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CN109326696A - 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 PDF

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Publication number
CN109326696A
CN109326696A CN201811098835.XA CN201811098835A CN109326696A CN 109326696 A CN109326696 A CN 109326696A CN 201811098835 A CN201811098835 A CN 201811098835A CN 109326696 A CN109326696 A CN 109326696A
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layer
sputtering
preparation
substrate
aln
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CN109326696B (en
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洪威威
王倩
韦春余
周飚
胡加辉
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Boe Huacan Optoelectronics Suzhou Co ltd
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HC Semitek Suzhou Co Ltd
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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
    • 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
    • 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
    • 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 kind of preparation methods of the epitaxial wafer of light emitting diode, belong to light emitting diode manufacturing field.In the AlN layers of multiple sputtering process grown on substrate, so that the sputtering power of magnetron sputtering apparatus is gradually successively decreased can be such that the rate of Al target in magnetron sputtering apparatus intermediate ion bombardment magnetron sputtering apparatus gradually decreases, so that the kinetic energy of Al atom gradually decreases, rate when Al atom is grown on substrate along the growth of its deposition direction reduces, Al atom is easier cross growth on substrate, the profile pattern of obtained AlN layer is preferable, and since AlN layers of deposition velocity gradually decreases, the defect that the AlN layer obtained compared to fast-growth can generate is less, AlN layers of quality is guaranteed, the quality of epitaxial layer entirety can be guaranteed, the luminous efficiency of light emitting diode can be improved.

Description

A kind of preparation method of the epitaxial wafer of light emitting diode
Technical field
The present invention relates to light emitting diode manufacturing field, in particular to a kind of preparation side of the epitaxial wafer of light emitting diode Method.
Background technique
Light emitting diode is a kind of semiconductor diode that electric energy can be converted to luminous energy, have small in size, the service life is long, The advantages that low in energy consumption, is widely used in automobile signal light, traffic lights, display screen and lighting apparatus at present.Epitaxial wafer It is the foundation structure for making light emitting diode, the structure of epitaxial wafer includes substrate and the epitaxial layer grown on substrate.Wherein, The structure of epitaxial layer specifically includes that AlN layer, the low temperature GaN buffer, undoped GaN layer, N-type successively grown on substrate GaN layer, active layer and p-type GaN layer.
The AlN layer being arranged between N-type GaN layer and substrate can reduce the lattice mismatch between substrate and epitaxial layer, guarantee The quality of epitaxial layer, and then improve the luminous efficiency of light emitting diode.Existing AlN layers can be given birth to by way of magnetron sputtering It is long, but the quality of the AlN layer grown by way of magnetron sputtering is still defective, and these defects in AlN layers can be external The total quality for prolonging piece impacts, so that the luminous efficiency of light emitting diode is affected.
Summary of the invention
The embodiment of the invention provides a kind of preparation methods of the epitaxial wafer of light emitting diode, can further increase luminous The luminous efficiency of diode.The technical solution is as follows:
The embodiment of the invention provides a kind of preparation method of the epitaxial wafer of light emitting diode, the preparation method includes:
One substrate is provided；
Growing AIN layer over the substrate；
N-type GaN layer is grown on the AlN layer；
Active layer is grown in the N-type GaN layer；
Growth P-type GaN layer on the active layer,
Growing AIN layer over the substrate, comprising:
The substrate is put into magnetron sputtering apparatus；
The substrate is repeatedly sputtered, forms AlN layers over the substrate, repeatedly the magnetron sputtering is set when sputtering Standby sputtering power gradually successively decreases.
Optionally, the sputtering power of the magnetron sputtering apparatus is arithmetic progression when repeatedly sputtering.
Optionally, the difference of the sputtering power of magnetron sputtering apparatus described in sputtering process adjacent twice when repeatedly sputtering It is 300~500W.
Optionally, the sputtering power of the magnetron sputtering apparatus is in 3000~5000W when repeatedly sputtering.
