CN106816362B - Based on c-plane Al2O3AlN thin film of graphic substrate and preparation method thereof - Google Patents

Based on c-plane Al2O3AlN thin film of graphic substrate and preparation method thereof Download PDF

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CN106816362B
CN106816362B CN201710021288.4A CN201710021288A CN106816362B CN 106816362 B CN106816362 B CN 106816362B CN 201710021288 A CN201710021288 A CN 201710021288A CN 106816362 B CN106816362 B CN 106816362B
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许晟瑞
赵颖
杜金娟
张进成
牛牧童
林志宇
李培咸
姜腾
郝跃
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Xian University of Electronic Science and Technology
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Abstract

The invention discloses Al based on c surface2O3A polar c-plane AlN film of a pattern substrate mainly solves the problems of complex process flow, long manufacturing period and high cost in the prior art. It includes from bottom to top: 200-500um thick c-surface Al2O3A substrate layer, an AlN nucleating layer with the thickness of 10-90nm, an Al component gradient AlGaN layer with the thickness of 2000-5000nm and a polar c-surface AlN layer with the thickness of 1000-3000nm, wherein the c-surface Al2O3Substrate stripes formed by grinding diamond abrasive paper are arranged on the surface of the substrate layer so as to improve the quality of the AlN material; the Al composition of the Al composition gradient AlGaN layer is gradually changed from 0.01 to 1 so as to reduce the stress of the AlN material. The preparation process of the invention does not need photoetching, shortens the preparation period and reduces the cost, and can be used for preparing polar c-plane AlN-based ultraviolet and deep ultraviolet semiconductor devices.

