CN113644170A - LED epitaxial structure based on in-situ heat treatment method and growth method thereof - Google Patents
LED epitaxial structure based on in-situ heat treatment method and growth method thereof Download PDFInfo
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- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
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- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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Abstract
The application provides an LED epitaxial structure based on an in-situ heat treatment method and a growth method thereof, wherein a multi-quantum well active layer grows on a stress release layer, the multi-quantum well active layer comprises GaN quantum barrier layers and InGaN quantum well layers which alternately grow periodically, and the InGaN quantum well layers are composed of a plurality of InGaN quantum well layer sublayers; most of C, O and other impurities In the InGaN epitaxial material are decomposed and removed In the heat treatment process through multiple In-situ heat treatments, and because the epitaxial growth is interrupted during the In-situ heat treatment, namely the In-situ heat annealing is carried out on the surface of the epitaxial InGaN material, the InGaN crystal lattice with poor crystal lattice quality is fully recombined, the built-In stress of the material is released as far as possible, the crystal lattice quality of an InGaN quantum well layer is integrally improved, and the light emitting efficiency of the GaN-based LED with high In component is improved.
Description
Technical Field
The invention relates to the technical field of light emitting diode epitaxy, in particular to an LED epitaxial structure based on an in-situ heat treatment method and a growth method thereof.
Background
Light Emitting Diodes (LEDs) have many advantages such as small size, long life, low power consumption, high brightness, and easy integration, and are widely used in the epitaxial GaN-based LED technology using Metal Organic Chemical Vapor Deposition (MOCVD) equipment based on gallium nitride (GaN) -based materials. The key light emitting structure of the GaN-based LED structure can realize the mass production of the LED from an Ultraviolet (UV) waveband to a green waveband by changing the components doped with Al and In. Among them, the GaN-based LED can further realize emission of different wavelengths by increasing the composition of In element In GaN.
However, since the vapor pressure of In atoms is higher than that of Ga atoms, when a GaN-based material is epitaxially grown on a Si substrate or a sapphire substrate by using an MOCVD apparatus, the increase of In components requires the reduction of the epitaxial temperature, which reduces the lattice quality of InGaN materials, and In addition, the lattice constant of InGaN is larger than that of GaN, and the built-In stress In the epitaxial process increases with the increase of In components, thereby causing serious deterioration of InGaN materials from GaN-based LEDs with high In components to a light emitting layer, which is characterized by uneven surface, dense pits, uneven In element doping, excessive impurity such as C, O, and the like; eventually leading to a GaN-based LED with a high In composition with a very weak or even no light emission.
Disclosure of Invention
In order to overcome the problems In the prior art, the invention provides an LED epitaxial structure based on an In-situ heat treatment method and a growth method thereof, so as to ensure that most of C, O and other impurities In an InGaN epitaxial material are decomposed and removed In the heat treatment process, promote the sufficient recombination of the original InGaN crystal lattice with poor crystal lattice quality and release the built-In stress of the material as far as possible, thereby integrally improving the crystal lattice quality of the InGaN of the core luminescent material layer and solving the problem of low luminescent efficiency of a GaN-based LED with high In component.
In one aspect, the present application provides a method for growing an LED epitaxial structure based on an in situ heat treatment method, including:
sequentially growing a buffer layer and an N-type electron injection layer on a substrate;
growing a stress release layer on the N-type electron injection layer;
growing a multi-quantum well active layer on the stress release layer, wherein the multi-quantum well active layer comprises GaN quantum barrier layers and InGaN quantum well layers which alternately grow periodically, and the InGaN quantum well layer consists of a plurality of InGaN quantum well layer sublayers;
and sequentially growing an electron blocking layer, a P-type hole injection layer and an ohmic contact layer on the multi-quantum well active layer.
