conductivity, high resistivity and the like, is a typical wide-energy-gap direct band-gap semiconductor, and the film of the aluminum nitride can be used in microelectronic instruments based on GaAs and InP and can also be used as an insulating substance to replace silicon dioxide in SiC high-power high-temperature equipment. The high-quality aluminum nitride also has the characteristics of extremely high sound transmission rate, smaller sound wave loss, large piezoelectric coupling constant, thermal expansion coefficient similar to that of Si and GaAs and the like, particularly, the AlN film with certain preferred orientation has high sound wave transmission speed, excellent piezoelectric property and high-temperature thermal stability, and is a preferred material for GHz-level Surface Acoustic Wave (SAW) and Bulk Acoustic Wave (BAW). The unique property of the aluminum nitride enables the aluminum nitride to have wide application prospect in the fields of micro-electro-mechanical systems (MEMS), Light Emitting Diodes (LED), radio frequency filters (RFT), Surface Acoustic Wave (SAW) device manufacturing, high-frequency broadband communication and the like.
Epitaxial growth of high quality thick film AlN on Si (111) substrates presents a number of problems. Firstly, because of the large lattice mismatch between the Si (111) substrate and AlN, the epitaxial material contains a large number of defects, which greatly limit the improvement of the device performance and seriously affect the reliability of the device; secondly, due to thermal mismatch, when AlN grows at high temperature, the AlN epitaxial layer can be subjected to huge tensile stress applied by the Si substrate in the growth and cooling processes, so that the epitaxial material is seriously warped and even cracked, and the process requirements are difficult to meet; third, the diffusion barrier of Al atoms on the surface is high, surface migration is difficult, and Al adsorbed atoms are difficult to incorporate into the crystal lattice at the position with the lowest energy, resulting in a large amount of threading dislocations in the AlN epitaxial layer. In the prior art, in order to epitaxially grow high-quality thick-film AlN on a Si (111) substrate and improve the performance of a device, the following methods are generally adopted internationally:
(1) pulsed laser deposition techniques such as [1] Yang, Hui, et al, CrystEngComm 15.36:7171-7176 (2013). The technology has the advantages that an AlN thin film with uniform thickness and smooth surface can be obtained on a Si (111) substrate, but the crystal quality of AlN is poor due to low growth temperature, the crystal quality of a subsequent functional layer is greatly influenced, and the performance of a device is difficult to improve.
(2) Reactive magnetron sputtering techniques, such as [2] Zhang, J.X., et al. surface and Coatings Technology 198.1-3:68-73 (2005). The technology can prepare the AlN thin film with a single crystal orientation, but the growth temperature is limited, so that the AlN thickness and the crystal quality are not ideal, the crystal quality of a subsequent functional layer is influenced, and the performance of a device is difficult to improve.
(3) Multilayer high and low temperature AlN technologies, such as [3] Tran B T, Lin K L, Sahoo K C, et al. electronic Materials Letters,10(6): 1063-. Although this technique can obtain an AlN film with a smooth surface and without cracking in a large range, the thickness of AlN is difficult to increase due to limitations of lattice mismatch and thermal mismatch, so that the crystal quality of AlN cannot meet the requirements of subsequent functional layers, and it is difficult to improve the performance of the device.
(4) Pulsed ammonia technology, such as [4] Fujikawa S, Hirayama H.applied physics express,4(6):061002 (2011). The technology can obtain the AlN thin film with higher crystal quality on the premise of smaller thickness of the epitaxial layer, but has certain difficulty in the preparation of thick film AlN, and meanwhile, the growth period is long, the growth process is complex, and the epitaxial cost is greatly increased.
(5) AlN/AlGaN superlattice technology, such as [5] Fukushima Y, Ueda T.Japan Journal of Applied Physics,49(3R):032101 (2010). The technology can grow the AlN thin film with higher crystal quality, but the growth period is long, the epitaxial process is complex, and the epitaxial cost is greatly increased.
(6) Micron-pattern Si substrate technologies such as [6] Tran B T, Hirayama H, Maeda N, et al scientific reports,5:14734 (2015). The technology can form periodic air gaps on the interface of AlN and a Si substrate through patterning of the Si substrate, the air gaps are utilized to release the stress of the AlN thin film and improve the crystal quality, but the micron periodic pattern needs an extremely thick AlN epitaxial layer to obtain a smooth surface, so the growth period is greatly increased, and the epitaxial cost is increased.
