CN112687771A - Method for preparing AlN thin layer - Google Patents
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Abstract
The invention provides a method for preparing an aluminum nitride thin layer. The method comprises growing an aluminum nitride thin layer on a substrate, and etching the aluminum nitride thin layer to form dislocation pits. After the aluminum nitride thin layer with the etched dislocation pits grows for the second time, the dislocation generated at the bottom layer can be effectively blocked in the dislocation pits to form the aluminum nitride thin layer with low dislocation density, and the quality of the aluminum nitride thin layer is greatly improved.
Description
Technical Field
The invention relates to an epitaxial growth method for improving the quality of aluminum nitride (AlN), in particular to a method for preparing an AlN thin layer.
Background
Aluminum nitride (AlN) belongs to the third generation wide bandgap semiconductor material, and has the advantages of high forbidden bandwidth, high breakdown electric field, high heat conductivity, high electron saturation rate, high radiation resistance and the like. AlN crystals have a stable hexagonal wurtzite structure, AlN has the largest direct band gap in group III-V semiconductor materials, about 6.2 eV. The wide forbidden band of AlN enables the wavelength coverage range of the AlGaN semiconductor luminescent material to be reduced to 200nm and to extend to an ultraviolet band. For this reason, AlN is widely used for ultraviolet detectors, HEMTs, ultraviolet Light Emitting Diodes (LEDs), ultraviolet Lasers (LDs), and the like.
Although AlN has many advantages, AlGaN materials grown on this basis have wide applications. However, high quality AlN materials are very difficult to produce, requiring high temperature and high pressure equipment and precision flow control systems from the source. At present, the quality of commercial AlN crystals is not good enough, the half width of an X-ray diffractometer in the (002) direction is 200 arcsec, the half width of the X-ray diffractometer in the (102) direction is 500 arcsec, and the dislocation density is more than 109cm-2. Dislocation generated by the AlN thin film can be directly transferred into the AlGaN thin film layer, and the high-dislocation-density AlGaN thin film can influence the performance of the AlGaN device, so that the AlGaN detector, the HEMT, the LED and the LD device are further optimized. And the difference between the lattice constant of the AlN and the lattice constant of the sapphire substrate is large, so that the AlN has large lattice mismatch, cracks are easily generated on the surface of the AlN in the growth process, and the yield of subsequent devices is not influenced slightly.
Based on the reasons, the invention provides a method for improving the quality of an aluminum nitride thin layer, which can improve the crystal quality of an AlN thin film and reduce surface cracks of the AlN thin film, thereby being beneficial to improving the performances of AlN and AlGaN devices.
Disclosure of Invention
The invention aims to overcome the defects of the traditional method, improve the growth quality of AlN by modifying the surface of the substrate, thereby improving the crystal quality of the AlN thin film and simultaneously solving the problem that the surface is easy to generate cracks to a certain extent.
The invention is realized by the following modes:
a method of preparing a thin layer of aluminum nitride (AlN), comprising the steps of:
(1) pre-growing an AlN thin layer on the substrate, wherein the thickness of the AlN thin layer is 300-2000 nm;
(2) carrying out hot alkali treatment on the AlN thin layer growing on the AlN thin layer for 10-60 minutes, wherein dislocation corrosion pits are generated in a dislocation gathering area after the hot alkali treatment;
(3) corroding the AlN thin layer with the dislocation pit to carry out secondary AlN thin layer growth;
(4) the secondary-grown AlN thin layer can cover the dislocation pits, and dislocations generated on the bottom layer due to mismatch between the substrate and AlN are blocked in the dislocation pits and do not extend any more, so that the quality of the secondary-grown AlN thin layer is greatly improved.
The substrate can be one of sapphire, silicon carbide, glass and the like;
the growth reaction chamber of the pre-grown AlN thin layer is one of metal organic chemical vapor deposition equipment (MOCVD), molecular beam epitaxy equipment (MBE) and hydride vapor phase epitaxy equipment (HVPE);
the thickness of the pre-grown AlN thin layer is controlled to be 300-2000 nm, and the growth temperature is 1000-1300 ℃;
the hot alkali comprises alkaline solutions such as NaOH and KOH, and the heating temperature is 30-100 ℃;
the secondary growth AlN thin layer is carried out by adopting a mode of adjusting V/III and growth temperature, and the purpose is to better enable the secondary growth AlN thin layer to cover the dislocation pit;
the secondary growth AlN thin layer is grown in a low V/III and high-temperature growth mode at the initial stage, the low V/III is controlled to be 5-50 ℃, the high temperature is controlled to be 1200-1300 ℃, and the growth thickness of the secondary growth AlN thin layer is 300-1000 nm;
continuously growing the AlN thin layer, wherein a high V/III and high-temperature growth mode is adopted, the high V/III is controlled to be 100-1000, the high temperature is controlled to be 1100-1250 ℃, and the growth thickness of the AlN thin layer is 300-1000 nm;
the low V/III and high-temperature growth mode and the high V/III and high-temperature growth mode can be periodically and alternately grown, and the period number can be 2-100.
