CN109326696B - A kind of preparation method of epitaxial wafer of light-emitting diode - Google Patents
A kind of preparation method of epitaxial wafer of light-emitting diode Download PDFInfo
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- CN109326696B CN109326696B CN201811098835.XA CN201811098835A CN109326696B CN 109326696 B CN109326696 B CN 109326696B CN 201811098835 A CN201811098835 A CN 201811098835A CN 109326696 B CN109326696 B CN 109326696B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims abstract description 62
- 239000000758 substrate Substances 0.000 claims abstract description 47
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 6
- 230000008021 deposition Effects 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 abstract description 3
- 239000013077 target material Substances 0.000 abstract description 3
- 230000000903 blocking effect Effects 0.000 description 7
- 230000004888 barrier function Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
- H10H20/80—Constructional details
- H10H20/81—Bodies
- H10H20/822—Materials of the light-emitting regions
- H10H20/824—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP
- H10H20/825—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP containing nitrogen, e.g. GaN
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
- H10H20/01—Manufacture or treatment
- H10H20/011—Manufacture or treatment of bodies, e.g. forming semiconductor layers
- H10H20/013—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials
- H10H20/0137—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials the light-emitting regions comprising nitride materials
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
- H10H20/80—Constructional details
- H10H20/81—Bodies
- H10H20/815—Bodies having stress relaxation structures, e.g. buffer layers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
- H10H20/80—Constructional details
- H10H20/81—Bodies
- H10H20/822—Materials of the light-emitting regions
- H10H20/824—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP
- H10H20/825—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP containing nitrogen, e.g. GaN
- H10H20/8252—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP containing nitrogen, e.g. GaN characterised by the dopants
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Abstract
The invention discloses a preparation method of an epitaxial wafer of a light-emitting diode, belonging to the field of light-emitting diode manufacturing. In the multiple sputtering process of the AlN layer growing on the substrate, the sputtering power of the magnetron sputtering equipment is gradually reduced, so that the speed of bombarding the Al target material in the magnetron sputtering equipment by ions in the magnetron sputtering equipment is gradually reduced, further, the kinetic energy of Al atoms is gradually reduced, the growth speed of the Al atoms along the deposition direction is reduced when the Al atoms grow on the substrate, the Al atoms are easier to grow transversely on the substrate, the surface smoothness of the obtained AlN layer is better, and because the deposition speed of the AlN layer is gradually reduced, the defects generated compared with the AlN layer obtained by rapid growth are fewer, the quality of the AlN layer is ensured, the overall quality of the epitaxial layer can be ensured, and the luminous efficiency of the light-emitting diode can be improved.
Description
Technical Field
The invention relates to the field of light emitting diode manufacturing, in particular to a method for preparing an epitaxial wafer of a light emitting diode.
Background
The light emitting diode is a semiconductor diode capable of converting electric energy into light energy, has the advantages of small volume, long service life, low power consumption and the like, and is widely applied to automobile signal lamps, traffic signal lamps, display screens and lighting equipment at present. The epitaxial wafer is a basic structure for manufacturing the light emitting diode, and the structure of the epitaxial wafer comprises a substrate and an epitaxial layer grown on the substrate. Wherein, the structure of epitaxial layer mainly includes: an AlN layer, a low-temperature GaN buffer layer, an undoped GaN layer, an N-type GaN layer, an active layer and a P-type GaN layer which are sequentially grown on the substrate.
The AlN layer arranged between the N-type GaN layer and the substrate can reduce lattice mismatch between the substrate and the epitaxial layer, ensure the quality of the epitaxial layer and further improve the luminous efficiency of the light-emitting diode. The existing AlN layer can grow in a magnetron sputtering mode, but the quality of the AlN layer obtained by the growth in the magnetron sputtering mode still has defects, and the defects in the AlN layer can influence the overall quality of an epitaxial wafer, so that the luminous efficiency of the light-emitting diode is influenced.
Disclosure of Invention
The embodiment of the invention provides a preparation method of an epitaxial wafer of a light-emitting diode, which can further improve the light-emitting efficiency of the light-emitting diode. The technical scheme is as follows:
the embodiment of the invention provides a preparation method of an epitaxial wafer of a light-emitting diode, which comprises the following steps:
providing a substrate;
growing an AlN layer on the substrate;
growing an N-type GaN layer on the AlN layer;
growing an active layer on the N-type GaN layer;
growing a P-type GaN layer on the active layer,
growing an AlN layer on the substrate, comprising:
putting the substrate into a magnetron sputtering device;
and sputtering the substrate for multiple times to form an AlN layer on the substrate, wherein the sputtering power of the magnetron sputtering equipment is gradually reduced during the multiple sputtering.
