CN101901760B - MOCVD growing method of polar c-plane GaN based on c-plane SiC substrate - Google Patents
MOCVD growing method of polar c-plane GaN based on c-plane SiC substrate Download PDFInfo
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Abstract
The invention discloses a growing method of a polar c-plane GaN film based on a c-plane SiC substrate, which mainly solves the problem of poor material quality in the conventional polar c-plane GaN material growth. The growing method comprises the following growing steps: (1) arranging a c-plane Al2O2 substrate in an MOCVD reaction chamber, and carrying out heat treatment on the substrate; (2) on the c-plane Al2O3 substrate, growing a low-temperature unstressed AlInN layer which has the thickness of 100-300 nm and the temperature of 700 DEG C; (3) on the low-temperature unstressed AlInN layer, growing a high-temperature GaN layer which has the thickness of 1000-2000 nm and the temperature of 950-1100 DEG C; (4) growing a TiN layer of 1-10 nm on the high-temperature GaN layer; (5) on the TiN layer, growing a polar c-plane GaN layer which has the thickness of 2000-5000 nm and the temperature of 950-1100 DEG C; (6) on the polar c-plane GaN layer, growing a TiN layer which has the thickness of 1-10 nm; and (7) on the TiN layer, growing a polar c-plane GaN layer which has the thickness of 2000-5000 nm and the temperature of 950-1100 DEG C. The invention has the advantages of simple process and low defect, and can be used for manufacturing polar c-plane GaN light-emitting diodes and high electron mobility transistors.
Description
Technical field
The invention belongs to microelectronics technology; The growing method that relates to semi-conducting material; The metallo-organic compound chemical vapor deposition MOCVD growing method of c surface GaN semi-conducting material on particularly a kind of c face SiC substrate can be used for making the semiconductor device of c surface GaN base.
Technical background
Semi-conducting materials such as GaN is basic, GaAs is basic, InP base, their energy gap differs greatly, so people utilize these compound semiconductor materials to form various heterostructures usually.Because there is bigger difference in the energy gap of the compound semiconductor materials of heterojunction boundary both sides in heterojunction, makes these heterostructures have a common feature, promptly near heterojunction boundary, produce a SQW.For the heterojunction of forming by these compound semiconductor materials; People are through mixing to material; Perhaps utilize the characteristics such as polarity effect of material, can in quantum well, produce the two-dimensional electron gas of high concentration, this two-dimensional electron gas is made up of a large amount of electric charge carriers.But because the GaN quality of materials is relatively poor, interface roughness is bigger simultaneously, and the quality of materials of c face GaN also has very big raising space.C face SiC backing material because and c face GaN material between have littler lattice mismatch; Can be on c face SiC substrate the base plate and then the growth heterojunction material of growing GaN; But very high thermal mismatching is still arranged between SiC substrate and the GaN, and the Grown GaN quality of materials is still very poor.
In order to reduce defective, the c surface GaN epitaxial loayer of growing high-quality on c face SiC substrate, many researchers have adopted different growing methods.1998; Tetsu Kachi; Adopted the method for InN nucleating layer Deng the people, referring to A new buffer layer for high quality GaN growth by metalorganic vapor phase epitaxy, APPLIED PHYSICS LETTERS V72 p 704-706 1998.But the fault in material density of this method growth is still very high; 2009; Z.Chen; Adopt AlGaN to insert the growth pattern of layer Deng the people; The polarity c face GaN material of on c face SiC substrate, having grown is referring to Growth of AlGaN/GaN heteroiunction field effect transistors on semiinsulating GaN using an AlGaN interlayer, APPLIED PHYSICS LETTERS V94 p112108 2009.But the quality of materials of this method growth is still very poor, and the stress in the material is bigger.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, a kind of c surface GaN growth for Thin Film method based on c face SiC substrate is provided, improve the c face GaN film quality, base plate is provided for making high-performance c surface GaN light emitting diode and heterojunction.