The invention has the following outstanding advantages:
(1) the method is easy to realize, and the process is simple and feasible;
(2) can effectively block dislocation extension of the AlN thin layer, obtain the AlN thin layer with low dislocation density, and can ensure that the dislocation density of the AlN thin layer is less than 108cm-2；
(3) The generation of the AlN thin layer cracks is mainly caused by stress concentration, the generation of the surface cracks is relieved by stress reduction, the stress is effectively reduced by utilizing secondary growth of the AlN thin layer, and the cracking condition of the AlN thin layer can be effectively improved.
Drawings
To further illustrate the present invention, the present invention is described in detail below with reference to the following schematic structural drawings and examples, which are briefly described below.
FIG. 1 is a schematic diagram of a method abstract.
Fig. 2 is a schematic diagram of growing an aluminum nitride thin layer on a substrate, 201: substrate, 202: and pre-growing a high-temperature AlN thin layer.
FIG. 3 is a schematic view of hot-alkali etching an aluminum nitride thin layer, 301: substrate, 302: pre-growing a high-temperature AlN thin layer, 303: hot alkali etched dislocation pits.
FIG. 4 is a schematic view of the growth of the aluminum nitride layer after the hot-alkali etching, 401: substrate, 402: pre-growing a high-temperature AlN thin layer, 303: hot base etched dislocation pits, 404: and growing an AlN thin layer at a high temperature for the second time.
Fig. 5 shows a schematic cross-sectional view of an aluminum nitride thin layer grown on a substrate, 501: substrate, 502: and pre-growing a high-temperature AlN thin layer 503, namely dislocation lines in the AlN thin layer.
FIG. 6 is a schematic cross-sectional view of an etch pit after hot alkali etching, 601: substrate, 602: pre-growing a high-temperature AlN thin layer, 603: dislocation lines in the AlN thin layer, 604: hot alkali etched dislocation pits.
FIG. 7 is a schematic cross-sectional view of aluminum nitride growth after hot-alkali etching, 701: substrate, 702: pre-growing a high-temperature AlN thin layer 703, dislocation lines in the AlN thin layer 704: hot base etched dislocation pits, 705: and growing an AlN thin layer at a high temperature for the second time.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, embodiments of the present invention will be described in detail below with reference to the accompanying drawings. However, it will be appreciated by those of ordinary skill in the art that numerous technical details are set forth in order to provide a better understanding of the present application in various embodiments of the present invention. However, the technical solution claimed in the present application can be implemented without these technical details and various changes and modifications based on the following embodiments. The following embodiments are divided for convenience of description, and should not constitute any limitation to the specific implementation manner of the present invention, and the embodiments may be mutually incorporated and referred to without contradiction.
Example 1:
a method of making a thin layer of aluminum nitride (AlN): the method comprises the following steps:
101: growing a 300-2000 nm AlN layer on a substrate at a high temperature, 102: taking out the substrate, carrying out thermokalite treatment on the AlN thin layer growing on the substrate for 10-60 minutes at 30-100 ℃, and 103: and (3) corroding dislocation pits by hot alkali, wherein a dislocation pit generation area is an AlN epitaxial layer dislocation gathering area, 104: and (3) continuously growing a 500-2000 nm AlN thin layer on the AlN epitaxial wafer corroded with the dislocation pit at high temperature, wherein the thickness of the AlN thin layer is 105: the AlN thin layer which continues to grow can cover the dislocation pit area, dislocation generated at the bottom layer due to mismatch between the substrate and the AlN is blocked in the dislocation pit, and a growth cavity is formed in the dislocation pit area, so that the dislocation is prevented from extending upwards, and the dislocation density is greatly reduced.
