CN111048403A - Aluminum nitride film and preparation method and application thereof - Google Patents
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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 195
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 61
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 18
- 230000007547 defect Effects 0.000 abstract description 14
- 230000001276 controlling effect Effects 0.000 description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 19
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000003111 delayed effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000010897 surface acoustic wave method Methods 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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Abstract
The invention provides an aluminum nitride film and a preparation method and application thereof. The invention provides a preparation method of an aluminum nitride film, which comprises the following steps: step 1, growing a silicon nitride layer with a porous structure on a substrate; step 2, placing the silicon nitride layer into a reaction chamber of the equipment, controlling the temperature of the reaction chamber to be 600-1000 ℃ and the pressure to be 20-200mbar, and growing an aluminum nitride buffer layer on the surface of the silicon nitride layer; and 3, controlling the temperature of the reaction chamber to be 1100-1500 ℃ and the pressure to be 20-200mbar, and growing the aluminum nitride layer on the surface of the aluminum nitride buffer layer. By the preparation method provided by the invention, line defects and dislocation of the aluminum nitride in the growth process are greatly annihilated, the aluminum nitride layer with low defect concentration and high crystal quality is obtained, and the problem of mechanical damage possibly caused when the aluminum nitride layer and the substrate are mechanically stripped in the follow-up process is avoided.
Description
Technical Field
The invention relates to the technical field of light emitting diodes, in particular to an aluminum nitride film and a preparation method and application thereof.
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, have the largest direct band gap in III-V semiconductor materials, about 6.2eV, and are important blue and ultraviolet light emitting materials. The material has high thermal conductivity, high resistivity, strong breakdown field and small dielectric coefficient, and is an excellent electronic material for high-temperature, high-frequency and high-power devices. Further, AlN oriented along the c-axis has excellent piezoelectric characteristics and high-speed propagation of surface acoustic waves, and is an excellent piezoelectric material for surface acoustic wave devices. Meanwhile, AlN crystal and gallium nitride crystal have very close lattice constants and thermal expansion coefficients, and are preferred materials for epitaxially growing AlGaN photoelectric devices.
The AlN film prepared by the existing method is directly grown on a substrate, which can generate the following adverse effects: 1. lattice mismatch exists between the AlN layer and the substrate, so that stress is introduced into the AlN crystal, and a large number of cracks are generated along with the increase of the thickness of the AlN layer, so that the yield of a final product is poor; 2. in order to reduce the generation of cracks and obtain better yield, a method of reducing the thickness of the AlN layer is generally adopted, but the quality of the AlN layer is deteriorated; 3. the conventional AlN layer may be mechanically damaged when it is subsequently mechanically stripped from the substrate.
The above reasons all limit the mass production and popularization and application of the AlN film on the photoelectric device.
Disclosure of Invention
The invention provides a preparation method of an aluminum nitride film, which is used for solving the problems that the lattice mismatch exists between an aluminum nitride layer and a substrate and the mechanical damage is possibly generated during subsequent mechanical stripping caused by the existing preparation method of the aluminum nitride film.
The invention provides a preparation method of an aluminum nitride film, which comprises the following steps:
step 1, growing a silicon nitride layer with a porous structure on a substrate;
step 2, placing the silicon nitride layer into an equipment reaction chamber, controlling the temperature of the reaction chamber to be 600-1000 ℃ and the pressure to be 20-200mbar, and growing an aluminum nitride buffer layer on the surface of the silicon nitride layer;
and 3, controlling the temperature of the reaction chamber to be 1100-1500 ℃, and controlling the pressure to be 20-200mbar, and growing an aluminum nitride layer on the surface of the aluminum nitride buffer layer.
The invention provides a preparation method of an aluminum nitride film, and figure 1 is a flow schematic diagram of the preparation method of the aluminum nitride film provided by the invention, as shown in figure 1, firstly a silicon nitride layer with a porous structure grows on a substrate, secondly the silicon nitride layer is placed in an equipment reaction chamber, the temperature of the reaction chamber is controlled to be 600-1000 ℃, the pressure is 20-200mbar, an aluminum nitride buffer layer grows on the surface of the silicon nitride layer, and finally the temperature of the reaction chamber is controlled to be 1100-1500 ℃, the pressure is 20-200mbar, and an aluminum nitride layer grows on the aluminum nitride buffer layer to obtain the final aluminum nitride film.