Optionally, the total duration repeatedly sputtered is 40~60s.
Optionally, the duration sputtered every time is equal.
Optionally, the when a length of 15~25s sputtered every time.
Optionally, the preparation method further include:
Before growing N-type GaN layer on the AlN layer, the substrate is placed on metallo-organic compound chemical gaseous phase It precipitates in MOCVD device；
It is passed through hydrogen into MOCVD device, the heat treatment of 10~15min is carried out to described AlN layers.
Optionally, the temperature of the heat treatment is 900~1100 DEG C.
Optionally, AlN layers of the growth pressure is 4~10mTorr.
Technical solution provided in an embodiment of the present invention have the benefit that AlN layers grow on substrate repeatedly splash During penetrating, so that the sputtering power of magnetron sputtering apparatus is gradually successively decreased can be such that magnetron sputtering apparatus intermediate ion bombardment magnetron sputtering sets The rate of standby middle Al target gradually decreases, so that the kinetic energy of Al atom gradually decreases, edge when Al atom is grown on substrate The rate of its deposition direction growth reduces, and Al atom is easier cross growth on substrate, the profile pattern of obtained AlN layer Preferably, and since AlN layers of deposition velocity gradually decreases, the defect that the AlN layer obtained compared to fast-growth can generate is less, AlN layers of quality is guaranteed, and the quality of epitaxial layer entirety can be guaranteed, the luminous efficiency of light emitting diode can be mentioned It is high.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other Attached drawing.
Fig. 1 is a kind of preparation method flow chart of the epitaxial wafer of light emitting diode provided in an embodiment of the present invention；
Fig. 2 is a kind of structural schematic diagram of the epitaxial wafer of light emitting diode provided in an embodiment of the present invention；
Fig. 3 is the preparation method flow chart of the epitaxial wafer of another light emitting diode provided in an embodiment of the present invention；
Fig. 4 is the structural schematic diagram of the epitaxial wafer of another light emitting diode provided in an embodiment of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention Formula is described in further detail.
Fig. 1 is a kind of preparation method flow chart of the epitaxial wafer of light emitting diode provided in an embodiment of the present invention, such as Fig. 1 institute Show, which includes:
S11: a substrate is provided.
S12: growing AIN layer on substrate.
Step S12 includes: to place the substrate into magnetron sputtering apparatus.Substrate is repeatedly sputtered, is formed on the substrate AlN layers, repeatedly the sputtering power of magnetron sputtering apparatus gradually successively decreases when sputtering.
It needs herein illustratively, in the equipment using magnetron sputtering, repeatedly sputtering forms AlN layers over the substrate In the process, total gas volume in the equipment of magnetron sputtering is constant.
S13: N-type GaN layer is grown on AlN layer.
S14: active layer is grown in N-type GaN layer.
S15: the growth P-type GaN layer on active layer.
In the AlN layers of multiple sputtering process grown on substrate, so that the sputtering power of magnetron sputtering apparatus is gradually successively decreased can Gradually decrease the rate of Al target in magnetron sputtering apparatus intermediate ion bombardment magnetron sputtering apparatus, so that Al atom is dynamic It can gradually decrease, rate when Al atom is grown on substrate along the growth of its deposition direction reduces, and Al atom is easier in substrate The profile pattern of upper cross growth, obtained AlN layer is preferable, and since AlN layers of deposition velocity gradually decreases, compared to fast The defect that the long obtained AlN layer of fast-growing can generate is less, and AlN layers of quality is guaranteed, and the quality of epitaxial layer entirety is available Guarantee, the luminous efficiency of light emitting diode can be improved.
