CN103311100A - Production method of InN semiconductor component with nonpolar m plane GaN buffer layer - Google Patents
Production method of InN semiconductor component with nonpolar m plane GaN buffer layer Download PDFInfo
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- CN103311100A CN103311100A CN2013102382684A CN201310238268A CN103311100A CN 103311100 A CN103311100 A CN 103311100A CN 2013102382684 A CN2013102382684 A CN 2013102382684A CN 201310238268 A CN201310238268 A CN 201310238268A CN 103311100 A CN103311100 A CN 103311100A
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Abstract
The invention discloses a production method of an InN semiconductor component with a nonpolar m plane GaN buffer layer. The production method includes (1) placing a gamma plane LiAlO2 substrate in an MOCVD (metal organic chemical vapor deposition) reaction chamber, and heating the substrate; (2) generating a low-temperature AlN nucleation layer with the thickness of 30-100nm at the temperature between 500-600 DEG C on the gamma plane LiAlO2 substrate; (3) generating a high-temperature AlN layer with the thickness of 1000-5000nm at the temperature between 900-1050 DEG C on the low-temperature AlN nucleation layer; (4) generating an m plane GaN buffer layer with the thickness of 1000-5000nm at the temperature between 900-1050 DEG C on the high-temperature AlN layer; (5) depositing an SiNx inserted layer of 3-9s on the buffer layer through PECVD (plasma enhanced chemical vapor deposition); (6) placing the substrate with the inserted layer deposited on in the MOCVD reaction chamber, secondary generating an m plane GaN buffer layer with the thickness of 2000-5000nm at the temperature between1000-1100 DEG C; (7) generating InN materials with the thickness of 15-30nm, indium source flow of 90-250Mu mol/min and ammonia flow of 1000-5000sccm on the buffer layer. The production method has the advantages of high quality and smooth surface, and can be used for producing InN -based light emitting components.
Description
Technical field
The invention belongs to microelectronics technology, relate to the growing method of semi-conducting material, particularly a kind of SiN based on the PECVD deposit
xThe m face GaN of insert layer is as resilient coating, and the metallo-organic compound chemical vapor deposition MOVCD growing method of the InN semi-conducting material of growth thereon can be used for making the semiconductor device of InN base.
Technical background
The semi-conducting material that is formed by III family element and group Ⅴ element, it is the Ⅲ-Ⅴ compound semiconductor material, such as semi-conducting materials such as GaN, GaAs, their energy gap often differs greatly, therefore people utilize these Ⅲ-Ⅴ compound semiconductor materials to form various heterostructures usually, in order to do various electronic devices.And compare InN base electron device speed with GaN faster, and maximum electron mobility theoretical under its room temperature is 4400cm
2V
-1S
-1, much larger than the 1000cm of GaN
2V
-1S
-1The alloy of InN and GaN can extend to infrared region with the light emitting region of GaN base LED always from the ultra-violet (UV) band simultaneously.Yet the InN monocrystalline is difficult to obtain, and only has by the heteroepitaxial growth method to obtain.And epitaxial growth is difficult to avoid and the Lattice Matching of substrate and the problem of heat coupling.So growing high-quality InN material is the key of making above-mentioned photoelectric device.
Show roughness in order to improve the crystalline quality reduction, many researchers have adopted different growing methods.2004, Singha P in Sapphire Substrate by the GaN nucleating layer InN sill of having grown.Referring to Structural and optical characterization of InN layers grown by MOCVD, Superlattice and Microstructures V 81 p5372004.But this method is because just at the nucleating layer InN that grown, thereby causes the material crystalline quality relatively poor, and surface roughness is higher.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned prior art, provide a kind of based on γ face LiAlO
2The non-polar m-surface GaN of substrate is as the growing method of buffer growth InN, to improve surface topography and the crystalline quality of InN.