Disclosure of Invention
The invention aims to overcome the defects of the existing technology for growing high-quality thick-film AlN on Si and reduce the epitaxial cost, and provides a substrate preparation process for obtaining the high-quality thick-film AlN on a Si substrate and an epitaxial method thereof, namely, a high-quality thick-film AlN material on Si is prepared by utilizing a nano-pattern silicon substrate technology.
In order to realize the purpose, the technical scheme is as follows:
a method for preparing thick-film AlN on a Si substrate comprises the following steps:
1) growing an aluminum nitride nucleating layer on a Si substrate;
2) depositing a hard mask on the aluminum nitride nucleation layer;
3) coating nano-imprint glue with a certain thickness on the surface of the hard mask;
4) selecting a nano-imprinting template with a circular or polygonal hole array pattern, and transferring a graph on the nano-imprinting template to nano-imprinting glue, wherein in the circular or polygonal hole array of the nano-imprinting template, the aperture of a hole is 50 nm-1 μm, and the period is 100 nm-2 μm;
5) removing residual glue below the depressed area of the nanoimprint glue pattern by using oxygen plasma to expose the surface of the hard mask at the depressed area;
6) transferring the pattern on the nanoimprint glue to a hard mask through etching;
7) transferring the pattern on the hard mask to the aluminum nitride nucleating layer by etching;
8) removing the residual nano-imprinting glue on the surface;
9) transferring the patterns on the hard mask and the aluminum nitride nucleating layer to a Si substrate by etching, wherein the etching depth of the Si substrate is 10 nm-1 mu m;
10) removing the residual hard mask on the surface to obtain a nano-pattern substrate;
11) growing a high-temperature AlN transverse growth layer on the nano-pattern substrate;
12) and growing a high-temperature AlN longitudinal growth layer on the high-temperature AlN transverse growth layer.
The thick film AlN material on the nano-pattern Si substrate prepared by the method comprises a nano-pattern Si substrate, a nano-pattern AlN nucleating layer, a high-temperature AlN transverse growth layer and a high-temperature AlN longitudinal growth layer which are sequentially stacked from bottom to top, wherein air gaps which are periodically arranged are arranged in the nano-pattern Si substrate, the nano-pattern AlN nucleating layer and the high-temperature AlN transverse growth layer, the depth of each air gap in the Si substrate is 10 nm-1 mu m, the maximum width of the cross section of each air gap is 50 nm-1 mu m, and the period is 100 nm-2 mu m.
Further, in the above method, the aluminum nitride nucleation layer grown on the Si substrate in step 1) preferably has a thickness of 10nm to 2 μm. The Metal Organic Chemical Vapor Deposition (MOCVD) aluminum nitride nucleation layer is preferably adopted, the growth temperature is 900-1300 ℃, the growth pressure is 10-200mbar, and the growth can also be realized by adopting methods such as Molecular Beam Epitaxy (MBE), Hydride Vapor Phase Epitaxy (HVPE), Chemical Vapor Deposition (CVD) and the like.
The step 2) above preferably uses Plasma Enhanced Chemical Vapor Deposition (PECVD) to deposit a hard mask with a certain thickness on the nucleation layer, wherein the material of the hard mask can be silicon dioxide, silicon nitride and the like; or depositing a metal mask, such as nickel, aluminum and the like, by adopting a magnetron sputtering technology. The thickness of the hard mask is 10nm-2 mu m.
And step 3) spin-coating nano-imprint glue with a certain thickness on the surface of the hard mask by using a spin coater, wherein the thickness of the nano-imprint glue is determined according to the size characteristics of the nano-imprint template used in step 4).
The nano-imprinting template in the step 4) can be selected to have a structure and a size as required, and can be a nano-scale circular hole array, a hexagonal hole array and the like, and the aperture (the maximum width of the cross section of each hole) is less than 1 μm.
And 6) transferring the pattern on the nano-imprint glue onto the hard mask by preferably using an inductively coupled plasma etching (ICP) method until the surface of the aluminum nitride nucleation layer is etched.
And 7) transferring the pattern on the hard mask to the aluminum nitride nucleating layer by preferably using an inductively coupled plasma etching (ICP) method until the surface of the Si substrate is etched.