Fig. 2 is a kind of structural schematic diagram of the epitaxial wafer of light emitting diode provided in an embodiment of the present invention, as shown in Fig. 2, The structure for executing the step the epitaxial wafer after S15 includes: substrate 1 and the AlN being sequentially laminated on substrate 1 layer 2, N-type GaN Layer 3, active layer 4 and p-type GaN layer 5, wherein active layer 4 includes alternately stacked InGaN well layer 41 and GaN barrier layer 42.
Fig. 3 is the preparation method flow chart of the epitaxial wafer of another light emitting diode provided in an embodiment of the present invention, such as Fig. 3 Shown, which includes:
S21: a substrate is provided.
Wherein, Sapphire Substrate can be used in substrate.
S22: growing AIN layer on substrate.
Step S22 includes: to place the substrate into magnetron sputtering apparatus.Substrate is repeatedly sputtered, is formed on the substrate AlN layers, repeatedly the sputtering power of magnetron sputtering apparatus gradually successively decreases when sputtering.
Wherein, the sputtering power of magnetron sputtering apparatus can be in 3000~5000W when repeatedly sputtering.Magnetron sputtering apparatus splashes It penetrates power and can guarantee that AlN layers of growth quality is preferable in range above.
Illustratively, the sputtering power of magnetron sputtering apparatus is arithmetic progression when repeatedly sputtering.This set can be convenient for control AlN layers of growth course processed, and the quality for growing obtained AlN layer is also preferable.
Optionally, repeatedly sputtering when adjacent twice sputtering process in magnetron sputtering apparatus sputtering power difference For 300~500W.The difference of the sputtering power of magnetron sputtering apparatus is arranged at range above in sputtering process adjacent twice The certifiable quality for growing obtained AlN layer is preferable.
Illustratively, the total duration repeatedly sputtered can be 40~60s.When the total duration repeatedly sputtered is arranged within this range Obtained AlN layer can more efficiently reduce the mass defect in epitaxial layer entirety, guarantee the luminous efficiency of light emitting diode.
Optionally, the duration sputtered every time is equal.This set is relatively easy to realize, and it is preferable also to obtain quality AlN layers.
Wherein, the when a length of 15~25s sputtered every time.Sputtering duration is arranged within this range every time, it is ensured that splashes every time The quality for the AlN layer penetrated is guaranteed.
Illustratively, temperature when repeatedly sputtering in magnetron sputtering apparatus is 600~800 DEG C.In AlN layers of growth course In, it is ALN layer preferable that AlN layers of sputter temperature is that range above can be obtained quality, guarantees in AlN, and then guarantee light-emitting diodes The arrangement quality of pipe.
Optionally, pressure when repeatedly sputtering in the magnetron sputtering apparatus can be 4~10mtorr.By AlN layers of sputtering Range above, which is arranged in, in pressure can guarantee that the quality of obtained AlN layer is preferable, and then guarantee the epitaxial layer grown on AlN layer Quality, the final luminous efficiency for improving light emitting diode.
Illustratively, during carrying out deposition growing by magnetron sputtering apparatus for AlN layers, it may include 3~5 sputterings The more appropriate AlN layer of thickness can be obtained in conjunction with aforementioned AlN layers of each sputtering time in process, and this set also more holds It is easy to control.
Optionally, AlN layers of thickness can be 15~40nm.Every time sputtering obtained AlN film, (repeatedly sputtering obtains AlN film form AlN layers) thickness can be 3~8nm.
Illustratively, before growing N-type GaN layer on AlN layer, substrate is placed on metallo-organic compound chemical gaseous phase It precipitates in MOCVD device；It is passed through hydrogen into MOCVD device, AlN layers are carried out with the heat treatment of 10~15min.Have that will grow AlN layers of substrate is transferred to after MOCVD, first in H2To AlN layers of progress high-temperature heat treatment under atmosphere, AlN layer surface can remove Partial impurities, guarantee the cleaning of AlN layer surface, and then guarantee the quality of the epitaxial layer grown on AlN layer.