Description

Based on c-plane Al2O3AlN thin film of graphic substrate and preparation method thereof
Technical Field
The invention belongs to the technical field of microelectronics, and particularly relates to a preparation method of an AlN thin film, which can be used for manufacturing polar c-surface AlN-based ultraviolet and deep ultraviolet semiconductor devices.
Technical Field
Group iii-v nitride semiconductor materials, such as AlN-based, GaN-based, InN-based, and the like, have a large difference in their forbidden bandwidths, for example, 6.2eV for AlN, 3.42eV for GaN, and 0.7eV for InN, and thus, these group iii-v compound semiconductor materials are generally used to form various heterojunction structures. In particular, InGaN material systems have enjoyed great success in blue LEDs, and akazakio, sky hao and middle village in 2014 have enjoyed the nobel prize in physics because of the great contribution in blue LEDs. In addition, the material of the AlGaN system has a large forbidden bandwidth and a small light emitting wavelength, and if the ratio of Ga to Al is adjusted, the light emitting wavelength can cover ultraviolet and deep ultraviolet. AlN is currently predominantly heteroepitaxial on sapphire substrates. But the AlN material prepared on the conventional sapphire substrate has poor crystalline quality.
In order to reduce defects, Al is formed on the c-plane2O3Growing high quality polar c-plane AlN epitaxial layers for which a number of researchers have adopted different approaches to Al2O3The effect of the substrate processing is also obvious. See, Correlation of sapphire off-cut and reduction of defect density in MOVPE growth AlN, Phys. StatusSolidiB, 253, No.5, 809-813 (2016) and High-quality AlNepitaxy on nanopatterne primers prepared by nano-imprinting, Scientific Reports,6, 35934 (2016). However, due to these Al2O3The patterned substrate is required to be subjected to a photolithography process, so that the process is complicated, the manufacturing period is long, and the cost is high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a C-plane-based Al without photoetching2O3The AlN film of the patterned substrate and the preparation method thereof are used for reducing stress, simplifying the process, shortening the manufacturing period and reducing the cost.
To achieve the above object, the present invention is based on c-plane Al2O3The AlN film of the pattern substrate comprises the following components from bottom to top: c surface Al2O3Substrate layer, AlN nucleation layer, AlGaN layer and c face AlN layer, its characterized in that:
c surface Al2O3The surface of the substrate layer is provided with substrate stripes formed by grinding diamond abrasive paper so as to improve the quality of the AlN material,
the AlGaN layer adopts an Al component gradient AlGaN layer with the Al component gradually changing from 0.01 to 1 so as to reduce the stress of the AlN material.
Furthermore, the thickness of the AlN nucleating layer is 10-90 nm.
Furthermore, the thickness of the gradient AlGaN layer is 2000-5000 nm.
Furthermore, the thickness of the AlN layer on the c surface is 1000-3000 nm.
To achieve the above object, the present invention is based on c-plane Al2O3The preparation method of the AlN thin film of the pattern substrate comprises the following steps:
(1) substrate polishing
Mixing the c surface Al2O3Placing the substrate horizontally, placing diamond abrasive paper on the surface of the substrate, and applying 3-9 newton force on the diamond abrasive paper to the c-plane Al2O3Parallel polishing is carried out on the substrate to obtain a polished substrate parallel to Al2O3Stripe pattern of reference edge of substrate or perpendicular to Al2O3A stripe pattern of a reference edge of the substrate;
(2) substrate cleaning
Polishing the c surface Al2O3The substrate is firstly placed in HF acid or HCl acid for ultrasonic cleaning for 5-10min, then placed in acetone solution for ultrasonic cleaning for 5-10min, then absolute ethyl alcohol solution is used for ultrasonic cleaning for 5-10min, deionized water is used for ultrasonic cleaning for 5-10min, and finally nitrogen is used for blow-drying;
(3) thermal treatment
Cleaning the c surface Al2O3Placing the substrate in MOCVD reaction chamber, and vacuumizing to make the pressure in the reaction chamber less than 2X 10-2Torr; introducing mixed gas of hydrogen and ammonia gas into the reaction chamber, heating the substrate to the temperature of 900-1200 ℃ under the condition that the pressure of the MOCVD reaction chamber reaches 20-760Torr, and keeping the temperature for 5-10min to finish the heat treatment of the substrate;
(4) epitaxial AlN layer
(4a) C-plane Al after heat treatment2O3Growing an AlN nucleating layer with the thickness of 10-90nm on the substrate by adopting a Metal Organic Chemical Vapor Deposition (MOCVD) process;
(4b) growing an Al component gradient AlGaN layer with the thickness of 2000-5000nm on the AlN nucleating layer by adopting an MOCVD process, wherein the growth temperature is 950-1100 ℃;
(4c) and growing an AlN layer with the thickness of 1000-3000nm on the AlGaN layer with the gradually changed Al component by adopting an MOCVD process.
The invention has the following advantages:
1. the invention adopts diamond sand paper on the surface C of Al2O3The pattern substrate is prepared by grinding stripe patterns in the direction parallel to the reference edge or in the direction vertical to the reference edge, so that the material quality is improved, the process flow is simplified, the manufacturing period is shortened, and the cost is saved.