Realize that the object of the invention key problem in technology is: adopt two step TiN to insert the mode of layer, growth regulation one deck TiN layer successively on c face SiC substrate, GaN nucleating layer, c face GaN resilient coating, second layer TiN layer, c face GaN epitaxial loayer.Performing step comprises as follows:
(1) c face SiC substrate is placed metal organic chemical vapor deposition MOCVD reative cell, and feed the mist of hydrogen and ammonia to reative cell, substrate base is heat-treated, the vacuum degree of reative cell is less than 2 * 10
-2Torr, substrate heating temperature are 900-1200 ℃, and the time is 5-10min, and chamber pressure is 20-760Torr;
(2) the Ti metal level of growth regulation one deck 1-10nm on c face SiC substrate, and this Ti metal level is carried out nitrogenize form ground floor TiN layer;
(3) growth thickness is 20-100nm on ground floor TiN layer, and temperature is 550-650 ℃ a low temperature GaN nucleating layer;
(4) growth thickness is 2000-3000nm on low temperature GaN nucleating layer, and temperature is 950-1100 ℃ a c face GaN resilient coating;
(5) the Ti metal level of growth second layer 1-10nm on c face GaN resilient coating, and this Ti metal level is carried out nitrogenize form second layer TiN layer;
(6) growth thickness is 2000-5000nm on second layer TiN layer, and temperature is 950-1100 ℃ a GaN epitaxial loayer.
The present invention has following advantage:
1. owing to adopt the used TiN of the present invention to insert layer, the defect concentration in the material reduces greatly.
2. owing to adopt the used TiN of the present invention to insert layer, the stress in the material reduces greatly.
Technical scheme of the present invention and effect can further specify through following accompanying drawing and embodiment.
Description of drawings
Fig. 1 is a c surface GaN film growth flow chart of the present invention;
Fig. 2 is a c surface GaN film generalized section of the present invention.
Embodiment
With reference to Fig. 1, the present invention provides following embodiment:
Embodiment 1, and performing step of the present invention is following:
Step 1 is heat-treated substrate base.
C face SiC substrate is placed metal organic chemical vapor deposition MOCVD reative cell, and feeds the mist of hydrogen and ammonia to reative cell, in the vacuum degree of reative cell less than 2 * 10
-2Torr, substrate heating temperature are 1100 ℃, and the time is 8min, and chamber pressure is under the condition of 40Torr, and substrate base is heat-treated.
Step 2, growth regulation one deck TiN inserts layer.
It is 1000 ℃ that substrate base temperature after the heat treatment is raise; To SiC substrate surface deposition thickness is the Ti layer of 5nm; Be in the ammonia environment of 4000sccm at flow then, nitrogenize formed the thick TiN layer of 5nm in 8 minutes under keep-uping pressure to the condition of 40Torr and 1000 ℃.
Step 3, growth polarity c face GaN nucleating layer.
The substrate temperature of the TiN layer of having grown is reduced to 600 ℃; Feeding flow to reative cell is that gallium source, the flow of 30 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 4000sccm, and growth thickness is the c surface GaN nucleating layer of 30nm under keep-uping pressure to the condition of 40Torr.
Step 4, growth polarity c face GaN resilient coating.
With the substrate temperature rising of the GaN nucleating layer of having grown is 1000 ℃; Feeding flow to reative cell is that gallium source, the flow of 5 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 4000sccm, and growth thickness is the c surface GaN resilient coating of 2500nm under keep-uping pressure to the condition of 40Torr.
Step 5, growth second layer TiN inserts layer.
The substrate temperature of the c surface GaN resilient coating of having grown is remained on 1000 ℃; To GaN surface deposition thickness is the Ti layer of 5nm; Be in the ammonia environment of 4000sccm at flow then, nitrogenize formed the thick second layer TiN layer of 5nm in 8 minutes under keep-uping pressure to the condition of 40Torr and 1000 ℃.
Step 6, growth polarity c face GaN epitaxial loayer.
The substrate temperature of the second layer TiN layer of having grown is remained on 1000 ℃; Feeding flow to reative cell is that gallium source, the flow of 40 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 4000sccm, and growth thickness is the c surface GaN epitaxial loayer of 2500nm under keep-uping pressure to the condition of 40Torr.
Step 7 will be taken out from the MOCVD reative cell through the c surface GaN material of said process growth.
Grow the c face GaN film structure of polarity through above-mentioned steps; Of Fig. 2, it is followed successively by the GaN nucleating layer of c face SiC substrate that thickness is 200-500 μ m, ground floor TiN layer that thickness is 30nm, 30nm that thickness is, the c surface GaN resilient coating that thickness is 2500nm, the second layer TiN layer that thickness is 5nm, the c surface GaN epitaxial loayer that thickness is 2500nm from bottom to top.
Embodiment 2:
Performing step of the present invention is following:
Steps A is heat-treated substrate base.
C face SiC substrate is placed metal organic chemical vapor deposition MOCVD reative cell, and feeds the mist of hydrogen and ammonia to reative cell, in the vacuum degree of reative cell less than 2 * 10
-2Torr, substrate heating temperature are 1100 ℃, and the time is 8min, and chamber pressure is under the condition of 40Torr, and substrate base is heat-treated.