Wherein, the temperature of heat treatment is 900~1100 DEG C.The heat treatment that AlN layers are carried out under the conditions of this temperature, can remove Most of impurity of AlN layer surface, is further ensured that the quality of the epitaxial layer grown on AlN layer.
S23: layer of undoped gan is grown on AlN layers.
The growth temperature of layer of undoped gan can be 1000~1100 DEG C, and growth pressure can be 100~500Torr.At this The quality of the layer of undoped gan grown under part is preferable.
Illustratively, the thickness of layer of undoped gan can be 1~5 μm.
S24: N-type GaN layer is grown in the layer of undoped gan.
Wherein, the growth temperature of N-type GaN layer can be 1000~1200 DEG C, and growth pressure can be 100~500Torr.
N-type GaN layer can carry out Si doping, and the concentration of Si doping can be 1 × 1018~1 × 1019cm-3。
S25: active layer is grown in N-type GaN layer.
Optionally, in step S25, active layer may include the InGaN/GaN multiple quantum well layer in 5~11 periods.Wherein, The growth temperature of InGaN well layer can be 720~829 DEG C, and the growth pressure of InGaN well layer can be 100~500Torr, InGaN trap The growth thickness of layer can be 2~3nm；The growth temperature of GaN barrier layer can be 850~959 DEG C, and the growth pressure of GaN barrier layer can be The growth thickness of 100~500Torr, GaN barrier layer can be 9~20nm.
S26: the growing low temperature p-type GaN layer on active layer.
Wherein, the growth temperature of p-type GaN layer can be 600~800 DEG C, and growth pressure can be 200~500Torr.
The thickness of p-type GaN layer can be 50~100nm.
The setting of low temperature p-type GaN layer can guarantee that have enough holes to enter active layer compound with electronics, to guarantee luminous two The luminous efficiency of pole pipe.
Step S27: electronic barrier layer is grown in low temperature P-type layer.
In the present embodiment, the growth temperature of electronic barrier layer can be 700~1000 DEG C, growth pressure can for 100~ 500Torr。
Optionally, the growth thickness of electronic barrier layer can be 20~100nm.
Electronic barrier layer may include p-type AlGaN electronic barrier layer.
S28: the growth P-type GaN layer on electronic barrier layer.
Wherein, the growth temperature of p-type GaN layer can be 800~1000 DEG C, the growth pressure of p-type GaN layer can for 200~ 600Torr, the growth thickness of p-type GaN layer can be 100~200nm.
S29: the growing P-type contact layer in p-type GaN layer.
Wherein, the growth temperature of p-type contact layer can be 850~1000 DEG C, the growth pressure of p-type GaN layer can for 100~ 300Torr, the growth thickness of p-type GaN layer can be 10~50nm.
Illustratively, after executing the step S29, this preparation method further includes carrying out under nitrogen atmosphere to epitaxial wafer Annealing, wherein annealing temperature is 650~850 DEG C, and anneal duration is 5~15min.