Example 2:
a method of making a thin layer of aluminum nitride (AlN): the method comprises the following steps:
1. putting a 2-inch sapphire substrate into an MOCVD reaction chamber, raising the temperature to 1100 ℃, adjusting the pressure to 50mBar, introducing hydrogen, and staying for 10min to remove pollutants on the surface of the sapphire substrate;
2. reducing the temperature to 900 ℃, adjusting the pressure to 50mBar, introducing trimethyl aluminum and ammonia gas, growing a 20nm low-temperature AlN buffer layer, and forming a nuclear island on the substrate by the low-temperature buffer layer; the low-temperature buffer layer is used for forming a nuclear island, the temperature is low, so that amorphous AlN is formed, the thickness is not too thick, and the nuclear island aggregation is facilitated;
3. raising the MOCVD temperature to 1250 ℃, keeping the pressure at 50mBar, introducing trimethylaluminum and ammonia gas, adjusting the V/III to 200 (wherein V/III is the molar flow ratio of the group V source material and the group III source material, specifically, V/III is the molar ratio of the ammonia gas and the metal source), and growing a high-temperature AlN layer with the thickness of about 500nm for 30 minutes, wherein the growth of the high-temperature AlN layer needs to be laterally combined and grown on the basis of the nucleation layer, and the higher the temperature, the lower the pressure and the more favorable the lateral combination. The thickness is controlled by the growth time, the quality of the lateral merging is improved as the thickness increases, but the time taken is increased correspondingly;
4. and taking out the 500nm AlN thin layer from the reaction chamber, putting the AlN thin layer into a 30% NaOH solution, heating to 50 ℃, carrying out hot alkali corrosion for 20min, and taking out the AlN thin layer to form a corroded dislocation pit on the surface, wherein the higher the concentration of the alkali liquor is, the higher the temperature is, the higher the corrosion speed is, but the deeper the surface dislocation pit is corroded is, and the difficulty in control is caused. On the contrary, the lower the concentration of the alkali liquor is, the lower the temperature is, the slower the corrosion rate is, and the control is easier;
5. cleaning the AlN thin layer corroded out of the dislocation pit with sulfuric acid, hydrochloric acid and water, and then putting the AlN thin layer back to the MOCVD reaction chamber for secondary growth;
6. raising the MOCVD temperature to 1250 ℃, keeping the pressure at 50mBar, introducing trimethylaluminum and ammonia gas, adjusting the V/III to 20, and growing an AlN layer with the thickness of about 300nm for 15 minutes; the growth of the AlN layer needs to be laterally combined and grown on the basis of the etch pit, and the higher the temperature is, the lower the pressure is, the more the lateral combination is facilitated;
7. reducing the MOCVD temperature to 1150 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 200, growing for 15 minutes, and growing an AlN layer with the thickness of about 250 nm;
8. repeating the step 6 and the step 7 for 4 times;
9. raising the MOCVD temperature to 1250 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 50, growing for 15 minutes, and forming a high-temperature AlN layer with the thickness of about 250 nm; the growth of the AlN layer in the step 8 is finished under the condition of low temperature (1150 ℃) in the step 7, after the growth is finished, the growth of the AlN layer with high temperature in the step 9 is finished, the AlN layer with high temperature has higher quality than the AlN layer with low temperature, and the quality of the final AlN layer can be ensured by the high-temperature AlN. In the step 6-8, high-low temperature alternative growth is adopted, because the low temperature is favorable for relieving the stress of a growth layer and is favorable for annihilation of dislocation;
10. the obtained AlN thin film material has high crystal quality and no surface cracks, and the dislocation density is 8 multiplied by 107cm-2。
In the above examples, the growth of the AlN layer in steps 6-9 is secondary growth, and the stress is effectively reduced. Since the generation of surface cracks in the AlN thin film is mainly caused by stress concentration, the reduction of stress alleviates the generation of surface cracks. Meanwhile, stress can be relieved by low-temperature growth at high and low temperatures, the generation of cracks is reduced, the crystal quality of the high-quality crystal in the step 10 is greatly influenced by two places, the first is the density of dislocation pits, in order to enable dislocations generated at the bottom layer to be annihilated as much as possible, the higher the density of the dislocation pits is, the better the density of the dislocation pits is, and meanwhile, the deeper the depth of the dislocation pits is, so that dislocations in the subsequent AlN thin film growth process can be bent and annihilated more easily. And secondly, the dislocation density can be reduced by using a high-low temperature alternate growth method, the low-temperature growth layer can block the extension of dislocation, the high-temperature layer has higher quality, and the dislocation density can be effectively reduced by using the high-low temperature alternate growth method and the high-temperature layer alternately. The quality of the aluminum nitride (AlN) thin layer prepared by the method can be greatly improved.