Step B, growth regulation one deck TiN insert layer.
It is 900 ℃ that substrate base temperature after the heat treatment is raise; To SiC substrate surface deposition thickness is the Ti layer of 1nm; Be in the ammonia environment of 3000sccm at flow then, nitrogenize formed the thick ground floor TiN layer of 1nm in 5 minutes under keep-uping pressure to the condition of 20Torr and 900 ℃.
Step C, growth polarity c face GaN nucleating layer.
The substrate temperature of the ground floor TiN that grown is reduced to 550 ℃; Feeding flow to reative cell is that gallium source, the flow of 5 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 3000sccm, and growth thickness is the c surface GaN nucleating layer of 20nm under keep-uping pressure to the condition of 20Torr.
Step D, growth polarity c face GaN resilient coating.
With the substrate temperature rising of the GaN nucleating layer of having grown is 950 ℃; Feeding flow to reative cell is that gallium source, the flow of 5 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 3000sccm, and growth thickness is the c surface GaN resilient coating of 2000nm under keep-uping pressure to the condition of 20Torr.
Step e, growth second layer TiN layer.
With the substrate surface deposition thickness of the c surface GaN resilient coating of having grown is the second layer Ti layer of 1nm; Be in the ammonia environment of 3000sccm at flow then, nitrogenize formed the thick second layer TiN layer of 1nm in 5 minutes under keep-uping pressure to the condition of 20Torr and 900 ℃.
Step F, growth polarity c face GaN epitaxial loayer.
With the substrate temperature rising of the second layer TiN layer of having grown is 950 ℃; Feeding flow to reative cell is that gallium source, the flow of 5 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 3000sccm, and growth thickness is the c surface GaN epitaxial loayer of 2000nm under keep-uping pressure to the condition of 20Torr.
Step G will take out from the MOCVD reative cell through the c surface GaN material of said process growth.
The c surface GaN membrane structure that grows through above-mentioned steps; Of Fig. 2, it is followed successively by the c face SiC substrate that thickness is 200-500 μ m, the TiN layer that thickness is 1nm, the GaN nucleating layer that thickness is 20nm, the c surface GaN resilient coating that thickness is 2000nm, the TiN layer that thickness is 1nm, the c surface GaN epitaxial loayer that thickness is 2000nm from bottom to top.
Embodiment 3:
Performing step of the present invention is following:
Step 1 is heat-treated substrate base.
C surface SiC substrate is placed metal organic chemical vapor deposition MOCVD reative cell, and feeds the mist of hydrogen and ammonia to reative cell, in the vacuum degree of reative cell less than 2 * 10
-2Torr, substrate heating temperature are 1200 ℃, and the time is 10min, and chamber pressure is under the condition of 760Torr, and substrate base is heat-treated.
Step 2, growth regulation one deck TiN inserts layer.
It is 1200 ℃ that substrate base temperature after the heat treatment is raise; To GaN surface deposition thickness is the Ti layer of 10nm; Be in the ammonia environment of 10000sccm at flow then, nitrogenize formed the thick TiN layer of 10nm in 10 minutes under keep-uping pressure to the condition of 760Torr and 1200 ℃.
Step 3, growth polarity c face GaN nucleating layer.
The substrate temperature of the TiN that grown is reduced to 650 ℃; Feeding flow to reative cell is that gallium source, the flow of 100 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 10000sccm, and growth thickness is the c surface GaN nucleating layer of 100nm under keep-uping pressure to the condition of 760Torr.
Step 4, growth polarity c face GaN resilient coating.
With the substrate temperature rising of the GaN nucleating layer of having grown is 1100 ℃; Feeding flow to reative cell is that gallium source, the flow of 100 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 10000sccm, and growth thickness is the c surface GaN layer of 3000nm under keep-uping pressure to the condition of 760Torr.
Step 5, growth second layer TiN layer.
With the substrate surface deposition thickness of the c surface GaN layer of having grown is the Ti layer of 10nm, is in the ammonia environment of 10000sccm at flow then, and nitrogenize formed the thick TiN layer of 10nm in 10 minutes under keep-uping pressure to the condition of 760Torr and 1200 ℃.
Step 6, growth polarity c face GaN epitaxial loayer.
With the substrate temperature rising of the TiN layer of having grown is 1100 ℃; Feeding flow to reative cell is that gallium source, the flow of 100 μ mol/min is that 1200sccm hydrogen and flow are the ammonia of 10000sccm, and growth thickness is the c surface GaN epitaxial loayer of 5000nm under keep-uping pressure to the condition of 760Torr.