Growing a multi-quantum well active layer on the stress relief layer comprises:
growing a GaN quantum barrier layer on the stress release layer;
growing an InGaN quantum well layer on the GaN quantum barrier layer, wherein the InGaN quantum well layer is composed of a plurality of InGaN quantum well layer sub-layers subjected to in-situ heat treatment, and the number of the InGaN quantum well layer sub-layers is at least 2;
judging whether the number of InGaN quantum well layers reaches a preset number;
if the number of layers does not reach the preset number of layers, repeating the cycle to alternately grow the GaN quantum barrier layer and the InGaN quantum well layer on the topmost InGaN quantum well layer until the preset number of layers is reached.
And if the number of layers reaches a preset number, growing a GaN quantum barrier layer on the InGaN quantum well layer at the topmost layer to obtain a multi-quantum well active layer.
The method for growing the InGaN quantum well layer on the GaN quantum barrier layer specifically comprises the following steps:
growing an InGaN quantum well layer sublayer on the GaN quantum barrier layer to obtain a first InGaN quantum well layer sublayer;
growing an InGaN quantum well layer sub-layer on the first InGaN quantum well layer sub-layer to obtain a second InGaN quantum well layer sub-layer;
judging whether the number of layers of the InGaN quantum well layer sub-layer reaches a preset number of layers or not;
if the number of layers does not reach the preset number of layers, repeatedly growing InGaN quantum well layer sub-layers on the second InGaN quantum well layer sub-layer until the number of layers reaches the preset number of layers;
and if the number of layers reaches a preset number, obtaining the InGaN quantum well layer.
The InGaN quantum well layer sub-layer growing on the GaN quantum barrier layer specifically comprises the following steps:
and under a preset gas atmosphere, starting the input of an In source and a Ga source on the GaN quantum barrier layer, controlling the temperature to be at a first preset temperature, stopping the input of the In source and the Ga source after a first preset time, maintaining the temperature to be at the first preset temperature, and obtaining an InGaN quantum well layer sublayer subjected to In-situ heat treatment after a second preset time.
The preset gas atmosphere is nitrogen atmosphere or nitrogen/hydrogen mixed atmosphere.
The first preset temperature is 600-800 ℃.
The first preset time is 12s-60s, the second preset time is 5s-60s, and the second preset time is a fixed value in the growth process of the same LED epitaxial structure.
In a second aspect, the present application provides an in situ heat treatment based LED epitaxial structure, comprising:
a substrate;
the buffer layer, the N-type electron injection layer, the stress release layer, the multi-quantum well active layer electron barrier layer, the P-type hole injection layer and the ohmic contact layer are sequentially arranged from bottom to top on the substrate;
the active layer of the multi-quantum well comprises a plurality of InGaN quantum well layers and GaN quantum barrier layers, the InGaN quantum well layers and the GaN quantum barrier layers are alternately arranged from bottom to top, and the InGaN quantum well layers are composed of a plurality of InGaN quantum well layer sub-layers subjected to in-situ heat treatment.
According to the technical scheme, the LED epitaxial structure based on the in-situ heat treatment method and the growth method thereof are provided, wherein a multi-quantum well active layer grows on the stress release layer, the multi-quantum well active layer comprises GaN quantum barrier layers and InGaN quantum well layers which alternately grow periodically, and the InGaN quantum well layer consists of a plurality of InGaN quantum well layer sublayers; most of C, O and other impurities In the InGaN epitaxial material are decomposed and removed In the heat treatment process through multiple In-situ heat treatments, and because the epitaxial growth is interrupted during the In-situ heat treatment, namely the In-situ heat annealing is carried out on the surface of the epitaxial InGaN material, the InGaN crystal lattice with poor crystal lattice quality is fully recombined, the built-In stress of the material is released as far as possible, the crystal lattice quality of an InGaN quantum well layer is integrally improved, and the light emitting efficiency of the GaN-based LED with high In component is improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
Fig. 1 is a flowchart of a method for growing an LED epitaxial structure based on an in-situ heat treatment method according to the present application;
fig. 2 is a schematic structural diagram corresponding to step S1;
fig. 3 is a schematic structural diagram corresponding to step S2;
fig. 4 is a schematic structural diagram corresponding to step S3;
FIG. 5 is a flow chart of one embodiment of a method for growing an LED epitaxial structure based on an in situ heat treatment process as set forth herein;
fig. 6 is a flowchart illustrating another embodiment of a method for growing an LED epitaxial structure based on an in situ heat treatment process according to the present application;
fig. 7 is a schematic structural diagram corresponding to step S32;
fig. 8 is a schematic structural diagram corresponding to step S4.