Fig. 4 is the structural schematic diagram of the epitaxial wafer of another light emitting diode provided in an embodiment of the present invention, has executed step The structure of epitaxial wafer after rapid S29 as shown in figure 4, epitaxial wafer include substrate 1 and the AlN being sequentially laminated on substrate 1 layer 2, Layer of undoped gan 6, N-type GaN layer 3, active layer 4, low temperature p-type GaN layer 7, electronic barrier layer 8, p-type GaN layer 5 and p-type contact layer 9, wherein active layer 4 includes alternately stacked InGaN well layer 41 and GaN barrier layer 42.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (10)

1.一种发光二极管的外延片的制备方法，所述制备方法包括：1. A preparation method of an epitaxial wafer of a light-emitting diode, the preparation method comprising: 提供一衬底；providing a substrate; 在所述衬底上生长AlN层；growing an AlN layer on the substrate; 在所述AlN层上生长N型GaN层；growing an N-type GaN layer on the AlN layer; 在所述N型GaN层上生长有源层；growing an active layer on the N-type GaN layer; 在所述有源层上生长P型GaN层，growing a p-type GaN layer on the active layer, 其特征在于，在所述衬底上生长AlN层，包括：It is characterized in that, growing the AlN layer on the substrate includes: 将所述衬底放入磁控溅射设备中；placing the substrate into a magnetron sputtering device; 对所述衬底进行多次溅射，在所述衬底上形成AlN层，多次溅射时所述磁控溅射设备的溅射功率逐渐递减。The substrate is sputtered multiple times to form an AlN layer on the substrate, and the sputtering power of the magnetron sputtering device gradually decreases during multiple sputtering. 2.根据权利要求1所述的制备方法，其特征在于，多次溅射时所述磁控溅射设备的溅射功率为等差数列。2 . The preparation method according to claim 1 , wherein the sputtering power of the magnetron sputtering equipment is an arithmetic progression during multiple sputtering. 3 . 3.根据权利要求2所述的制备方法，其特征在于，多次溅射时两次相邻的溅射过程中所述磁控溅射设备的溅射功率的差值均为300～500W。3 . The preparation method according to claim 2 , wherein the difference between the sputtering powers of the magnetron sputtering equipment in two adjacent sputtering processes during multiple sputtering is 300-500 W. 4 . 4.根据权利要求2所述的制备方法，其特征在于，多次溅射时所述磁控溅射设备的溅射功率在3000～5000W。4 . The preparation method according to claim 2 , wherein the sputtering power of the magnetron sputtering equipment is 3000-5000W during multiple sputtering. 5 . 5.根据权利要求1～4任一项所述的制备方法，其特征在于，多次溅射的总时长为40～60s。5 . The preparation method according to claim 1 , wherein the total duration of multiple sputtering is 40 to 60 s. 6 . 6.根据权利要求2所述的制备方法，其特征在于，每次溅射的时长相等。6 . The preparation method according to claim 2 , wherein each sputtering has the same duration. 7 . 7.根据权利要求6所述的制备方法，其特征在于，每次溅射的时长为15～25s。7 . The preparation method according to claim 6 , wherein the duration of each sputtering is 15-25 s. 8 . 8.根据权利要求1～4任一项所述的制备方法，其特征在于，所述制备方法还包括：8. The preparation method according to any one of claims 1 to 4, wherein the preparation method further comprises: 在所述AlN层上生长N型GaN层之前，将所述衬底放置在金属有机化合物化学气相沉淀MOCVD设备中；before growing the N-type GaN layer on the AlN layer, placing the substrate in a metal organic compound chemical vapor deposition MOCVD apparatus; 向MOCVD设备中通入氢气，对所述AlN层进行10～15min的热处理。Pour hydrogen into the MOCVD equipment, and perform heat treatment on the AlN layer for 10 to 15 minutes. 9.根据权利要求8所述的制备方法，其特征在于，所述热处理的温度为900～1100℃。9 . The preparation method according to claim 8 , wherein the temperature of the heat treatment is 900-1100° C. 10 . 10.根据权利要求1～4任一项所述的制备方法，其特征在于，所述AlN层的生长压力为4～10mTorr。10 . The preparation method according to claim 1 , wherein the growth pressure of the AlN layer is 4-10 mTorr. 11 .
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CN118712057A (en) * 2024-08-28 2024-09-27 广东中图半导体科技股份有限公司 Preparation method of aluminum nitride thin film

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CN113481593A (en) * 2021-05-14 2021-10-08 华灿光电（浙江）有限公司 Preparation method of light-emitting diode epitaxial wafer with AlN
CN118712057A (en) * 2024-08-28 2024-09-27 广东中图半导体科技股份有限公司 Preparation method of aluminum nitride thin film
CN118712057B (en) * 2024-08-28 2024-12-31 广东中图半导体科技股份有限公司 Preparation method of aluminum nitride film

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