Optionally, the sputtering power of the magnetron sputtering device during multiple times of sputtering is an arithmetic progression.
Optionally, the difference of the sputtering power of the magnetron sputtering device in two adjacent sputtering processes during multiple times of sputtering is 300-500W.
Optionally, the sputtering power of the magnetron sputtering device during multiple times of sputtering is 3000-5000W.
Optionally, the total time length of the multiple times of sputtering is 40-60 s.
Optionally, the duration of each sputtering is equal.
Optionally, the time length of each sputtering is 15-25 s.
Optionally, the preparation method further comprises:
placing the substrate in a Metal Organic Chemical Vapor Deposition (MOCVD) apparatus before growing an N-type GaN layer on the AlN layer;
and introducing hydrogen into MOCVD equipment, and carrying out heat treatment on the AlN layer for 10-15 min.
Optionally, the temperature of the heat treatment is 900-1100 ℃.
Optionally, the growth pressure of the AlN layer is 4-10 mTorr.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: in the multiple sputtering process of the AlN layer growing on the substrate, the sputtering power of the magnetron sputtering equipment is gradually reduced, so that the speed of bombarding the Al target material in the magnetron sputtering equipment by ions in the magnetron sputtering equipment is gradually reduced, further, the kinetic energy of Al atoms is gradually reduced, the growth speed of the Al atoms along the deposition direction is reduced when the Al atoms grow on the substrate, the Al atoms are easier to grow transversely on the substrate, the surface smoothness of the obtained AlN layer is better, and because the deposition speed of the AlN layer is gradually reduced, the defects generated compared with the AlN layer obtained by rapid growth are fewer, the quality of the AlN layer is ensured, the overall quality of the epitaxial layer can be ensured, and the luminous efficiency of the light-emitting diode can be improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a flowchart of a method for manufacturing an epitaxial wafer of a light emitting diode according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an epitaxial wafer of a light emitting diode according to an embodiment of the present invention;
fig. 3 is a flowchart of another method for manufacturing an epitaxial wafer of a light emitting diode according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of an epitaxial wafer of another light emitting diode according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Fig. 1 is a flowchart of a method for manufacturing an epitaxial wafer of a light emitting diode according to an embodiment of the present invention, and as shown in fig. 1, the method includes:
S11: a substrate is provided.
S12: an AlN layer is grown on the substrate.
Step S12 includes: the substrate is placed in a magnetron sputtering apparatus. And sputtering the substrate for multiple times to form an AlN layer on the substrate, wherein the sputtering power of the magnetron sputtering equipment is gradually reduced during the multiple sputtering.
It should be noted here that, in the process of forming an AlN layer by sputtering on the substrate a plurality of times using a magnetron sputtering apparatus, the total gas volume in the magnetron sputtering apparatus is not changed.
S13: and growing an N-type GaN layer on the AlN layer.
S14: and growing an active layer on the N-type GaN layer.
S15: and growing a P-type GaN layer on the active layer.
In the multiple sputtering process of the AlN layer growing on the substrate, the sputtering power of the magnetron sputtering equipment is gradually reduced, so that the speed of bombarding the Al target material in the magnetron sputtering equipment by ions in the magnetron sputtering equipment is gradually reduced, further, the kinetic energy of Al atoms is gradually reduced, the growth speed of the Al atoms along the deposition direction is reduced when the Al atoms grow on the substrate, the Al atoms are easier to grow transversely on the substrate, the surface smoothness of the obtained AlN layer is better, and because the deposition speed of the AlN layer is gradually reduced, the defects generated compared with the AlN layer obtained by rapid growth are fewer, the quality of the AlN layer is ensured, the overall quality of the epitaxial layer can be ensured, and the luminous efficiency of the light-emitting diode can be improved.
Fig. 2 is a schematic structural diagram of an epitaxial wafer of a light emitting diode according to an embodiment of the present invention, and as shown in fig. 2, the structure of the epitaxial wafer after step S15 is executed includes: the GaN-based light-emitting diode comprises a substrate 1, and an AlN layer 2, an N-type GaN layer 3, an active layer 4 and a P-type GaN layer 5 which are sequentially laminated on the substrate 1, wherein the active layer 4 comprises InGaN well layers 41 and GaN barrier layers 42 which are alternately laminated.