Detailed Description
Based on the above, the embodiment of the application provides an LED epitaxial structure based on an in-situ heat treatment method and a growth method thereof, wherein a multiple quantum well active layer is grown on a stress release layer, the multiple quantum well active layer comprises GaN quantum barrier layers and InGaN quantum well layers which are alternately grown periodically, and the InGaN quantum well layers are composed of a plurality of InGaN quantum well layer sublayers; most of C, O and other impurities In the InGaN epitaxial material are decomposed and removed In the heat treatment process through multiple In-situ heat treatments, and because the epitaxial growth is interrupted during the In-situ heat treatment, namely the In-situ heat annealing is carried out on the surface of the epitaxial InGaN material, the InGaN crystal lattice with poor crystal lattice quality is fully recombined, the built-In stress of the material is released as far as possible, the crystal lattice quality of an InGaN quantum well layer is integrally improved, and the light emitting efficiency of the GaN-based LED with high In component is improved. In order to achieve the above object, the technical solutions provided by the embodiments of the present application are described in detail below, specifically with reference to fig. 1 to 8.
Referring to fig. 1, a flowchart of a method for growing an LED epitaxial structure based on an in-situ heat treatment method is provided in an embodiment of the present application, where the method includes:
s1: sequentially growing a buffer layer and an N-type electron injection layer on a substrate;
s2: growing a stress release layer on the N-type electron injection layer;
s3: growing a multi-quantum well active layer on the stress release layer, wherein the multi-quantum well active layer comprises GaN quantum barrier layers and InGaN quantum well layers which alternately grow periodically, and the InGaN quantum well layer consists of a plurality of InGaN quantum well layer sublayers;
s4: and sequentially growing an electron blocking layer, a P-type hole injection layer and an ohmic contact layer on the multi-quantum well active layer.
Referring to fig. 2, a buffer layer 200 and an N-type electron injection layer 300 are sequentially grown on a substrate 100, corresponding to step S1.
In an embodiment of the present application, the substrate provided in the present application may be a silicon substrate or a sapphire substrate, and the present application is not particularly limited.
In an embodiment of the present application, the buffer layer 200 may be an undoped GaN buffer layer, and the N-type electron injection layer 300 may be an N-type GaN layer.
Referring to fig. 3, corresponding to step S2, a stress relief layer 400 is grown on the N-type electron injection layer 300, wherein the stress relief layer 400 is formed by combining one or more of AlGaN, InGaN, or GaN, and the LED epitaxial structure is optimized by the stress relief layer.
Referring to fig. 4, a multi-quantum well active layer 500 is grown on the stress relieving layer 400, corresponding to step S3. The multiple quantum well active layer comprises an InGaN quantum well layer 510 and a GaN quantum barrier layer 520 which grow periodically, and the InGaN quantum well layer is composed of a plurality of InGaN quantum well layer sublayers 5101 which are subjected to in-situ heat treatment.
In an embodiment of the present application, the InGaN quantum well layer 510 provided herein may have a thickness ranging from 1nm to 5nm, inclusive; the thickness range of the GaN quantum barrier layer 520 provided by the present application may be 3nm to 30nm, inclusive; the InGaN quantum well layer sublayers 5101 may have a thickness in a range of 0.5nm to 2.5nm, inclusive;
in an embodiment of the present application, the multiple quantum well active layer provided by the present application may first grow a GaN quantum barrier layer, and finally end with the growth of the GaN quantum barrier layer, specifically, as shown in fig. 5, the growing of the multiple quantum well active layer on the stress release layer includes:
s31: growing a GaN quantum barrier layer on the stress release layer;
s32: growing an InGaN quantum well layer on the GaN quantum barrier layer, wherein the InGaN quantum well layer is composed of a plurality of InGaN quantum well layer sub-layers subjected to in-situ heat treatment, and the number of the InGaN quantum well layer sub-layers is at least 2;
s33: judging whether the number of InGaN quantum well layers reaches a preset number;
s34: if the number of layers does not reach the preset number of layers, repeating the cycle to alternately grow the GaN quantum barrier layer and the InGaN quantum well layer on the topmost InGaN quantum well layer until the preset number of layers is reached.