2. The invention adopts the gradually-changed AlGaN layer with the continuously-improved Al component, thereby greatly reducing the material stress.
The technical solution of the present invention can be further illustrated by the following figures and examples.
Drawings
FIG. 1 is a schematic cross-sectional view of a polar c-plane AlN thin film according to the present invention;
FIG. 2 shows the surface Al of FIG. 1 which has been sanded with diamond paper2O3A cross-sectional view of the patterned substrate. (ii) a
FIG. 3 is a flow chart of the present invention for fabricating a polar c-plane AlN thin film.
Detailed Description
The invention is described in further detail below with reference to the attached drawing figures:
referring to fig. 1, the polar c-plane AlN film of the present invention includes: c surface Al2O3The device comprises a substrate layer, an AlN nucleating layer, a gradient AlGaN layer and a c-plane AlN layer.
The c-face Al2O3A substrate layer having a surface provided with substrate stripes formed by diamond sanding, the substrate stripes being parallel to Al as shown in FIG. 22O3Reference edge of substratePattern of or perpendicular to Al2O3A pattern of a reference edge of the substrate for improving the quality of the AlN material;
the AlN nucleating layer is positioned on the c-plane Al2O3The thickness of the substrate layer is 10-90 nm;
the gradient AlGaN layer: the Al component is gradually changed from 0.01 to 1 on the AlN nucleating layer to reduce the stress of the material, and the thickness of the gradually changed AlGaN layer is 2000-5000 nm;
the c-surface AlN layer is positioned on the gradient AlGaN layer, and the thickness of the c-surface AlN layer is 1000-3000 nm.
Referring to fig. 3, three examples of preparing a polar c-plane AlN film are presented.
Example 1 c-plane based Al with a 50nm AlN nucleation layer thickness, 2500nm graded AlGaN layer thickness and 1500nm c-plane AlN layer thickness was prepared2O3And patterning the AlN thin film of the substrate.
Step 1, for c-surface Al2O3The substrate is ground.
Mixing the c surface Al2O3The substrate was placed horizontally, a diamond abrasive paper having a particle diameter of 6 μm was placed on the surface of the substrate, and a force of 6N was applied to the diamond abrasive paper so that the abrasive paper was parallel to Al2O3Polishing the substrate at the reference edge of the substrate, and polishing Al on the substrate2O3The substrate is milled with a pattern of stripes as shown in figure 2.
Step 2, the grinded Al is treated2O3The substrate is cleaned.
Will grind the good Al2O3The substrate is firstly placed in HF acid for ultrasonic cleaning for 7min, then placed in acetone solution for ultrasonic cleaning for 7min, then absolute ethyl alcohol solution is used for ultrasonic cleaning for 7min, finally deionized water is used for ultrasonic cleaning for 7min, and then nitrogen is used for drying.
And 3, carrying out heat treatment on the substrate.
Mixing the c surface Al2O3Placing the substrate in MOCVD reaction chamber, and vacuumizing to make the pressure in the reaction chamber less than 2X 10-2Torr, then introducing a mixed gas of hydrogen and ammonia gas into the reaction chamberThe substrate was heated to 1100 ℃ for 8min while maintaining a pressure of 40Torr in the reaction chamber.
And 4, growing an AlN nucleating layer with the thickness of 50 nm.
The temperature of the substrate after the heat treatment is reduced to 960 ℃, an aluminum source with the flow rate of 20 mu mol/min, hydrogen with the flow rate of 1200sccm and ammonia with the flow rate of 4000sccm are simultaneously introduced into the reaction chamber, and an AlN nucleating layer with the thickness of 50nm is grown under the condition that the pressure is kept at 40 Torr.
And 5, growing a gradient AlGaN layer with the thickness of 2500nm on the AlN nucleating layer.
And raising the temperature of the substrate on which the AlN nucleating layer grows to 1000 ℃, adjusting the flow rates of the aluminum source and the gallium source to gradually increase the Al component from 0.01 to 1, and growing a gradient AlGaN layer with the thickness of 2500nm on the AlN nucleating layer.
And 6, growing a 1500nm thick polar c-plane AlN layer.
The temperature of the substrate on which the graded AlGaN layer had been grown was maintained at 1000 ℃, and an aluminum source with a flow rate of 30. mu. mol/min, a hydrogen gas with a flow rate of 1200sccm, and an ammonia gas with a flow rate of 4000sccm were simultaneously introduced into the reaction chamber, and an AlN layer with a thickness of 1500nm was grown under a condition in which the pressure was maintained at 40 Torr.
And 7, taking the polar c-plane AlN material grown through the process out of the MOCVD reaction chamber, and finishing the preparation of the c-plane AlN thin film.
Example 2 c-plane based Al with a 30nm AlN nucleation layer thickness, a 2000nm graded AlGaN layer thickness and a 1000nm c-plane AlN layer thickness was prepared2O3And patterning the AlN thin film of the substrate.
Step one, carrying out treatment on c-surface Al2O3The substrate is ground.
Mixing the c surface Al2O3The substrate was placed horizontally, the diamond abrasive paper having a particle diameter of 1 μm was placed on the surface of the substrate, and a force of 3N was applied to the diamond abrasive paper so that the abrasive paper was perpendicular to Al2O3Polishing the substrate at the reference edge of the substrate, and polishing Al on the substrate2O3The substrate is milled with a pattern of stripes as shown in figure 2.