One aspect of the present invention relates to a kind of preparation method who contains the InN semiconductor device of non-polar m-surface GaN resilient coating, and described preparation method comprises the steps:
(1) with γ face LiAlO
2Substrate base places metal organic chemical vapor deposition MOCVD reative cell, and passes into hydrogen to reative cell, and substrate is heat-treated, and the initial vacuum degree of reative cell is less than 2 * 10
-2Torr, substrate heating temperature are 800-1000 ℃, and the time is 3-5min, pass into that chamber pressure is 10-700Torr after the gaseous mixture;
(2) in the situation that temperature is 500-600 ℃, the γ face LiAlO after heat treatment
2Growth thickness is the low temperature AI N nucleating layer of 30-100nm on the substrate base;
(3) in the situation that temperature is 900-1050 ℃, growth thickness is 60-200nm high temperature AlN layer on described low temperature AI N nucleating layer;
(4) in the situation that temperature is 900-1050 ℃, growth thickness is 1000-5000nm non-polar m-surface GaN resilient coating on described high temperature AlN layer;
(5) will the grow m face GaN material of resilient coating is put into plasma enhanced CVD (PECVD) reative cell, and passes into ammonia and silane in the reative cell at 200-250 ℃, and pressure is that reaction generates layer of sin under the 600-800mTorr
xAs the insert layer of material, the reaction time is 3-9s;
(6) SiN is crossed in the PECVD deposit
xMaterial place the MOCVD reative cell, in the situation that temperature is 1000-1100 ℃, continued growth thickness is the non-polar m-surface GaN resilient coating of 2000-5000nm.
(7) pass into indium source and ammonia, growth thickness is the 15-30nmInN base on resilient coating, and wherein the indium source flux is 80-160 μ mol/min, and ammonia flow is 1000-5000sccm.
In a preferred embodiment of the present invention, wherein the described process conditions of step (2) are as follows:
Pressure: 10-700Torr; Aluminium source flux: 10-120 μ mol/min;
Ammonia flow: 1000-10000sccm.
In a preferred embodiment of the present invention, wherein the described process conditions of step (3) are as follows:
Pressure: 10-700Torr; Aluminium source flux: 10-120 μ mol/min;
Ammonia flow: 1000-10000sccm.
In a preferred embodiment of the present invention, wherein the described process conditions of step (4) are as follows:
Pressure: 10-700Torr; Gallium source flux: 40-120 μ mol/min;
Ammonia flow: 1000-10000sccm.
In a preferred embodiment of the present invention, wherein the described process conditions of step (5) are as follows:
Growth temperature is 200-250 ℃; Growth pressure is 600-800mTorr;
Silane flow rate is the mixed gas of the SiH4/N2 of 200sccm; Ammonia flow is 2sccm.
In a preferred embodiment of the present invention, wherein the described process conditions of step (6) are as follows:
Pressure: 10-700Torr; Gallium source flux: 40-200 μ mol/min;
Ammonia flow: 1000-5000sccm.
In a preferred embodiment of the present invention, wherein the described process conditions of step (7) are as follows:
Growth temperature is 400-600 ℃; Growth pressure is 80-160Torr;
The indium source flux is 30-60 μ mol/min; Ammonia flow is 1000-5000sccm.
In a preferred embodiment of the present invention, described aluminium source is selected from trimethyl aluminium.
In another preferred embodiment of the present invention, described gallium source is selected from triethyl-gallium.
In another preferred embodiment of the present invention, described indium source is selected from trimethyl indium.
The present invention has following advantage:
1. because PECVD has inserted SiN
xInsert layer is so that the non-polar m-surface GaN resilient coating quality of diauxic growth is better, thereby the InN surface topography that makes it rear growth is improved.
2. because PECVD has inserted SiN
xInsert layer is so that the non-polar m-surface GaN resilient coating quality of diauxic growth is better, thereby the InN crystalline quality that makes it rear growth is improved.
Technical scheme of the present invention and effect can further specify by the following drawings and embodiment.