S35: and if the number of layers reaches a preset number, growing a GaN quantum barrier layer on the InGaN quantum well layer at the topmost layer to obtain a multi-quantum well active layer.
The method for growing the InGaN quantum well layer on the GaN quantum barrier layer specifically comprises the following steps:
s321: growing an InGaN quantum well layer sublayer on the GaN quantum barrier layer to obtain a first InGaN quantum well layer sublayer;
s322: growing an InGaN quantum well layer sub-layer on the first InGaN quantum well layer sub-layer to obtain a second InGaN quantum well layer sub-layer;
s323: judging whether the number of layers of the InGaN quantum well layer sub-layer reaches a preset number of layers or not;
s324: if the number of layers does not reach the preset number of layers, repeatedly growing InGaN quantum well layer sub-layers on the second InGaN quantum well layer sub-layer until the number of layers reaches the preset number of layers;
s325: and if the number of layers reaches a preset number, obtaining the InGaN quantum well layer.
Growing an InGaN quantum well layer sublayer on the GaN quantum barrier layer to obtain a first InGaN quantum well layer sublayer, and specifically comprising the following steps:
and under a preset gas atmosphere, starting the input of an In source and a Ga source on the GaN quantum barrier layer, controlling the temperature to be at a first preset temperature, stopping the input of the In source and the Ga source after a first preset time, maintaining the temperature at the first preset temperature, and obtaining a first InGaN quantum well layer sublayer after a second preset time.
In an embodiment of the application, the preset number of layers of the InGaN quantum well layer is 3, the number of layers of the GaN quantum barrier layer is 4 because the GaN quantum barrier layer and the InGaN quantum well layer alternately grow periodically, and meanwhile, each InGaN quantum well layer consists of 4 InGaN quantum well layer sublayers subjected to in-situ heat treatment, first, a first GaN quantum barrier layer grows on the stress release layer, and the primary carrier gas is H2Introducing Ga source and ammonia gas in the atmosphere, growing a GaN quantum barrier layer with the thickness range of 8-15 nm and including end points, growing the GaN quantum barrier layer in the reaction chamber at 800-950 ℃ including the end points, growing a first InGaN quantum well layer after growing the GaN quantum barrier layer, and switching the main carrier gas to be N and reducing the growth temperature in the reaction chamber to 600-800 ℃ including the end points2Simultaneously introducing a Ga source, an In source and ammonia gas, stopping the input of the In source and the Ga source after 12s-60s, maintaining the temperature at 600-800 ℃, and after 5s-60s, specifically, 20s In the embodiment, obtaining a first InGaN quantum well layer sublayer, and growing a second InGaN quantum well layer on the first InGaN quantum well layer sublayer againAnd (4) until the number of the InGaN quantum well layer sublayers is 4, and at the moment, the growth of the first InGaN quantum well layer is finished.
And sequentially growing a second GaN quantum barrier layer, a second InGaN quantum well layer, a third GaN quantum barrier layer, a third InGaN quantum well layer and a fourth GaN quantum barrier layer on the first InGaN quantum well layer to obtain a multi-quantum well active layer on the stress release layer.