According to the invention, firstly, a silicon nitride layer with a porous structure is added between an aluminum nitride layer and a substrate, and the surface of the substrate is patterned similarly, so that on one hand, the growth mode of aluminum nitride can be changed, the growth of aluminum nitride crystal nucleus from three-dimensional to two-dimensional is delayed, the line defect and dislocation of aluminum nitride in the growth process are greatly annihilated, and the aluminum nitride layer with low defect concentration and high crystal quality is obtained, and on the other hand, because the silicon nitride has excellent physical properties, the problem that mechanical damage is possibly generated when the aluminum nitride layer and the substrate are mechanically stripped subsequently is avoided; secondly, on the basis of the silicon nitride layer, an aluminum nitride buffer layer grows by controlling the reaction temperature to be 600-; and finally, on the basis of the aluminum nitride buffer layer, the temperature of the reaction chamber is controlled to be 1100-1500 ℃, and the pressure is controlled to be 20-200mbar, so that the aluminum atomic mobility is favorably improved, and the quality of the final aluminum nitride film can be effectively improved.
In one embodiment, the substrate is selected from one of sapphire, silicon carbide, zinc oxide, copper, and glass.
Further, in step 1, a nitrogen source and a silicon source are used as raw materials, so that a silicon nitride layer with a porous structure is grown on the surface of the substrate.
Specifically, the nitrogen source is nitrogen, and the silicon source is monocrystalline silicon.
In order to ensure that the silicon nitride layer has a porous structure, in step 1, the silicon nitride layer is grown at 25-250 ℃ by a magnetron sputtering method.
The method adopts a magnetron sputtering method to grow the silicon nitride layer, and controls the temperature within 25-250 ℃, so that the surface of the sputtered silicon nitride layer has a porous structure. Specifically, an amorphous silicon nitride layer having a sparse pore structure on the surface is obtained by the method. The applicant finds that the surface of the silicon nitride layer is more compact along with the increase of the temperature, when the temperature is controlled to be 25-250 ℃, the silicon nitride layer obtained by sputtering can meet the requirement, an amorphous silicon nitride layer with a sparse porous structure on the surface is obtained, and when the temperature is higher than 250 ℃, the surface of the silicon nitride layer is more compact, and the porous structure cannot be obtained; when the temperature is lower than 25 ℃, the uniformity of silicon nitride is poor, and clusters are easily formed.
In order to ensure the performance of the final aluminum nitride film, the nitrogen introduction amount and the growth time need to be reasonably set so as to control the thickness of the silicon nitride layer and ensure the performance of the final aluminum nitride film.
Specifically, the thickness of the silicon nitride layer is a, and a is more than or equal to 5 and less than or equal to 2000 nm.
And placing the substrate with the silicon nitride layer in an equipment reaction chamber, and sequentially growing an aluminum nitride buffer layer, a first aluminum nitride layer and a second aluminum nitride layer on the surface of the silicon nitride layer.
The skilled person can select a suitable growth apparatus according to the prior art without further limitation, for example, the apparatus may be selected from one of a metal organic chemical vapor deposition apparatus, a molecular beam epitaxy apparatus and a hydride vapor phase epitaxy apparatus.
Further, step 2 comprises: controlling the temperature of the reaction chamber at 600-.
Specifically, trimethylaluminum and ammonia gas are respectively selected as an aluminum source and a nitrogen source.
The substrate with the silicon nitride layer is placed into a reaction chamber of the equipment, the temperature is controlled to be 600-1000 ℃, the pressure is 20-200mbar, and the aluminum nitride buffer layer grows, so that the pre-reaction between sources can be weakened under the temperature and the pressure, and the influence on the subsequent aluminum nitride layer is reduced.
In addition, in order to ensure the performance of the final aluminum nitride film, the introduction amount of trimethyl aluminum and ammonia gas needs to be reasonably set, so that the thickness of the aluminum nitride buffer layer is controlled, and the performance of the final aluminum nitride film is ensured.
Specifically, the thickness of the aluminum nitride buffer layer is b, and b is more than 0 and less than or equal to 50 nm.
In the growth process, the growth time can be controlled to be 3-10min in order to improve the growth efficiency.
Further, in step 3, the temperature of the reaction chamber is controlled to be 1100-.
Specifically, trimethylaluminum and ammonia gas were continuously selected as the aluminum source and nitrogen source, respectively.