Step 7 will be taken out from the MOCVD reative cell through the c surface GaN material of said process growth.
The c surface GaN membrane structure that grows through above-mentioned steps; Of Fig. 2, it is followed successively by the c face SiC substrate that thickness is 200-500 μ m, the ground floor TiN layer that thickness is 10nm, the GaN nucleating layer that thickness is 100nm, the c surface GaN resilient coating that thickness is 3000nm, the second layer TiN layer that thickness is 10nm, the c surface GaN epitaxial loayer that thickness is 5000nm from bottom to top.
To those skilled in the art; After understanding content of the present invention and principle; Can be under the situation that does not deviate from the principle and scope of the present invention; Carry out various corrections and change on form and the details according to the method for the invention, but these are based on correction of the present invention with change still within claim protection range of the present invention.
Claims (10)
1. the MOCVD growing method based on the c surface GaN film of c face SiC substrate comprises the steps:
(1) c face SiC substrate is placed metal organic chemical vapor deposition MOCVD reative cell, and feed the mist of hydrogen and ammonia to reative cell, substrate base is heat-treated, the vacuum degree of reative cell is less than 2 * 10
-2Torr, substrate heating temperature are 900-1200 ℃, and the time is 5-10min, and chamber pressure is 20-760Torr;
(2) growth 1-10nm thick Ti metal level on the c face SiC substrate after the heat treatment, and this Ti metal level is carried out nitrogenize form ground floor TiN layer;
(3) growth thickness is 20-100nm on ground floor TiN layer, and temperature is 550-650 ℃ a low temperature GaN nucleating layer;
(4) growth thickness is 2000-3000nm on low temperature GaN nucleating layer, and temperature is 950-1100 ℃ a c face GaN resilient coating;
(5) growth 1-10nm thick Ti metal level on c face GaN resilient coating, and this Ti metal level is carried out nitrogenize form second layer TiN layer;
(6) growth thickness is 2000-5000nm on second layer TiN layer, and temperature is 950-1100 ℃ a GaN epitaxial loayer.
2. the MOCVD growing method of c surface GaN film according to claim 1; Wherein step (2) is described carries out nitrogenize formation ground floor TiN layer to the Ti metal level; Be to be 900-1200 ℃ in temperature; Time is 5-10min, and pressure is 20-760Torr, and ammonia flow is to form under the process conditions of 3000-10000sccm.
3. the MOCVD growing method of c surface GaN film according to claim 1; The described nucleating layer of step (3) wherein; Be to be 20-760Torr at pressure, the gallium source flux is 5-100 μ mol/min, and ammonia flow is that growth forms under the process conditions of 3000-10000sccm.
4. the MOCVD growing method of c surface GaN film according to claim 1; The described resilient coating of step (4) wherein; Be to be 20-760Torr at pressure, the gallium source flux is 5-100 μ mol/min, and ammonia flow is that growth forms under the process conditions of 3000-10000sccm.
5. the MOCVD growing method of c surface GaN film according to claim 1; Wherein step (5) is described carries out nitrogenize formation second layer TiN layer to the Ti metal level; Be to be 900-1200 ℃ in temperature; Time is 5-10min, and pressure is 20-760Torr, and ammonia flow is to form under the condition of 3000-10000sccm.
6. the MOCVD growing method of c surface GaN film according to claim 1; The described epitaxial loayer of step (6) wherein; Be to be 20-760Torr at pressure, the gallium source flux is 5-100 μ mol/min, and ammonia flow is that growth forms under the process conditions of 3000-10000sccm.
7. c surface GaN film based on c face SiC substrate; Comprise successively from bottom to top: c face SiC substrate, GaN nucleating layer, c face GaN resilient coating and c face GaN epitaxial loayer is characterized in that being respectively equipped with on c face SiC substrate and the c face GaN resilient coating TiN insertion layer that nitrogenize forms.
8. according to the said c surface GaN film of claim 7, it is characterized in that: it is 1-10nm that described TiN inserts layer thickness.
9. according to the said c surface GaN film of claim 7, it is characterized in that: described GaN buffer layer thickness is 2000-3000nm.
10. according to the said c surface GaN film of claim 7, it is characterized in that: described GaN epitaxy layer thickness is 2000-5000nm.
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Effective date of registration: 20161206 Address after: 650221 Yunnan city of Kunming province Dabanqiao Street office office building No. 7 room 7-114 Patentee after: Yunnan Hui Hui Electronic Technology Co., Ltd. Address before: Xi'an City, Shaanxi province Taibai Road 710071 No. 2 Patentee before: Xidian University |