Step two, grinding oppositelyPrepared Al2O3The substrate is cleaned.
Will grind the good Al2O3The substrate is firstly placed in HF acid for ultrasonic cleaning for 5min, then placed in acetone solution for ultrasonic cleaning for 5min, then absolute ethyl alcohol solution is used for ultrasonic cleaning for 5min, finally deionized water is used for ultrasonic cleaning for 5min, and then nitrogen is used for drying.
And step three, carrying out heat treatment on the substrate.
Mixing the c surface Al2O3Placing the substrate in MOCVD reaction chamber, and vacuumizing to make the pressure in the reaction chamber less than 2X 10-2And then introducing a mixed gas of hydrogen and ammonia gas into the reaction chamber to make the pressure in the reaction chamber 20Torr, heating the substrate to 1000 ℃ and carrying out heat treatment on the substrate for 5 min.
And step four, growing an AlN nucleating layer with the thickness of 30 nm.
And reducing the temperature of the substrate after the heat treatment to 900 ℃, simultaneously introducing an aluminum source with the flow rate of 10 mu mol/min, hydrogen with the flow rate of 1200sccm and ammonia with the flow rate of 3000sccm into the reaction chamber, and growing the AlN nucleating layer with the thickness of 30nm under the condition of keeping the pressure of 20 Torr.
And step five, growing a gradient AlGaN layer with the thickness of 2000nm on the AlN nucleating layer.
And raising the temperature of the substrate on which the AlN nucleating layer grows to 950 ℃, and simultaneously adjusting the flow of an aluminum source and a gallium source to grow a gradually-changed AlGaN layer with Al components gradually increased from 0.01 to 1 and the thickness of 2000 nm.
And step six, growing a 1000nm thick polar c-plane AlN layer.
The temperature of the substrate on which the graded AlGaN layer had been grown was maintained at 950 ℃, and an aluminum source with a flow rate of 15. mu. mol/min, a hydrogen gas with a flow rate of 1200sccm, and an ammonia gas with a flow rate of 4000sccm were simultaneously introduced into the reaction chamber, and an AlN layer with a thickness of 1000nm was grown under a condition in which the pressure was maintained at 20 Torr.
And step seven, taking the polar c-plane AlN material grown through the process out of the MOCVD reaction chamber, and finishing the preparation of the c-plane AlN thin film.
EXAMPLE 3 preparation of AlNThe thickness of the nuclear layer is 90nm, the thickness of the gradient AlGaN layer is 5000nm, and the thickness of the c-surface AlN layer is 3000nm2O3And patterning the AlN thin film of the substrate.
Step A, Al on the c surface2O3The substrate was placed horizontally, a diamond sandpaper having a particle diameter of 9 μm was placed on the surface of the substrate, and a force of 9N was applied to the diamond sandpaper so that the sandpaper was parallel to Al2O3Polishing the substrate at the reference edge of the substrate, and polishing Al on the substrate2O3The substrate is milled with a pattern of stripes as shown in figure 2.
Step B, grinding the Al2O3The substrate is firstly put into HF acid for ultrasonic cleaning for 10min, then put into acetone solution for ultrasonic cleaning for 10min, then the substrate is also subjected to ultrasonic cleaning for 10min by using absolute ethyl alcohol solution, finally the substrate is subjected to ultrasonic cleaning for 10min by using deionized water, and then the substrate is dried by using nitrogen.
Step C, Al of the C surface2O3Placing the substrate in MOCVD reaction chamber, and vacuumizing to make the pressure in the reaction chamber less than 2X 10-2And then introducing a mixed gas of hydrogen and ammonia gas into the reaction chamber to make the pressure in the reaction chamber 760Torr, heating the substrate to 1200 ℃, and carrying out heat treatment on the substrate for 10 min.
And D, reducing the temperature of the substrate after heat treatment to 1000 ℃, simultaneously introducing an aluminum source with the flow rate of 50 mu mol/min, hydrogen with the flow rate of 1200sccm and ammonia with the flow rate of 4000sccm into the reaction chamber, and growing an AlN nucleating layer with the thickness of 90nm under the condition of keeping the pressure of 760 Torr.
And E, raising the temperature of the substrate on which the AlN nucleating layer grows to 1100 ℃, adjusting the flow of an aluminum source and a gallium source, and growing the gradient AlGaN layer with the thickness of 5000nm, wherein the Al component is gradually increased from 0.01 to 1.
And step F, keeping the temperature of the substrate on which the gradient AlGaN layer grows at 1100 ℃, simultaneously introducing an aluminum source with the flow rate of 100 mu mol/min, hydrogen with the flow rate of 1200sccm and ammonia with the flow rate of 5000sccm into the reaction chamber, and growing the c-plane AlN layer with the thickness of 3000nm under the condition of keeping the pressure of 760 Torr.
And G, taking the polar c-plane AlN material grown through the process out of the MOCVD reaction chamber, and finishing the preparation of the c-plane AlN thin film.
The foregoing description is only three specific examples of the present invention and should not be construed as limiting the invention in any way, and it will be apparent to those skilled in the art that various modifications and variations in form and detail can be made without departing from the principle and structure of the invention, but these modifications and variations will still fall within the scope of the appended claims.