In the step 8), the residual nanoimprint lithography glue on the surface of the aluminum nitride can be removed by adopting an etching solution composed of concentrated sulfuric acid and hydrogen peroxide.
The step 9) preferably adopts an inductively coupled plasma etching (ICP) method.
The step 10) can remove the residual silicon dioxide hard mask on the surface of the substrate by using hydrofluoric acid.
The method for growing the aluminum nitride nucleation layer in step 1), the high-temperature AlN lateral growth layer in step 11), and the high-temperature AlN longitudinal growth layer in step 12) described above may be selected from one or more of Metal Organic Compound Vapor Deposition (MOCVD), Molecular Beam Epitaxy (MBE), Hydride Vapor Phase Epitaxy (HVPE), and Chemical Vapor Deposition (CVD).
Step 11) growth conditions of the high-temperature AlN lateral growth layer are preferably as follows: the temperature is 900-1300 ℃, the pressure is 10-200mbar, the V/III is 50-500, and the growth thickness is 10 nm-10 μm. The growth conditions of the high-temperature AlN longitudinal growth layer in the step 12) are preferably as follows: the temperature is 500-1300 ℃, the pressure is 10-100mbar, the V/III is 500-1000, and the growth thickness is 10 nm-10 μm.
The invention adopts the unique nano-pattern Si substrate to replace the traditional flat Si substrate, can effectively overcome the difficulty that the thick-film AlN cannot be extended on the Si substrate, and further can effectively improve the epitaxial thickness of the AlN, effectively reduce the defect density in the AlN epitaxial layer, greatly improve the crystal quality of the AlN and improve the crystal quality and the device performance of subsequent device materials by accurately controlling the growth conditions such as temperature, pressure, V/III and the like. The method of the invention obtains the high-quality thick-film AlN on the Si substrate, and the thickness can reach more than 4 mu m. Referring to fig. 2, the rocking curves of the X-ray diffraction (XRD) symmetric plane (002) and asymmetric plane (102) of the AlN epitaxial layer have full widths at half maximum (FWHM) of 508arcsec and 665arcsec, respectively.
Compared with the existing complicated AlN-on-Si material epitaxial technology and the micron-pattern Si substrate, the method for growing the high-quality thick-film AlN material on the nano-pattern Si substrate is simple and easy to implement, can be applied in large-scale industrialization, can obtain high crystal quality in the AlN material with a certain thickness, improves the crystal quality of subsequent device materials, improves the device performance, and has important significance for the development of UV-LED devices with vertical structures, the manufacturing of Micro Electro Mechanical Systems (MEMS), Light Emitting Diodes (LED), radio frequency filters (RFT), surface acoustic wave devices (SAW) and the like and the fields of high-frequency broadband communication by utilizing the characteristic that the silicon substrate is easy to strip, thereby having wide application prospects.
Drawings
FIG. 1 is a schematic structural diagram of a high quality thick film AlN material on a nano-pattern Si substrate according to the present invention;
FIG. 2 is a schematic flow diagram of the method of the present invention for preparing a nanopatterned Si substrate and a nanopatterned AlN nucleation layer;
in fig. 1 and 2: the device comprises a 1-Si substrate, a 2-AlN nucleating layer, a 3-air gap, a 4-high-temperature AlN transverse growth layer, a 5-high-temperature AlN longitudinal growth layer, 6-hard mask silicon dioxide, 7-nano imprinting glue and an 8-nano imprinting template.
FIG. 3 is an X-ray diffraction (XRD) pattern of an AlN epitaxial layer prepared in example 1 of the present invention; wherein (a) is an XRD symmetric plane (002) rocking curve of the AlN epitaxial layer; (b) is an XRD asymmetric surface (102) rocking curve of the AlN epitaxial layer.
Detailed Description
The invention will now be described in further detail by way of examples with reference to the accompanying drawings, without in any way limiting the scope of the invention.
As shown in fig. 1, the structure of the high quality thick film AlN material on the nano-pattern Si substrate prepared by the present invention sequentially includes, from bottom to top: the nano-pattern silicon substrate comprises a nano-pattern Si substrate 1, a nano-pattern AlN nucleating layer 2, an air gap 3, a high-temperature AlN transverse growth layer 4 and a high-temperature AlN longitudinal growth layer 5.