In order to make the surface of the final aluminum nitride film smoother, in step 3, growing an aluminum nitride layer on the surface of the aluminum nitride buffer layer includes: and sequentially growing a first aluminum nitride layer and a second aluminum nitride layer on the surface of the aluminum nitride buffer layer, wherein the growth rate of the first aluminum nitride layer is less than that of the second aluminum nitride layer.
Specifically, a first aluminum nitride layer is grown on the surface of the aluminum nitride buffer layer at a relatively low growth rate, and then a second aluminum nitride layer is grown on the surface of the first aluminum nitride layer at an increased growth rate.
In the growth process of the aluminum nitride layer, the aluminum nitride layer grows in stages by changing the growth rate of the aluminum nitride layer, so that the surface of the final aluminum nitride layer is smoother.
Specifically, the growth rate of the first aluminum nitride layer is 0.5-1 μm/h.
The growth rate of the second aluminum nitride layer is 1-2 mu m/h.
On the basis of setting the growth rates of the first aluminum nitride layer and the second aluminum nitride layer, the growth time can be reasonably set by a person skilled in the art, so that the thicknesses of the first aluminum nitride layer and the second aluminum nitride layer are controlled, and the performance of the final aluminum nitride layer is ensured.
Specifically, the thickness of the first aluminum nitride layer is c, and c is more than or equal to 100 and less than or equal to 800 nm;
the thickness of the second aluminum nitride layer is d, and d is more than or equal to 1000 and less than or equal to 5000 nm.
The invention provides a preparation method of an aluminum nitride film, which is characterized in that a silicon nitride layer with a porous structure is added between an aluminum nitride layer and a substrate, and the surface of the substrate is patterned similarly, so that on one hand, the growth mode of the aluminum nitride can be changed, the growth of aluminum nitride crystal nucleus from three-dimension to two-dimension is delayed, the line defect and dislocation of the aluminum nitride in the growth process are greatly annihilated, and the aluminum nitride layer with low defect concentration and high crystal quality is obtained, and on the other hand, because the silicon nitride has excellent physical property, the problem of mechanical damage possibly generated when the aluminum nitride layer and the substrate are mechanically stripped subsequently is avoided; secondly, on the basis of the silicon nitride layer, the temperature of the reaction chamber is controlled to be 600-; and finally, on the basis of the aluminum nitride buffer layer, the temperature of the reaction chamber is controlled to be 1100-1500 ℃, and the pressure is controlled to be 20-200mbar, so that the aluminum atomic mobility is favorably improved, and the quality of the final aluminum nitride film can be effectively improved.
A second aspect of the present invention provides an aluminum nitride film prepared according to any one of the above methods, and fig. 2 is a schematic structural view of the aluminum nitride film provided by the present invention, as shown in fig. 2, the aluminum nitride film sequentially includes, from bottom to top, a silicon nitride layer, an aluminum nitride buffer layer, and an aluminum nitride layer, where the silicon nitride layer has a porous structure.
According to the aluminum nitride film provided by the invention, the silicon nitride layer with the surface provided with the porous structure is added between the aluminum nitride layer and the substrate, so that on one hand, the growth mode of the aluminum nitride can be changed, the growth of aluminum nitride crystal nucleus from three-dimensional to two-dimensional is delayed, the line defect and dislocation of the aluminum nitride in the growth process are greatly eliminated, and the aluminum nitride layer with low defect concentration and high crystal quality is obtained, on the other hand, because the silicon nitride has excellent physical properties, the problem that mechanical damage is possibly generated when the aluminum nitride layer and the substrate are subsequently stripped mechanically is avoided, and the finally obtained aluminum nitride film has the advantages of stable growth, low dislocation density and the like.
In a third aspect, the invention provides an LED epitaxial structure comprising an aluminum nitride film according to the above aluminum nitride film or any one of the above preparation methods.
The person skilled in the art can grow an N-type doped layer, a quantum well light-emitting layer and a P-type doped layer on the aluminum nitride film provided by the invention in sequence according to the prior art to obtain the final LED epitaxial structure.
According to the LED epitaxial structure provided by the invention, the silicon nitride layer with the porous structure is added between the aluminum nitride layer and the substrate, the substrate surface is patterned similarly, on one hand, the growth mode of the aluminum nitride can be changed, the aluminum nitride crystal nucleus is delayed from three-dimensional to two-dimensional growth, the line defects and dislocations generated in the growth process of the aluminum nitride are greatly annihilated, and the aluminum nitride film with low defect concentration and high crystal quality is obtained.