Claims (8)

1. Al based on c surface2O3The polarity c face AlN film of figure substrate includes from bottom to top: c surface Al2O3Substrate layer, AlN nucleation layer, AlGaN layer and c face AlN layer, its characterized in that:
c surface Al2O3The surface of the substrate layer is provided with substrate stripes formed by grinding diamond abrasive paper so as to improve the quality of the AlN material,
the AlGaN layer adopts an Al component gradient AlGaN layer with the Al component gradually changing from 0.01 to 1 so as to reduce the stress of the AlN material.
2. The film of claim 1, wherein: the AlN nucleating layer is 10-90nm thick.
3. The film of claim 1, wherein: the thickness of the gradient AlGaN layer of the Al component from 0.01 to 1 is 2000-5000 nm.
4. The film of claim 1, wherein: the thickness of the c-surface AlN layer is 1000-3000 nm.
5. Al based on c surface2O3The preparation method of the polar c-surface AlN thin film of the graphic substrate comprises the following steps:
(1) substrate polishing
Mixing the c surface Al2O3The substrate is horizontally arranged, and the diamond is placedPlacing stone sand paper on the surface of the substrate, and applying 3-9 newton force on the diamond sand paper to the c-plane Al2O3Parallel polishing is carried out on the substrate to obtain a polished substrate parallel to Al2O3Stripe pattern of reference edge of substrate or perpendicular to Al2O3A stripe pattern of a reference edge of the substrate;
(2) substrate cleaning
Polishing the c surface Al2O3The substrate is firstly placed in HF acid or HCl acid for ultrasonic cleaning for 5-10min, then placed in acetone solution for ultrasonic cleaning for 5-10min, then absolute ethyl alcohol solution is used for ultrasonic cleaning for 5-10min, deionized water is used for ultrasonic cleaning for 5-10min, and finally nitrogen is used for blow-drying;
(3) thermal treatment
Cleaning the c surface Al2O3Placing the substrate in MOCVD reaction chamber, and vacuumizing to make the reaction pressure less than 2 × 10-2Torr; introducing mixed gas of hydrogen and ammonia gas into the reaction chamber, heating the substrate to the temperature of 900-1200 ℃ under the condition that the pressure of the MOCVD reaction chamber reaches 20-760Torr, and keeping the temperature for 5-10min to finish the heat treatment of the substrate;
(4) epitaxial AlN layer
(4a) C-plane Al after heat treatment2O3Growing an AlN nucleating layer with the thickness of 10-90nm on the substrate by adopting a Metal Organic Chemical Vapor Deposition (MOCVD) process;
(4b) on the AlN nucleating layer, an MOCVD process is adopted, under the conditions that the pressure of a reaction chamber is 20-760Torr and the temperature is 950-1100 ℃, the flow of an aluminum source and the flow of a gallium source are continuously changed, so that the Al component is gradually changed from 0.01 to 1, and a gradually changed AlGaN layer with the thickness of 2000-5000nm is grown;
(4c) and growing a polar c-surface AlN layer with the thickness of 1000-3000nm on the AlGaN layer with the gradually changed Al component by adopting an MOCVD process.
6. The method according to claim 5, wherein the diamond coated abrasive of step (1) is coated abrasive having a particle diameter of 1 to 9 μm.
7. The method of claim 5, wherein the process conditions for growing the AlN nucleation layer in step (4a) using the MOCVD process are as follows:
the pressure in the reaction chamber is 20-760Torr,
the temperature is 900-1000 ℃,
the flow rate of the aluminum source is 10-50 mu mol/min,
the flow rate of hydrogen was 1200sccm,
the flow rate of ammonia gas is 3000-4000 sccm.
8. The method of claim 5, wherein the process conditions for growing the polar c-plane AlN layer in the step (4c) by using the MOCVD process are as follows:
the pressure in the reaction chamber is 20-760Torr,
the temperature is 950 ℃ and 1100 ℃,
the flow rate of the aluminum source is 5-100 mu mol/min,
the flow rate of ammonia gas was 2000-.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101390201A (en) * 2005-12-28 2009-03-18 日本电气株式会社 Field effect transistor, and multilayered epitaxial film for use in preparation of field effect transistor
CN101847578A (en) * 2010-04-23 2010-09-29 西安电子科技大学 Method for growing semi-polar GaN based on Al2O3 substrate with m sides
CN102119243A (en) * 2008-07-16 2011-07-06 奥斯坦多科技公司 Growth of planar non-polar {1-1 0 0} m-plane and semi-polar {1 1-2 2} gallium nitride with hydride vapor phase epitaxy (HVPE)
CN102597863A (en) * 2009-08-31 2012-07-18 高丽大学校产学协力团 Transparent structures

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8710511B2 (en) * 2011-07-29 2014-04-29 Northrop Grumman Systems Corporation AIN buffer N-polar GaN HEMT profile

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101390201A (en) * 2005-12-28 2009-03-18 日本电气株式会社 Field effect transistor, and multilayered epitaxial film for use in preparation of field effect transistor
CN102119243A (en) * 2008-07-16 2011-07-06 奥斯坦多科技公司 Growth of planar non-polar {1-1 0 0} m-plane and semi-polar {1 1-2 2} gallium nitride with hydride vapor phase epitaxy (HVPE)
CN102597863A (en) * 2009-08-31 2012-07-18 高丽大学校产学协力团 Transparent structures
CN101847578A (en) * 2010-04-23 2010-09-29 西安电子科技大学 Method for growing semi-polar GaN based on Al2O3 substrate with m sides

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