Description of drawings
Fig. 1 is γ face LiAlO of the present invention
2InN growth flow chart on the non-polar m-surface GaN resilient coating on the substrate;
Fig. 2 is γ face LiAlO of the present invention
2InN cross-sectional view on the non-polar m-surface GaN resilient coating on the substrate.
Fig. 3: the AFM surface topography map that does not have insert layer 10um * 10um;
Fig. 4: the AFM surface topography map that the 10um * 10um of insert layer is arranged.
Embodiment
With reference to Fig. 1, the present invention provides following embodiment:
Embodiment 1:
Performing step of the present invention is as follows:
Step 1 is heat-treated substrate.
With γ face LiAlO
2Substrate base places metal organic chemical vapor deposition MOCVD reative cell, and passes into hydrogen to reative cell, in the vacuum degree of reative cell less than 2 * 10
-2Torr, substrate heating temperature are 900 ℃, and the time is 4min, and chamber pressure is under the condition of 40Torr, and substrate is heat-treated.
Step 2, the 550 ℃ of low temperature AI N nucleating layers of growing.
Underlayer temperature after the heat treatment is reduced to 550 ℃, passing into aluminium source, the flow that flow is 20 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1500sccm, is that growth thickness is the low temperature AI N nucleating layer of 40nm under the condition of 40Torr keeping pressure.
Step 3, the 1000 ℃ of high temperature AlN layers of growing.
The underlayer temperature of the low temperature AI N nucleating layer of having grown is elevated to 1000 ℃, passing into aluminium source, the flow that flow is 20 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1500sccm, be under the condition of 40Torr keeping pressure, growth thickness is the high temperature AlN layer of 100nm.
Step 4, growing nonpolar m face GaN resilient coating.
The underlayer temperature of the high temperature AlN layer of having grown is remained on 1000 ℃, passing into gallium source, the flow that flow is 60 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1500sccm, is that growth thickness is the non-polar m-surface GaN resilient coating of 3000nm under the condition of 40Torr keeping pressure.
Step 5 uses PECVD at 240 ℃ of deposit SiN
xInsert layer.
The GaN resilient coating of will having grown is put into the PECVD reative cell, passes into the SiH that flow is 200sccm to reative cell
4/ N
2Mixed gas and flow are the ammonia of 2sccm, are deposit 5s SiN under the condition of 700mTorr keeping pressure
xInsert layer.
Step 6, diauxic growth non-polar m-surface GaN resilient coating.
The m face GaN that insert layer is crossed in the PECVD deposit puts into the MOCVD reative cell and carries out diauxic growth, temperature remains on 1050 ℃, passing into gallium source, the flow that flow is 60 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1500sccm, is that growth thickness is the non-polar m-surface GaN resilient coating of 3000nm under the condition of 40Torr keeping pressure.
Step 7, growth InN sill.
To be reduced to 530 ℃ with the GaN of growth, passing into indium source, the flow that flow is 50 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 3000sccm, is under the condition of 100Torr keeping pressure, and growth thickness is the InN sill of 25nm.
Step 8 will be taken out from the MOCVD reative cell by InN material on the non-polar m-surface GaN resilient coating of said process growth.
With reference to Fig. 2, according to InN material on the non-polar m-surface GaN resilient coating of said method making of the present invention, it is followed successively by from bottom to top: thickness is the γ face LiAlO of 200-500 μ m
2Substrate, thickness are that the AlN layer of the low temperature AI N nucleating layer of 40nm, 100nm that thickness is, non-polar m-surface GaN resilient coating, the deposition time that thickness is 3000nm are the SiN of 5s
x, insert layer thickness is the non-polar m-surface GaN resilient coating of 3000nm and the InN sill that thickness is 25nm.