Fig. 3 is a flowchart of a method for manufacturing an epitaxial wafer of a light emitting diode according to another embodiment of the present invention, as shown in fig. 3, the method includes:
s21: a substrate is provided.
Among them, a sapphire substrate may be used as the substrate.
S22: an AlN layer is grown on the substrate.
Step S22 includes: the substrate is placed in a magnetron sputtering apparatus. And sputtering the substrate for multiple times to form an AlN layer on the substrate, wherein the sputtering power of the magnetron sputtering equipment is gradually reduced during the multiple sputtering.
Wherein, the sputtering power of the magnetron sputtering equipment can be 3000-5000W during multiple times of sputtering. The sputtering power of the magnetron sputtering equipment is in the range above, so that the growth quality of the AlN layer can be ensured to be better.
Illustratively, the sputtering power of the magnetron sputtering device is an arithmetic progression in a plurality of times of sputtering. The arrangement can facilitate the control of the growth process of the AlN layer, and the quality of the AlN layer obtained by growth is better.
Optionally, the difference of the sputtering power of the magnetron sputtering device in two adjacent sputtering processes during multiple times of sputtering can be 300-500W. The difference value of the sputtering power of the magnetron sputtering equipment in the two adjacent sputtering processes is set in the range, so that the good quality of the grown AlN layer can be ensured.
Illustratively, the total duration of the multiple sputters can be 40-60 seconds. The AlN layer obtained when the total time of the multiple times of sputtering is set within the range can effectively reduce the quality defect of the whole epitaxial layer and ensure the luminous efficiency of the light-emitting diode.
Optionally, the duration of each sputtering is equal. This arrangement is relatively easy to implement and also enables a good quality AlN layer.
Wherein the time length of each sputtering is 15-25 s. The time length of each sputtering is set within the range, so that the quality of the AlN layer obtained by each sputtering can be guaranteed.
Illustratively, the temperature in the magnetron sputtering device is 600-800 ℃ during multiple times of sputtering. In the growth process of the AlN layer, the AlN layer with better quality can be obtained when the sputtering temperature of the AlN layer is in the range, the AlN is ensured, and the finishing quality of the light-emitting diode is further ensured.
Optionally, the pressure in the magnetron sputtering equipment during multiple times of sputtering can be 4-10 mtorr. The sputtering pressure of the AlN layer is set in the range, so that the obtained AlN layer can be guaranteed to have good quality, the quality of an epitaxial layer growing on the AlN layer is further guaranteed, and the luminous efficiency of the light-emitting diode is finally improved.
Illustratively, during the process of depositing and growing the AlN layer by the magnetron sputtering equipment, 3-5 times of sputtering processes can be included, and in combination with each sputtering time of the AlN layer, the AlN layer with a proper thickness can be obtained, and the arrangement is easy to control.
Alternatively, the AlN layer may have a thickness of 15 to 40 nm. The AlN thin film obtained by each sputtering (the AlN thin film obtained by multiple times of sputtering constitutes an AlN layer) may have a thickness of 3 to 8 nm.
Illustratively, prior to growing the N-type GaN layer on the AlN layer, the substrate is placed in a metal-organic chemical vapor deposition MOCVD apparatus; and introducing hydrogen into the MOCVD equipment, and carrying out heat treatment on the AlN layer for 10-15 min. After the substrate on which the AlN layer is grown is transferred to MOCVD, it is first subjected to H2And (3) carrying out high-temperature heat treatment on the AlN layer in the atmosphere, removing partial impurities on the surface of the AlN layer, and ensuring the cleanness of the surface of the AlN layer so as to ensure the quality of the epitaxial layer growing on the AlN layer.
Wherein the temperature of the heat treatment is 900-1100 ℃. The heat treatment of the AlN layer is carried out under the temperature condition, so that most impurities on the surface of the AlN layer can be removed, and the quality of an epitaxial layer grown on the AlN layer is further ensured.
S23: an undoped GaN layer is grown on the AlN layer.
The growth temperature of the undoped GaN layer can be 1000-1100 ℃, and the growth pressure can be 100-500 Torr. The quality of the undoped GaN layer grown under the condition is better.
Illustratively, the thickness of the undoped GaN layer may be 1-5 μm.
S24: and growing an N-type GaN layer on the undoped GaN layer.
Wherein the growth temperature of the N-type GaN layer can be 1000-1200 deg.C, and the growth pressure can be 100-500 Torr.
The N-type GaN layer can be doped with Si at a concentration of 1 × 1018～1×1019cm-3。
S25: and growing an active layer on the N-type GaN layer.