The implementation of the invention has at least the following advantages:
1. according to the invention, the silicon nitride layer with the porous structure is added between the aluminum nitride layer and the substrate, and the surface of the substrate is patterned similarly, so that on one hand, the growth mode of the aluminum nitride can be changed, the growth of aluminum nitride crystal nucleus from three-dimensional to two-dimensional is delayed, the line defect and dislocation of the aluminum nitride in the growth process are greatly annihilated, and the aluminum nitride film with low defect concentration and high crystal quality is obtained, and on the other hand, the problem of mechanical damage possibly generated when the aluminum nitride layer and the substrate are mechanically stripped subsequently is avoided due to the excellent physical property of the silicon nitride.
2. On the basis of the silicon nitride layer, the aluminum nitride buffer layer grows at the temperature of 600-1000 ℃ and the pressure of 20-200mbar, so that the pre-reaction between sources is weakened, and the influence on the subsequent aluminum nitride layer is reduced.
3. On the basis of the aluminum nitride buffer layer, the temperature of the reaction chamber is controlled to be 1100-1500 ℃, and the pressure is controlled to be 20-200mbar, so that the aluminum atomic mobility is favorably improved, and the quality of the final aluminum nitride film can be effectively improved.
4. The aluminum nitride layer grows in stages by changing the growth rate of the aluminum nitride layer, so that the surface of the final aluminum nitride film is smoother.
5. The method is simple and easy to implement, and does not need the assistance of large-scale equipment.
6. By the preparation method provided by the invention, the high-quality aluminum nitride film can be obtained, and the performance of a device containing the aluminum nitride film is further improved.
In conclusion, the method for preparing the aluminum nitride film can effectively solve the problems that lattice mismatch exists between the aluminum nitride layer and the substrate and mechanical damage is possibly generated during subsequent mechanical stripping, and the prepared aluminum nitride film has the advantages of stable growth, low dislocation density, high crystal quality and the like by controlling the temperature and the pressure, so that the LED epitaxial structure and the LED product comprising the aluminum nitride film have good luminous brightness and long service life.
Drawings
FIG. 1 is a flow chart of a method for preparing an aluminum nitride film according to the present invention;
fig. 2 is a schematic structural diagram of an aluminum nitride film according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the embodiment provided by the invention, the substrates are all 2-inch circular sapphire substrates.
The silicon source is monocrystalline silicon with the purity of 99.9 percent.
Example 1
Step 1: cleaning a substrate, then sending the substrate into a magnetron sputtering reaction chamber, controlling the temperature of the reaction chamber to be 150 ℃, putting monocrystalline silicon, introducing 15sccm nitrogen, sputtering and growing a silicon nitride layer with a porous structure on the substrate, and growing for 200min to obtain a silicon nitride layer with the thickness of 1000 nm;
step 2: placing the grown silicon nitride layer into Metal Organic Chemical Vapor Deposition (MOCVD) equipment, controlling the temperature in a reaction chamber of the equipment at 600 ℃ and the pressure at 200mbar, and introducing 50ml of trimethylaluminum and 10000ml of NH3Growing an aluminum nitride buffer layer on the silicon nitride layer, and obtaining the aluminum nitride buffer layer with the thickness of 25nm after growing for 10 min;
and step 3: the temperature of the reaction chamber is controlled at 1150 ℃ and the pressure is 50mbar, 300ml of solution is introducedTrimethylaluminum and 10000ml of NH3Growing a first aluminum nitride layer on the aluminum nitride buffer layer, controlling the growth rate of the first aluminum nitride layer to be 0.8 mu m/h, and growing for 30min to obtain a first aluminum nitride layer with the thickness of 400 nm;
the temperature of the reaction chamber was controlled at 1300 ℃ and the pressure at 50mbar, 500ml of trimethylaluminum and 10000ml of NH were introduced3And controlling the growth rate to be 1.5 mu m/h, and growing for 60min to obtain a second aluminum nitride layer with the thickness of 1500 nm.
The finally obtained aluminum nitride film has a flat surface and no cracks, and XRD tests show that the half width in the (002) direction is 190arcsec, and the half width in the (102) direction is 380 arcsec.