Example 3:
a method of making a thin layer of aluminum nitride (AlN): the method comprises the following steps:
1. putting a 2-inch sapphire substrate into an MOCVD reaction chamber, raising the temperature to 1100 ℃, adjusting the pressure to 50mBar, introducing hydrogen, and staying for 20min to remove pollutants on the surface of the sapphire substrate;
2. reducing the temperature to 1000 ℃, adjusting the pressure to 50mBar, introducing trimethylaluminum and ammonia gas, and growing a 20nm low-temperature AlN buffer layer;
3. raising the MOCVD temperature to 1200 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 200, and growing a high-temperature AlN layer with the thickness of about 1000nm for 60 minutes;
4. taking out the 1000nm AlN thin layer from the reaction chamber, putting the AlN thin layer into a 30% NaOH solution, heating to 80 ℃, carrying out hot alkali corrosion for 20min, and taking out the AlN thin layer to form a corroded dislocation pit on the surface;
5. cleaning the AlN thin layer corroded out of the dislocation pit with sulfuric acid, hydrochloric acid and water, and then putting the AlN thin layer back to the MOCVD reaction chamber for secondary growth;
6. raising the MOCVD temperature to 1350 ℃, keeping the pressure at 50mBar, introducing trimethylaluminum and ammonia gas, adjusting the V/III to 40, and growing an AlN layer with the thickness of about 500nm for 30 minutes;
7. reducing the MOCVD temperature to 1100 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, regulating the V/III to 1000, and growing an AlN layer with the thickness of about 250nm for 15 minutes;
8. repeating the step 6 and the step 7 for 3 times;
9. finally raising the MOCVD temperature to 1200 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 50, growing for 15 minutes, and forming a high-temperature AlN layer with the thickness of about 250 nm;
10. the obtained AlN thin film material has high crystal quality and no surface cracks, and the dislocation density is 5 multiplied by 107cm-2。
Example 4:
a method of making a thin layer of aluminum nitride (AlN): the method comprises the following steps:
1. putting a 2-inch sapphire substrate into an MOCVD reaction chamber, raising the temperature to 1100 ℃, adjusting the pressure to 50mBar, introducing hydrogen, and staying for 10min to remove pollutants on the surface of the sapphire substrate;
2. reducing the temperature to 800 ℃, adjusting the pressure to 50mBar, introducing trimethylaluminum and ammonia gas, and growing a 10nm low-temperature AlN buffer layer;
3. raising the MOCVD temperature to 1300 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 200, and growing a high-temperature AlN layer with the thickness of about 1000nm for 90 minutes;
4. taking out the 1000nm AlN thin layer from the reaction chamber, putting the AlN thin layer into a 20% NaOH solution, heating to 100 ℃, carrying out thermokalite corrosion for 20min, and taking out the AlN thin layer to form a corroded dislocation pit on the surface;
5. cleaning the AlN thin layer corroded out of the dislocation pit with sulfuric acid, hydrochloric acid and water, and then putting the AlN thin layer back to the MOCVD reaction chamber for secondary growth;
6. raising the MOCVD temperature to 1320 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 30, and growing an AlN layer with the thickness of about 1000nm for 60 minutes;
7. reducing the MOCVD temperature to 1200 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, regulating the V/III to 1000, and growing an AlN layer with the thickness of about 500nm for 30 minutes;
8. raising the MOCVD temperature to 1250 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 50, and growing a high-temperature AlN layer with the thickness of about 500nm for 30 minutes;
9. the obtained AlN thin film material has high crystal quality and no surface cracks, and the dislocation density is 6 multiplied by 107cm-2。
10. Preparing an ultraviolet LED on the basis, wherein the LED is manufactured into a chip with the thickness of 350 mu m multiplied by 350 mu m, 20mA of current is introduced, the working voltage is 6.0V, and the luminous brightness is 5 mW;
11. the lifetime of the ultraviolet LED device is 1 ten thousand hours.