Example 1
The preparation process of the high-quality thick-film AlN material on the nano-pattern Si substrate is shown in figure 2 and comprises the following steps:
(1) selecting a single crystal silicon substrate 1, the crystal orientation of silicon may be silicon (111), silicon (100), silicon (110), or the like;
(2) growing an aluminum nitride nucleation layer 2 on a monocrystalline silicon substrate 1 at a growth temperature of 900-;
(3) depositing a layer of hard mask silicon dioxide 6 on the aluminum nitride nucleation layer 2 by using a Plasma Enhanced Chemical Vapor Deposition (PECVD) method, wherein the deposition temperature is 200-400 ℃, and the growth thickness is 10nm-2 mu m, as shown in (b) in FIG. 2;
(4) selecting the structure and the size of a nano-imprinting template, and using a hexagonal hole array, wherein the pattern period is 1 mu m, the pattern aperture is 600nm, and the pattern depth is 500 nm;
(5) spin-coating nano-imprint glue with a specific thickness according to the size characteristics of the nano-imprint template, wherein TU7-220 imprint glue is selected, and spin-coating the nano-imprint glue 7 on the surface of the hard mask silicon dioxide 6 by using a spin coater, as shown in FIG. 2 (c);
(6) transferring the pattern on the nano-imprinting template 8 onto the nano-imprinting glue 7 by using a nano-imprinting machine, as shown in fig. 2 (d);
(7) removing the residual nanoimprint lithography glue 7 below the pattern recessed area by inductively coupled plasma etching (ICP), wherein the etching gas is oxygen plasma and the etching time is 5-300 s, as shown in (e) in FIG. 2;
(8) transferring the pattern on the nanoimprint resist 7 to the hard mask silicon dioxide 6 by using inductively coupled plasma etching (ICP) until the pattern is etched to the surface of the aluminum nitride nucleation layer 2, wherein the etching gas is trifluoromethane and the etching time is 10-2000 s as shown in (f) in FIG. 2;
(9) transferring the pattern on the hard mask silicon dioxide 6 to the aluminum nitride nucleation layer 2 by using inductively coupled plasma etching (ICP) until the pattern is etched to the surface of the Si substrate 1, wherein the etching gas is a mixed gas of chlorine, boron trichloride and bromine gas, and the etching time is 10-2000 s as shown in (g) in FIG. 2;
(10) removing residual nanoimprint lithography glue 7 by using an etching solution composed of concentrated sulfuric acid and hydrogen peroxide, wherein the mass ratio of the concentrated sulfuric acid to the hydrogen peroxide is 6:1-3:1, the etching temperature is 80-300 ℃, and the etching time is 10-1000 s, as shown in (h) in FIG. 2;
(11) transferring the pattern on the nano-pattern aluminum nitride nucleating layer 2 to the Si substrate 1 by using inductively coupled plasma etching (ICP), wherein the etching gas is mixed gas of tetrafluoromethane and oxygen, the mass flow ratio of the tetrafluoromethane to the oxygen is 6:1-3:1, the etching time is 10s-2000s, and the etching depth is 10nm as shown in (i) in FIG. 2;
(12) removing residual silicon dioxide on the surface by hydrofluoric acid, wherein the etching time is 10s-100s, and obtaining a nano-pattern Si substrate 1 and a nano-pattern aluminum nitride nucleating layer 2 shown in (j) in figure 2;
(13) growing a high-temperature AlN transverse growth layer 4 on the nano-pattern Si substrate 1 and the nano-pattern AlN nucleating layer 2, and forming an air gap 3, wherein the growth temperature is 900-;
(14) and growing a high-temperature AlN longitudinal growth layer on the high-temperature AlN transverse growth layer 4, wherein the growth temperature is 500-1300 ℃, the growth pressure is 10-100mbar, the V/III is 500-1000, and the growth thickness is 2 mu m.
Fig. 3 is an X-ray diffraction (XRD) pattern of the AlN epitaxial layer prepared in this example, in which (a) is the XRD symmetrical plane (002) rocking curve of the AlN epitaxial layer and (b) is the XRD asymmetrical plane (102) rocking curve of the AlN epitaxial layer, it can be seen that the full width at half maximum of the rocking curve is small, indicating that the quality of the AlN thick film is excellent, and the AlN crystal quality is at the internationally best level.