Optionally, in step S25, the active layer may include 5 to 11 periods of InGaN/GaN multiple quantum well layers. The growth temperature of the InGaN well layer can be 720-829 ℃, the growth pressure of the InGaN well layer can be 100-500 Torr, and the growth thickness of the InGaN well layer can be 2-3 nm; the growth temperature of the GaN barrier layer can be 850-959 ℃, the growth pressure of the GaN barrier layer can be 100-500 Torr, and the growth thickness of the GaN barrier layer can be 9-20 nm.
S26: and growing a low-temperature P-type GaN layer on the active layer.
Wherein the growth temperature of the P-type GaN layer can be 600-800 ℃, and the growth pressure can be 200-500 Torr.
The thickness of the P-type GaN layer can be 50-100 nm.
The arrangement of the low-temperature P-type GaN layer can ensure that enough holes enter the active layer to be compounded with electrons, so that the luminous efficiency of the light-emitting diode is ensured.
Step S27: and growing an electron blocking layer on the low-temperature P-type layer.
In the present embodiment, the growth temperature of the electron blocking layer can be 700-1000 ℃, and the growth pressure can be 100-500 Torr.
Optionally, the growth thickness of the electron blocking layer can be 20-100 nm.
The electron blocking layer may include a P-type AlGaN electron blocking layer.
S28: and growing a P-type GaN layer on the electron blocking layer.
Wherein the growth temperature of the P-type GaN layer can be 800-1000 ℃, the growth pressure of the P-type GaN layer can be 200-600 Torr, and the growth thickness of the P-type GaN layer can be 100-200 nm.
S29: and growing a P-type contact layer on the P-type GaN layer.
Wherein the growth temperature of the P-type contact layer can be 850-1000 ℃, the growth pressure of the P-type GaN layer can be 100-300 Torr, and the growth thickness of the P-type GaN layer can be 10-50 nm.
After the step S29 is completed, the method further includes annealing the epitaxial wafer in a nitrogen atmosphere, wherein the annealing temperature is 650 to 850 ℃, and the annealing time is 5 to 15 min.
Fig. 4 is a schematic structural diagram of another epitaxial wafer of a light emitting diode according to an embodiment of the present invention, and the structure of the epitaxial wafer after step S29 is completed is shown in fig. 4, where the epitaxial wafer includes a substrate 1, and an AlN layer 2, an undoped GaN layer 6, an N-type GaN layer 3, an active layer 4, a low-temperature P-type GaN layer 7, an electron blocking layer 8, a P-type GaN layer 5, and a P-type contact layer 9 sequentially stacked on the substrate 1, where the active layer 4 includes an InGaN well layer 41 and a GaN barrier layer 42 that are alternately stacked.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of an epitaxial wafer of a light-emitting diode comprises the following steps:
providing a substrate;
growing an AlN layer on the substrate;
growing an N-type GaN layer on the AlN layer;
growing an active layer on the N-type GaN layer;
growing a P-type GaN layer on the active layer,
wherein growing an AlN layer on the substrate comprises:
putting the substrate into a magnetron sputtering device;
sputtering the substrate for 3-5 times to form an AlN layer on the substrate, gradually decreasing the sputtering power of the magnetron sputtering equipment during 3-5 times of sputtering, setting the sputtering power of the magnetron sputtering equipment to be an arithmetic progression during 3-5 times of sputtering, setting the difference value of the sputtering power of the magnetron sputtering equipment in two adjacent sputtering processes during 3-5 times of sputtering to be 300-500W, setting the total duration of 3-5 times of sputtering to be 40-60 s, and setting the thickness of the AlN layer to be 15-40 nm.
2. The preparation method of claim 1, wherein the sputtering power of the magnetron sputtering device during multiple times of sputtering is 3000-5000W.
3. The method of claim 1, wherein the duration of each sputtering is equal.
4. The method according to claim 3, wherein the time period of each sputtering is 15 to 25 seconds.
5. The production method according to claim 1 or 2, characterized by further comprising:
placing the substrate in a Metal Organic Chemical Vapor Deposition (MOCVD) apparatus before growing an N-type GaN layer on the AlN layer;
and introducing hydrogen into MOCVD equipment, and carrying out heat treatment on the AlN layer for 10-15 min.
6. The method according to claim 5, wherein the heat treatment is carried out at a temperature of 900 to 1100 ℃.
7. The production method according to claim 1 or 2, wherein a growth pressure of the AlN layer is 4 to 10 mTorr.
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