Example 5:
a method of making a thin layer of aluminum nitride (AlN): the method comprises the following steps:
1. putting a 2-inch sapphire substrate into an MOCVD reaction chamber, raising the temperature to 1050 ℃, adjusting the pressure to 50mBar, introducing hydrogen, and staying for 20min to remove pollutants on the surface of the sapphire substrate;
2. reducing the temperature to 750 ℃, adjusting the pressure to 50mBar, introducing trimethyl aluminum and ammonia gas, and growing a 15nm low-temperature AlN buffer layer;
3. raising the MOCVD temperature to 1200 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 100, and growing a high-temperature AlN layer with the thickness of about 2000nm for 120 minutes;
4. taking out the 2000nm AlN thin layer from the reaction chamber, putting the AlN thin layer into 35% KOH solution, heating to 60 ℃, carrying out hot alkali corrosion for 30min, and taking out the AlN thin layer to form a corroded dislocation pit on the surface;
5. cleaning the AlN thin layer corroded out of the dislocation pit with sulfuric acid, hydrochloric acid and water, and then putting the AlN thin layer back to the MOCVD reaction chamber for secondary growth;
6. raising the MOCVD temperature to 1320 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 40, and growing an AlN layer with the thickness of about 500nm for 30 minutes;
7. reducing the MOCVD temperature to 1100 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, regulating the V/III to 1000, and growing an AlN layer with the thickness of about 500nm for 30 minutes;
8. repeating the step 6 and the step 7 for 3 times;
9. finally raising the MOCVD temperature to 1200 ℃, keeping the pressure at 50mBar, introducing trimethyl aluminum and ammonia gas, adjusting the V/III to 50, growing for 15 minutes, and forming a high-temperature AlN layer with the thickness of about 250 nm;
10. the obtained AlN thin film material has high crystal quality and no surface cracks, and the dislocation density is 8 multiplied by 107cm-2。
11. Preparing an ultraviolet LED on the basis, wherein the LED is manufactured into a chip with the thickness of 250 micrometers multiplied by 500 micrometers, 100mA current is introduced, the working voltage is 6.0V, and the luminous brightness is 20 mW;
the lifetime of the ultraviolet LED device is 1 ten thousand hours.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (9)
1. A method for preparing an AlN thin layer, characterized by comprising the steps of:
(1) pre-growing an AlN thin layer on a substrate;
(2) carrying out hot alkali treatment on the AlN thin layer growing on the AlN thin layer for 10-60 minutes, wherein dislocation corrosion pits are generated in a dislocation gathering area after the hot alkali treatment;
(3) corroding the AlN thin layer with the dislocation pit to perform secondary AlN thin layer growth to obtain a secondary-grown AlN thin layer;
(4) the secondarily grown AlN thin layer can cover the dislocation pits while dislocations generated at the bottom layer due to mismatch between the substrate and AlN are blocked in the dislocation pits and do not extend.
2. A method of producing an AlN thin layer according to claim 1, wherein: the substrate is one of sapphire, silicon carbide and glass substrate.
3. A method of producing an AlN thin layer according to claim 1, wherein: the growth reaction chamber of the pre-grown AlN thin layer is one of metal organic chemical vapor deposition equipment, molecular beam epitaxy equipment and hydride vapor phase epitaxy equipment.
4. A method of producing an AlN thin layer according to claim 1, wherein: the thickness of the pre-grown AlN thin layer is controlled to be 300-2000 nm, and the growth temperature is 1000-1300 ℃.
5. A method of producing an AlN thin layer according to claim 1, wherein: the hot alkali comprises NaOH and/or KOH alkaline solution, and the heating temperature is 30-100 ℃.
6. A method of producing an AlN thin layer according to claim 1, wherein: and the secondary growth of the AlN thin layer is carried out by adopting a mode of adjusting V/III and growth temperature.
7. A method of producing an AlN thin layer according to claim 6, wherein: the initial stage of secondary growth of the AlN thin layer uses a low V/III and high-temperature growth mode, the low V/III is controlled to be 5-50, the high temperature is controlled to be 1200-1300 ℃, and the growth thickness of the AlN thin layer is 300-1000 nm.
8. A method of producing an AlN thin layer according to claim 7, characterized in that: and after the initial stage of the secondary growth of the AlN thin layer, continuously growing the AlN thin layer, and adopting a high V/III and high-temperature growth mode, wherein the high V/III is controlled to be 100-1000, the high temperature is controlled to be 1100-1250 ℃, and the growth thickness of the AlN thin layer is 250-1000 nm.
9. A method of producing an AlN thin layer according to claim 8, wherein: the low V/III and high-temperature growth modes and the high V/III and high-temperature growth modes are periodically and alternately grown, and the periodicity is 2-100.
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