Example 2
Referring to fig. 2, the method for preparing the high-quality thick-film AlN material on the nano-pattern Si substrate comprises the following steps:
(1) selecting a monocrystalline silicon substrate 1, wherein the crystal orientation of silicon can be silicon (111) and silicon (100);
(2) growing an aluminum nitride nucleating layer 2 on a monocrystalline silicon substrate 1 at the growth temperature of 900-1300 ℃, the growth pressure of 10-200mbar and the growth thickness of 200 nm;
(3) depositing a layer of hard mask silicon dioxide on the aluminum nitride nucleating layer 2 by using a Plasma Enhanced Chemical Vapor Deposition (PECVD) method, wherein the deposition temperature is 200-400 ℃, and the growth thickness is 10nm-2 mu m;
(4) selecting the structure and the size of a nano-imprinting template, and using a hexagonal hole array, wherein the pattern period is 1.4 mu m, the pattern aperture is 1 mu m, and the pattern depth is 500 nm;
(5) spin-coating nano-imprint glue with a specific thickness according to the size characteristics of the nano-imprint template, wherein TU7-220 imprint glue is selected, and spin-coating the nano-imprint glue on the surface of the Si substrate 1 by using a spin coater;
(6) transferring the pattern on the nano-imprinting template to nano-imprinting glue by using a nano-imprinting machine;
(7) removing residual nano-imprinting glue below the pattern concave area by using Inductively Coupled Plasma (ICP), wherein etching gas is oxygen plasma, and etching time is 5-300 s;
(8) transferring the pattern on the nano imprinting glue to the hard mask silicon dioxide by using inductively coupled plasma etching (ICP) until the pattern is etched to the surface of the aluminum nitride nucleating layer 2, wherein the etching gas is trifluoromethane, and the etching time is 10-2000 s;
(9) transferring the pattern on the silicon dioxide to the aluminum nitride nucleating layer 2 by using inductively coupled plasma etching (ICP) until the pattern is etched to the surface of the Si substrate 1, wherein the etching gas is a mixed gas of chlorine, boron trichloride and bromine gas, and the etching time is 10-2000 s;
(10) removing the residual nanoimprint lithography glue on the surface of the aluminum nitride by using an etching solution composed of concentrated sulfuric acid and hydrogen peroxide, wherein the mass ratio of the concentrated sulfuric acid to the hydrogen peroxide is 6:1-3:1, the etching temperature is 80-300 ℃, and the etching time is 10-1000 s;
(11) transferring the pattern on the nano-pattern aluminum nitride nucleating layer 2 onto a Si substrate 1 by using inductively coupled plasma etching (ICP), wherein the etching gas is mixed gas of tetrafluoromethane and oxygen, the mass flow ratio of the tetrafluoromethane to the oxygen is 6:1-3:1, the etching time is 10s-2000s, and the etching depth is 10nm-5 mu m;
(12) removing residual silicon dioxide on the surface by using hydrofluoric acid, wherein the etching time is 10-100 s;
(13) growing a high-temperature AlN transverse growth layer 4 on the nano-pattern Si substrate 1 and the nano-pattern AlN nucleating layer 2, and forming an air gap 3, wherein the growth temperature is 900 plus materials at 1300 ℃, the growth pressure is 10-200mbar, the V/III is 10-500, and the growth thickness is 3 mu m;
(14) and growing a high-temperature AlN longitudinal growth layer on the high-temperature AlN transverse growth layer 4, wherein the growth temperature is 500-1300 ℃, the growth pressure is 10-100mbar, the V/III is 500-1000, and the growth thickness is 1 mu m.
The above-mentioned embodiments are merely illustrative of the technical ideas and features of the present invention, and the description thereof is specific and detailed, so as to enable those skilled in the art to understand the contents of the present invention and implement the same, therefore, the scope of the present invention should not be limited by the above-mentioned embodiments, but should not be construed as being limited by the scope of the present invention. It should be noted that variations and modifications can be effected without departing from the spirit of the invention, which is within the scope of the invention as defined by the appended claims.