After testing, there is not the XRD swing curve on the surface of insert layer to compare, there is the half-breadth of the surperficial swing curve of insert layer to be reduced to original half, the surface roughness never 1.95nm of insert layer is reduced to 0.62nm, concrete experimental data is referring to Fig. 3 and 4, as can be seen from the figure Fig. 4 stripe-shaped structure on [0001] direction is more obvious, and 4 show that more smooth stain still less with respect to Fig. 3, this explanation adds the afterwards roughness reduction of material of SiNx insert layer, and defective reduces surface topography very large improvement.
Embodiment 2:
Performing step of the present invention is as follows:
Steps A is heat-treated substrate.
With m face LiAlO
2Substrate base places metal organic chemical vapor deposition MOCVD reative cell, and passes into the mist of hydrogen and ammonia to reative cell, in the vacuum degree of reative cell less than 2 * 10
-2Torr, the substrate base heating-up temperature is 800 ℃, and the time is 3min, and chamber pressure is under the condition of 10Torr, and substrate base is heat-treated.
Step B, the 500 ℃ of low temperature AI N nucleating layers of growing.
Substrate base temperature after the heat treatment is reduced to 500 ℃, passing into aluminium source, the flow that flow is 10 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1000sccm, is that growth thickness is the low temperature AI N nucleating layer of 30nm under the condition of 10Torr keeping pressure.
Step C, growth high temperature AlN layer.
The substrate base temperature of the low temperature AI N nucleating layer of having grown is elevated to 900 ℃, passing into aluminium source, the flow that flow is 10 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1000sccm, be under the condition of 10Torr keeping pressure, growth thickness is the high temperature AlN nucleating layer of 60nm.
Step D, growing nonpolar m face GaN resilient coating.
The underlayer temperature of the high temperature AlN layer of having grown is remained on 900 ℃, passing into gallium source, the flow that flow is 40 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1000sccm, is that growth thickness is 1000nm non-polar m-surface GaN resilient coating under the condition of 10Torr keeping pressure.
Step e uses PECVD at 200 ℃ of deposit SiN
xInsert layer.
The GaN resilient coating of will having grown is put into the PECVD reative cell, passes into the SiH that flow is 200sccm to reative cell
4/ N
2Mixed gas and flow are the ammonia of 2sccm, are deposit 3s SiN under the condition of 600mTorr keeping pressure
xInsert layer.
Step F, diauxic growth non-polar m-surface GaN resilient coating.
The m face GaN resilient coating that insert layer is crossed in the PECVD deposit is put into the MOCVD reative cell and is carried out diauxic growth, temperature remains on 1000 ℃, passing into gallium source, the flow that flow is 40 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1000sccm, is that growth thickness is the non-polar m-surface GaN resilient coating of 2000nm under the condition of 10Torr keeping pressure.
Step G, growth InN sill.
To be reduced to 400 ℃ with the GaN of growth, passing into indium source, the flow that flow is 30 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 1000sccm, is under the condition of 80Torr keeping pressure, and growth thickness is the InN sill of 15nm.
Step H will take out from the MOCVD reative cell by InN material on the non-polar m-surface GaN resilient coating of said process growth.
With reference to Fig. 2, InN material on the non-polar m-surface GaN resilient coating of making according to said method of the present invention, it is followed successively by from bottom to top and is the γ face LiAlO of 200-500 μ m
2Substrate, thickness are that the AlN layer of the low temperature AI N nucleating layer of 30nm, 60nm that thickness is, non-polar m-surface GaN resilient coating, the deposition time that thickness is 1000nm are the SiN of 3s
xInsert layer, thickness are the non-polar m-surface GaN resilient coating of 2000nm and the InN sill that thickness is 15nm.
Embodiment 3:
Performing step of the present invention is as follows:
Step 1 is heat-treated substrate base.
With γ face LiAlO
2Substrate base places metal organic chemical vapor deposition MOCVD reative cell, and passes into hydrogen to reative cell, in the vacuum degree of reative cell less than 2 * 10
-2Torr, the substrate base heating-up temperature is 1000 ℃, and the time is 5min, and chamber pressure is under the condition of 700Torr, and substrate base is heat-treated.