Example 2
Step 1: cleaning a substrate, then sending the substrate into a magnetron sputtering reaction chamber, controlling the temperature of the reaction chamber to be 150 ℃, putting monocrystalline silicon, introducing 15sccm nitrogen, sputtering and growing a silicon nitride layer with a porous structure on the substrate, and growing for 240min to obtain a silicon nitride layer with the thickness of 1200 nm;
step 2: placing the grown silicon nitride layer into Metal Organic Chemical Vapor Deposition (MOCVD) equipment, controlling the temperature in a reaction chamber of the equipment at 600 ℃ and the pressure at 200mbar, and introducing 50ml of trimethylaluminum and 10000ml of NH3Growing an aluminum nitride buffer layer on the silicon nitride layer, and obtaining the aluminum nitride buffer layer with the thickness of 25nm after growing for 10 min;
and step 3: the temperature of the reaction chamber is controlled at 1150 ℃ and the pressure is 50mbar, 400ml of trimethylaluminum and 10000ml of NH are introduced3Growing a first aluminum nitride layer on the aluminum nitride buffer layer, controlling the growth rate of the first aluminum nitride layer to be 1 mu m/h, and growing for 30min to obtain a first aluminum nitride layer with the thickness of 500 nm;
the temperature of the reaction chamber was controlled at 1300 ℃ and the pressure at 50mbar, 500ml of trimethylaluminum and 10000ml of NH were introduced3And controlling the growth rate to be 1.5 mu m/h, and growing for 90min to obtain a second aluminum nitride layer with the thickness of 2250 nm.
The finally obtained aluminum nitride film has a flat surface and no cracks, and XRD tests show that the half width in the (002) direction is 150arcsec, and the half width in the (102) direction is 350 arcsec.
Example 3
Step 1: cleaning a substrate, then sending the substrate into a magnetron sputtering reaction chamber, controlling the temperature of the reaction chamber to be 120 ℃, adding monocrystalline silicon, introducing 15sccm nitrogen, sputtering and growing a silicon nitride layer with a porous structure on the substrate, and growing for 280min to obtain a silicon nitride layer with the thickness of 1400 nm;
step 2: placing the grown silicon nitride layer into Metal Organic Chemical Vapor Deposition (MOCVD) equipment, controlling the temperature in a reaction chamber of the equipment at 600 ℃ and the pressure at 200mbar, and introducing 50ml of trimethylaluminum and 10000ml of NH3Growing an aluminum nitride buffer layer on the silicon nitride layer, and obtaining the aluminum nitride buffer layer with the thickness of 25nm after growing for 10 min;
and step 3: the temperature of the reaction chamber is controlled at 1150 ℃ and the pressure is 50mbar, 400ml of trimethylaluminum and 10000ml of NH are introduced3Growing a first aluminum nitride layer on the aluminum nitride buffer layer, controlling the growth rate of the first aluminum nitride layer to be 1 mu m/h, and growing for 30min to obtain a first aluminum nitride layer with the thickness of 500 nm;
the temperature of the reaction chamber was controlled at 1300 ℃ and the pressure at 50mbar, 500ml of trimethylaluminum and 10000ml of NH were introduced3And controlling the growth rate to be 1.5 mu m/h, and growing for 120min to obtain a second aluminum nitride layer with the thickness of 3000 nm.
The finally obtained aluminum nitride film has a flat surface and no cracks, and XRD tests show that the half width in the (002) direction is 135arcsec, and the half width in the (102) direction is 300 arcsec.
Example 4
Step 1: cleaning a substrate, then sending the substrate into a magnetron sputtering reaction chamber, controlling the temperature of the reaction chamber to be 120 ℃, putting monocrystalline silicon, introducing 15sccmml of nitrogen, sputtering and growing a silicon nitride layer with a porous structure on the substrate, and growing for 300min to obtain a 1500nm silicon nitride layer;
step 2: placing the grown silicon nitride layer into Metal Organic Chemical Vapor Deposition (MOCVD) equipment, controlling the temperature in a reaction chamber of the equipment at 600 ℃ and the pressure at 200mbar, and introducing 50ml of trimethylaluminum and 10000ml of NH3Growing an aluminum nitride buffer layer on the silicon nitride layer for 10min,obtaining an aluminum nitride buffer layer with the thickness of 25 nm;
and step 3: the temperature of the reaction chamber is controlled at 1150 ℃ and the pressure is 50mbar, 300ml of trimethylaluminum and 10000ml of NH are introduced3Growing a first aluminum nitride layer on the aluminum nitride buffer layer, controlling the growth rate of the first aluminum nitride layer to be 0.8 mu m/h, and growing for 35min to obtain a first aluminum nitride layer with the thickness of 470 nm;
the temperature of the reaction chamber was controlled at 1300 ℃ and the pressure at 50mbar, 500ml of trimethylaluminum and 10000ml of NH were introduced3And controlling the growth rate to be 1.5 mu m/h, and growing for 125min to obtain a second aluminum nitride layer with the thickness of 3125 nm.