Claims (12)
1. A method for preparing thick-film AlN on a Si substrate comprises the following steps:
1) growing an aluminum nitride nucleation layer on a Si substrate by adopting a molecular beam epitaxy, hydride vapor phase epitaxy or chemical vapor deposition method;
2) depositing a hard mask on the aluminum nitride nucleation layer;
3) coating nano-imprint glue with a certain thickness on the surface of the hard mask;
4) selecting a nano-imprinting template with a circular or polygonal hole array pattern, and transferring a pattern on the nano-imprinting template to nano-imprinting glue, wherein in the circular or polygonal hole array of the nano-imprinting template, the aperture of a hole is 50 nm-1 μm, and the period is 100 nm-2 μm;
5) removing residual glue below the depressed area of the nanoimprint glue pattern by using oxygen plasma to expose the surface of the hard mask at the depressed area;
6) transferring the pattern on the nanoimprint glue to a hard mask through etching;
7) transferring the pattern on the hard mask to the aluminum nitride nucleating layer by etching;
8) removing the residual nano-imprinting glue on the surface;
9) transferring the patterns on the hard mask and the aluminum nitride nucleating layer to a Si substrate by etching, wherein the etching depth of the Si substrate is 10 nm-1 mu m;
10) removing the residual hard mask on the surface to obtain a nano-pattern substrate;
11) growing a high-temperature AlN transverse growth layer on the nano-pattern substrate;
12) and growing a high-temperature AlN longitudinal growth layer on the high-temperature AlN transverse growth layer.
2. The method of claim 1, wherein the chemical vapor deposition in step 1) is a metal organic compound vapor deposition.
3. The method of claim 1, wherein the aluminum nitride nucleation layer grown in step 1) on the Si substrate has a thickness of 10nm to 2 μ ι η.
4. The method of claim 1, wherein step 2) deposits a hard mask on the aluminum nitride nucleation layer using plasma enhanced chemical vapor deposition, the hard mask being of a material that is silicon dioxide or silicon nitride; or a metal hard mask is deposited by adopting a magnetron sputtering technology; the thickness of the hard mask is 10nm-2 mu m.
5. The method of claim 1, wherein step 6) transfers the pattern on the nanoimprint resist to the hard mask by an inductively coupled plasma etching method until the surface of the aluminum nitride nucleation layer is etched; and 7) transferring the pattern on the hard mask to the aluminum nitride nucleating layer by using an inductively coupled plasma etching method until the surface of the Si substrate is etched.
6. The method of claim 1, wherein in the step 8), the residual nanoimprint resist on the surface of the aluminum nitride nucleation layer is removed by using an etching solution consisting of concentrated sulfuric acid and hydrogen peroxide.
7. The method of claim 1, wherein step 9) etches the Si substrate using an inductively coupled plasma etching process.
8. The method of claim 1, wherein the material of the hard mask is silicon dioxide, and wherein the residual silicon dioxide hard mask on the surface of the substrate is removed with hydrofluoric acid in step 10).
9. The method of claim 1, wherein the method of growing the high temperature AlN lateral growth layer at step 11) and the high temperature AlN longitudinal growth layer at step 12) is selected from one or more of the following methods: molecular beam epitaxy, hydride vapor phase epitaxy, and chemical vapor deposition.
10. The method according to claim 9, wherein the chemical vapor deposition method used in step 11) and step 12) is metal organic compound vapor deposition.
11. The method of claim 1, wherein the growth conditions of the high temperature AlN lateral growth layer of step 11) are: the temperature is 900-1300 ℃, the pressure is 10-200mbar, the V/III is 50-500, and the growth thickness is 10 nm-10 mu m; step 12) the growth conditions of the high-temperature AlN longitudinal growth layer are as follows: the temperature is 500-1300 ℃, the pressure is 10-100mbar, the V/III is 500-1000, and the growth thickness is 10 nm-10 mu m.
12. A thick-film AlN material on a nano-pattern Si substrate comprises a nano-pattern Si substrate, a nano-pattern AlN nucleating layer, a high-temperature AlN transverse growth layer and a high-temperature AlN longitudinal growth layer which are sequentially stacked from bottom to top, wherein air gaps which are periodically distributed are arranged in the nano-pattern Si substrate, the nano-pattern AlN nucleating layer and the high-temperature AlN transverse growth layer, the depth of each air gap in the Si substrate is 10 nm-1 mu m, the maximum width of the cross section of each air gap is 50 nm-1 mu m, and the period of each air gap is 100 nm-2 mu m.
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| CN111261759B (en) * | 2020-02-17 | 2020-12-18 | 武汉大学 | Aluminum nitride epitaxial structure and growth method thereof |
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