Step 2, the 600 ℃ of low temperature AI N nucleating layers of growing.
Substrate base temperature after the heat treatment is reduced to 600 ℃, passing into aluminium source, the flow that flow is 120 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 10000sccm, is that growth thickness is the low temperature AI N nucleating layer of 100nm under the condition of 700Torr keeping pressure.
Step 3, the 1050 ℃ of high temperature AlN layers of growing.
It is 1050 ℃ that the substrate base temperature of the low temperature AI N nucleating layer of having grown is raise, passing into aluminium source, the flow that flow is 120 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 10000sccm, be under the condition of 700Torr keeping pressure, growth thickness is the high temperature AlN layer of 200nm.
Step 4, growing nonpolar m face GaN resilient coating.
The substrate base temperature of the high temperature AlN layer of having grown is remained on 1050 ℃, passing into gallium source, the flow that flow is 120 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 10000sccm, is that growth thickness is the non-polar m-surface GaN layer of 5000nm under the condition of 700Torr keeping pressure.
Step 5 uses PECVD at 250 ℃ of deposit SiN
xInsert layer.
The GaN resilient coating of will having grown is put into the PECVD reative cell, passes into the SiH that flow is 200sccm to reative cell
4/ N
2Mixed gas and flow are the ammonia of 2sccm, are deposit 9s SiN under the condition of 800mTorr keeping pressure
xInsert layer.
Step 6,
The m face GaN resilient coating that insert layer is crossed in the PECVD deposit is put into the MOCVD reative cell and is carried out diauxic growth, temperature remains on 1100 ℃, passing into gallium source, the flow that flow is 200 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 5000sccm, is that growth thickness is the non-polar m-surface GaN resilient coating of 5000nm under the condition of 700Torr keeping pressure.
Step 7, growth InN sill.
To be reduced to 600 ℃ with the GaN of growth, passing into indium source, the flow that flow is 60 μ mol/min to reative cell is that 1200sccm hydrogen and flow are the ammonia of 10000sccm, is under the condition of 160Torr keeping pressure, and growth thickness is the InN sill of 30nm
Step 8 will be taken out from the MOCVD reative cell by InN material on the non-polar GaN resilient coating of said process growth.
With reference to Fig. 2, according to InN material on the non-polar m-surface GaN resilient coating of said method making of the present invention, it is followed successively by from bottom to top: thickness is the γ face LiAlO of 200-500 μ m
2Substrate, thickness are that the AlN layer of the low temperature AI N nucleating layer of 40nm, 100nm that thickness is, non-polar m-surface GaN resilient coating, the deposition time that thickness is 3000nm are the SiN of 9s
xInsert layer, thickness are the non-polar m-surface GaN resilient coating of 3000nm and the InN sill that thickness is 30nm.。
For those skilled in the art; after understanding content of the present invention and principle; can be in the situation that do not deviate from the principle and scope of the present invention; the method according to this invention is carried out various corrections and the change on form and the details, but these are based on correction of the present invention with change still within claim protection range of the present invention.