The finally obtained aluminum nitride film has a flat surface and no cracks, and XRD tests show that the half width in the (002) direction is 100arcsec, and the half width in the (102) direction is 280 arcsec.
According to the preparation method of the aluminum nitride layer, firstly, the silicon nitride layer with the porous structure is added between the aluminum nitride layer and the substrate, and the substrate surface is patterned similarly, so that on one hand, the growth mode of the aluminum nitride can be changed, the growth of aluminum nitride crystal nuclei from three dimensions to two dimensions is delayed, the line defects and dislocations generated in the growth process of the aluminum nitride are greatly annihilated, and the aluminum nitride layer with low defect concentration and high crystal quality is obtained, and on the other hand, because the silicon nitride has excellent physical properties, the problem that mechanical damage is possibly generated when the aluminum nitride layer and the substrate are mechanically stripped subsequently is avoided; secondly, on the basis of the silicon nitride layer, the reaction temperature is controlled to be 600-1000 ℃ and the pressure is controlled to be 20-200mbar, an aluminum nitride buffer layer grows, and under the temperature and the pressure, the pre-reaction between sources can be weakened, and the influence on the subsequent aluminum nitride layer is reduced; finally, on the basis of the aluminum nitride buffer layer, the temperature of the reaction chamber is controlled to be 1100-1500 ℃, and the pressure is 20-200mbar, so that the increase of the aluminum atomic mobility is facilitated, and the first aluminum nitride layer and the second aluminum nitride layer are grown by regulating and controlling the growth rate, so that the surface of the aluminum nitride film is smoother, and the quality of the final aluminum nitride film is effectively improved.
An N-type doped layer, a quantum well light-emitting layer, and a P-type doped layer are sequentially grown on the basis of the aluminum nitride film obtained in the embodiment 4 according to the prior art, and an LED epitaxial structure is prepared.
The LED epitaxial structure is prepared into a chip with the size of 350 mu m multiplied by 350 mu m, 20mA current is introduced, the working voltage is 6.0V, and the luminous brightness is 5 mW; and the service life of the LED device comprising the LED epitaxial structure is 1.5 ten thousand hours.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the aluminum nitride film is characterized by comprising the following steps of:
step 1, growing a silicon nitride layer with a porous structure on a substrate;
step 2, placing the silicon nitride layer into an equipment reaction chamber, controlling the temperature of the reaction chamber to be 600-1000 ℃ and the pressure to be 20-200mbar, and growing an aluminum nitride buffer layer on the surface of the silicon nitride layer;
and 3, controlling the temperature of the reaction chamber to be 1100-1500 ℃, and controlling the pressure to be 20-200mbar, and growing an aluminum nitride layer on the surface of the aluminum nitride buffer layer.
2. The method according to claim 1, wherein the silicon nitride layer is grown at 25 to 250 ℃ in step 1 by a magnetron sputtering method.
3. The method according to claim 2, wherein the silicon nitride layer has a thickness a of 5. ltoreq. a.ltoreq.2000 nm.
4. The method according to claim 1, wherein the aluminum nitride buffer layer has a thickness b, 0 < b ≦ 50 nm.
5. The method according to claim 1, wherein in step 3, a first aluminum nitride layer and a second aluminum nitride layer are sequentially grown on the surface of the aluminum nitride buffer layer, and the growth rate of the first aluminum nitride layer is smaller than that of the second aluminum nitride layer.
6. The method of claim 5, wherein the first aluminum nitride layer has a growth rate of 0.5 to 1 μm/h.
7. The method of claim 5, wherein the growth rate of the second aluminum nitride layer is 1-2 μm/h.
8. The method according to claim 1, wherein the first aluminum nitride layer has a thickness c, 100 ≦ c ≦ 800 nm; the thickness of the second aluminum nitride layer is d, and d is more than or equal to 1000 and less than or equal to 5000 nm.
9. An aluminum nitride film obtained by the production method according to any one of claims 1 to 8.
10. An LED epitaxial structure, comprising the aluminum nitride film obtained by the method according to any one of claims 1 to 8 or the aluminum nitride film according to claim 9.
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