More specifically, In the process of growing the sub-layers of the multi-layer InGaN quantum well layer, the input of an In source and an Ga source is stopped, the temperature is maintained at the first preset temperature, after the second preset time, most of C, O and other impurities In the InGaN epitaxial material are decomposed and removed In the heat treatment process, and because the epitaxial growth is interrupted In the In-situ heat treatment, namely the In-situ heat annealing is carried out on the surface of the sub-layer of the InGaN quantum well layer, the InGaN crystal lattice with the original poor crystal lattice quality is promoted to be fully recombined and the built-In stress of the material is released as much as possible, so that the crystal lattice quality of the InGaN quantum well layer is integrally improved
The preset gas atmosphere is nitrogen atmosphere or nitrogen/hydrogen mixed atmosphere.
The first preset temperature is 600-800 ℃.
The first preset time is 12s-60s, the second preset time is 5s-60s, and the second preset time is a fixed value in the growth process of the same LED epitaxial structure. It should be noted that, in the process of repeatedly performing the heat treatment for a plurality of times, the second preset time is kept consistent. Further ensuring the uniform heat treatment effect and improving the material performance.
Referring to fig. 7, corresponding to step S32, the InGaN quantum well layer structure is schematically illustrated. And growing an InGaN quantum well layer on the GaN quantum barrier layer.
Referring to fig. 8, an electron blocking layer 600, a P-type hole injection layer 700, and an ohmic contact layer 800 are sequentially grown on the multiple quantum well active layer 500, corresponding to step S4.
In an embodiment of the present application, the electron blocking layer provided in the present application may be an AlGaN electron blocking layer, and the thickness of the AlGaN electron blocking layer may range from 10nm to 100nm, inclusive; the P-type hole injection layer may be a P-type GaN layer, and may have a thickness ranging from 5nm to 500nm, inclusive; and, the ohmic contact layer may have a thickness ranging from 1nm to 100nm, inclusive.
In a second aspect, the present application provides an in situ heat treatment based LED epitaxial structure, comprising:
a substrate;
the buffer layer, the N-type electron injection layer, the stress release layer, the multi-quantum well active layer electron barrier layer, the P-type hole injection layer and the ohmic contact layer are sequentially arranged from bottom to top on the substrate;
the active layer of the multi-quantum well comprises GaN quantum barrier layers and InGaN quantum well layers which alternately grow periodically, and the InGaN quantum well layer consists of a plurality of InGaN quantum well layer sublayers;
the embodiment of the application provides an LED epitaxial structure based on an in-situ heat treatment method and a growth method thereof, wherein the method comprises the following steps: the method comprises the steps of providing a substrate, sequentially growing a buffer layer and an N-type electron injection layer on the substrate, growing a stress release layer on the N-type electron injection layer, wherein the stress release layer is formed by combining one or more of AlGaN, InGaN or GaN, growing a multi-quantum well active layer on the stress release layer, the multi-quantum well active layer comprises an InGaN quantum well layer and a GaN quantum barrier layer which grow periodically, the InGaN quantum well layer is composed of a plurality of InGaN quantum well layer sublayers which undergo in-situ heat treatment, and sequentially growing an electron barrier layer, a P-type hole injection layer and an ohmic contact layer on the multi-quantum well active layer.
As can be seen from the above, in the technical solution provided in the embodiment of the present application, a multiple quantum well active layer is grown on the stress release layer, the multiple quantum well active layer includes an InGaN quantum well layer and a GaN quantum barrier layer which are periodically grown, and the InGaN quantum well layer is composed of a plurality of InGaN quantum well layer sublayers; most of C, O and other impurities In the InGaN epitaxial material are decomposed and removed In the heat treatment process through multiple In-situ heat treatments, and because the epitaxial growth is interrupted during the In-situ heat treatments, namely the In-situ heat annealing is carried out on the surface of the epitaxial InGaN material, the InGaN crystal lattice with poor crystal lattice quality is promoted to be fully recombined and the built-In stress of the material is released as much as possible, so that the crystal lattice quality of the InGaN quantum well layer is integrally improved, and the luminous efficiency of the GaN-based LED with the high In component is finally greatly improved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A growth method of an LED epitaxial structure based on an in-situ heat treatment method is characterized by comprising the following steps:
sequentially growing a buffer layer and an N-type electron injection layer on a substrate;
growing a stress release layer on the N-type electron injection layer;
growing a multi-quantum well active layer on the stress release layer, wherein the multi-quantum well active layer comprises GaN quantum barrier layers and InGaN quantum well layers which alternately grow periodically, and the InGaN quantum well layer consists of a plurality of InGaN quantum well layer sublayers;
and sequentially growing an electron blocking layer, a P-type hole injection layer and an ohmic contact layer on the multi-quantum well active layer.