Claims (7)
1. preparation method who contains the InN semiconductor device of non-polar m-surface GaN resilient coating, described preparation method comprises the steps:
(1) with γ face LiAlO
2Substrate base places metal organic chemical vapor deposition MOCVD reative cell, and passes into hydrogen to reative cell, and substrate is heat-treated, and the initial vacuum degree of reative cell is less than 2 * 10
- 2Torr, substrate heating temperature are 800-1000 ℃, and the time is 3-5min, pass into that chamber pressure is 10-700Torr after the gaseous mixture;
(2) in the situation that temperature is 500-600 ℃, the γ face LiAlO after heat treatment
2Growth thickness is the low temperature AI N nucleating layer of 30-100nm on the substrate base;
(3) in the situation that temperature is 900-1050 ℃, growth thickness is 60-200nm high temperature AlN layer on described low temperature AI N nucleating layer;
(4) in the situation that temperature is 900-1050 ℃, growth thickness is 1000-5000nm non-polar m-surface GaN resilient coating on described high temperature AlN layer;
(5) will the grow m face GaN material of resilient coating is put into plasma enhanced CVD (PECVD) reative cell, and passes into ammonia and silane in the reative cell at 200-250 ℃, and pressure is that reaction generates layer of sin under the 600-800mTorr
xAs the insert layer of material, the reaction time is 3-9s;
(6) SiN is crossed in the PECVD deposit
xMaterial place the MOCVD reative cell, in the situation that temperature is 1000-1100 ℃, continued growth thickness is the non-polar m-surface GaN resilient coating of 2000-5000nm.
(7) pass into indium source and ammonia, growth thickness is the 15-30nmInN base on resilient coating, and wherein the indium source flux is 80-160 μ mol/min, and ammonia flow is 1000-5000sccm.
2. preparation method according to claim 1, wherein the described process conditions of step (2) are as follows:
Pressure: 10-700Torr; Aluminium source flux: 10-120 μ mol/min;
Ammonia flow: 1000-10000sccm.
3. preparation method according to claim 1, wherein the described process conditions of step (3) are as follows:
Pressure: 10-700Torr; Aluminium source flux: 10-120 μ mol/min;
Ammonia flow: 1000-10000sccm.
4. preparation method according to claim 1, wherein the described process conditions of step (4) are as follows:
Pressure: 10-700Torr; Gallium source flux: 40-120 μ mol/min;
Ammonia flow: 1000-10000sccm.
5. preparation method according to claim 1, wherein the described process conditions of step (5) are as follows:
Growth temperature is 200-250 ℃; Growth pressure is 600-800mTorr;
Silane flow rate is the SiH of 200sccm
4/ N
2Mixed gas; Ammonia flow is 2sccm.
6. preparation method according to claim 1, wherein the described process conditions of step (6) are as follows: pressure: 10-700Torr; Gallium source flux: 40-200 μ mol/min;
Ammonia flow: 1000-5000sccm.
7. preparation method according to claim 1, wherein the described process conditions of step (7) are as follows:
Growth temperature is 400-600 ℃; Growth pressure is 80-160Torr;
The indium source flux is 30-60 μ mol/min; Ammonia flow is 1000-5000sccm.
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| CN104319233A (en) * | 2014-09-30 | 2015-01-28 | 东莞市中镓半导体科技有限公司 | InN/LT-AlN combined stress release buffer layer technology in MOCVD |
| WO2015144023A1 (en) * | 2014-03-24 | 2015-10-01 | 上海卓霖信息科技有限公司 | Non-polar blue led epitaxial wafer based on lao substrate and preparation method therefor |
| CN105098016A (en) * | 2015-08-18 | 2015-11-25 | 西安电子科技大学 | Yellow-light LED material based on gamma-surface LiAlO2 substrate and manufacturing method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015144023A1 (en) * | 2014-03-24 | 2015-10-01 | 上海卓霖信息科技有限公司 | Non-polar blue led epitaxial wafer based on lao substrate and preparation method therefor |
| US9978908B2 (en) | 2014-03-24 | 2018-05-22 | Shanghai Chiptek Semiconductor Technology Co., Ltd. | Non-polar blue light LED epitaxial wafer based on LAO substrate and preparation method thereof |
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| CN105098016A (en) * | 2015-08-18 | 2015-11-25 | 西安电子科技大学 | Yellow-light LED material based on gamma-surface LiAlO2 substrate and manufacturing method thereof |
| CN105098016B (en) * | 2015-08-18 | 2018-03-06 | 西安电子科技大学 | Based on γ faces LiAlO2Yellow light LED material and preparation method thereof on substrate |
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