2. The growing method of the LED epitaxial structure based on the in-situ heat treatment method according to claim 1, wherein the step of growing the multiple quantum well active layer on the stress relief layer specifically comprises the following steps:
growing a GaN quantum barrier layer on the stress release layer;
growing an InGaN quantum well layer on the GaN quantum barrier layer, wherein the InGaN quantum well layer is composed of a plurality of InGaN quantum well layer sub-layers subjected to in-situ heat treatment, and the number of the InGaN quantum well layer sub-layers is at least 2;
judging whether the number of InGaN quantum well layers reaches a preset number;
if the number of layers does not reach the preset number of layers, alternately growing a GaN quantum barrier layer and an InGaN quantum well layer on the InGaN quantum well layer at the topmost end in a repeated cycle until the preset number of layers is reached;
and if the number of layers reaches a preset number, growing a GaN quantum barrier layer on the InGaN quantum well layer at the topmost layer to obtain a multi-quantum well active layer.
3. The growing method of the LED epitaxial structure based on the in-situ heat treatment method of claim 2, wherein the InGaN quantum well layer is grown on the GaN quantum barrier layer, and the method specifically comprises the following steps:
growing an InGaN quantum well layer sublayer on the GaN quantum barrier layer to obtain a first InGaN quantum well layer sublayer;
growing an InGaN quantum well layer sub-layer on the first InGaN quantum well layer sub-layer to obtain a second InGaN quantum well layer sub-layer;
judging whether the number of layers of the InGaN quantum well layer sub-layer reaches a preset number of layers or not;
if the number of layers does not reach the preset number of layers, repeatedly growing InGaN quantum well layer sub-layers on the second InGaN quantum well layer sub-layer until the number of layers reaches the preset number of layers;
and if the number of layers reaches a preset number, obtaining the InGaN quantum well layer.
4. The method for growing an LED epitaxial structure based on an in situ heat treatment process according to claim 3,
the InGaN quantum well layer sub-layer growing on the GaN quantum barrier layer specifically comprises the following steps:
and under a preset gas atmosphere, starting the input of an In source and a Ga source on the GaN quantum barrier layer, controlling the temperature to be at a first preset temperature, stopping the input of the In source and the Ga source after a first preset time, maintaining the temperature at the first preset temperature, and obtaining an InGaN quantum well layer sublayer after a second preset time.
5. The method for growing the LED epitaxial structure based on the in-situ heat treatment method of claim 4, wherein the predetermined gas atmosphere is a nitrogen atmosphere or a nitrogen/hydrogen mixed atmosphere.
6. The method for growing the LED epitaxial structure based on the in-situ heat treatment method of claim 5, wherein the first preset temperature is between 600 ℃ and 800 ℃.
7. The method as claimed in claim 6, wherein the first predetermined time is between 12s and 60s, the second predetermined time is between 5s and 60s, and the second predetermined time is a fixed value during the growth of the same LED epitaxial structure.
8. An in-situ heat treatment process-based LED epitaxial structure, comprising:
a substrate;
the buffer layer, the N-type electron injection layer, the stress release layer, the multi-quantum well active layer electron barrier layer, the P-type hole injection layer and the ohmic contact layer are sequentially arranged from bottom to top on the substrate;
the active layer of the multi-quantum well comprises GaN quantum barrier layers and InGaN quantum well layers which alternately grow periodically, and the InGaN quantum well layers are composed of a plurality of InGaN quantum well layer sub-layers.
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