CN106784227B - C surface AlN film and preparation method thereof based on the face c SiC graph substrate - Google Patents
C surface AlN film and preparation method thereof based on the face c SiC graph substrate Download PDFInfo
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- CN106784227B CN106784227B CN201710021289.9A CN201710021289A CN106784227B CN 106784227 B CN106784227 B CN 106784227B CN 201710021289 A CN201710021289 A CN 201710021289A CN 106784227 B CN106784227 B CN 106784227B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of group III and group V of the periodic system
- H01L33/32—Materials of the light emitting region containing only elements of group III and group V of the periodic system containing nitrogen
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- 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
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
Abstract
The invention discloses a kind of c surface AlN films based on the face c SiC graph substrate, mainly solve prior art processes complexity, the long and costly problem of fabrication cycle.It includes: AlN layers of c surface of the face the c SiC substrate layer of 100-500 μ m-thick, the GaN nucleating layer of 10-150nm thickness, the Al content gradually variational AlGaN layer of 1000-6000nm thickness and 500-3000nm thickness from bottom to top, wherein the surface of the face c SiC substrate layer is equipped with the substrate striped formed of being polished by diamond sand paper, to improve the quality of AlN material；The Al component of Al content gradually variational AlGaN layer is from 5% gradual change to 100%, to reduce the stress of AlN material.Preparation process of the invention is simple, shortens fabrication cycle and reduces expense cost, can be used for making the ultraviolet and deep ultraviolet semiconductor devices of c surface AlN base.
Description
Technical field
The invention belongs to microelectronics technology, in particular to a kind of preparation method of AlN film can be used for making polarity
The ultraviolet and deep ultraviolet semiconductor devices of the face c AlN base.
Technical background
III-V hi-nitride semiconductor material, such as AlN base, GaN base, InN base semiconductor material, their forbidden band are wide
Degree often differs greatly, for example AlN is 6.2eV, GaN 3.42eV, InN 0.7eV, thus people usually utilize these III-
V group iii v compound semiconductor material forms various heterojunction structures.Especially InGaN material system achieves huge on blue-ray LED
Big success, red rugged brave, the wild skys in day in 2014 and Shuji Nakamura obtain Nuo Bei because of the tremendous contribution in terms of blue-ray LED
That Physics Prize.In addition, the material of AlGaN system is since forbidden bandwidth is very big, emission wavelength very little, if adjusting Ga's and Al
Ratio can make emission wavelength cover ultraviolet and deep ultraviolet, and due to this feature, the relevant material of AlN and device are at present
Current research hotspot.The face c SiC substrate material, can be in the face c SiC due to having smaller lattice mismatch between the AlN of the face c
Growing AIN material on substrate, but still have very high thermal mismatching between SiC substrate and AlN, the AlN quality of materials of growth is still
It is very poor.
In order to reduce defect, in the c surface AlN epitaxial layer of the face c SiC substrate growth high quality, in this regard, many researchers
Using different methods, referring to Pendeo-epitaxy of stress-free AlN layer on a profiled
SiC/Si substrate,Thin Solid Films,606,74-79(2016).Although the quality of materials of these methods growth
It increases, but complex process, fabrication cycle is long and costly.
Summary of the invention
It is an object of the invention to overcome the shortcomings of above-mentioned prior art, provide a kind of based on the face c SiC graph substrate
AlN film and preparation method thereof simplifies technique to reduce stress, shortens fabrication cycle and reduces expense cost.
To achieve the above object, the present invention is based on the AlN films of the face c SiC graph substrate, from bottom to top include the following: the face c
AlN layers of SiC substrate layer, GaN nucleating layer, AlGaN layer and the face c, it is characterised in that:
The surface of the face c SiC substrate layer is equipped with the substrate striped to be formed of polishing by diamond sand paper, to improve AlN material
The quality of material,
AlGaN layer uses Al content gradually variational AlGaN layer of the Al component from 5% gradual change to 100%, to reduce AlN material
Stress.
Further, the GaN nucleating layer is with a thickness of 10-120nm.
Further, the Al content gradually variational AlGaN layer is with a thickness of 1000-6000nm.
Further, AlN layers of the face c is with a thickness of 500-3000nm.
To achieve the above object, the present invention is based on the preparation method of the c surface AlN film of the face c SiC graph substrate, packets
Include following steps:
(1) substrate is polished
The face c SiC substrate is horizontally arranged, diamond sand paper is placed on substrate surface, applies 1- on diamond sand paper
The power of 20 newton carries out parallel grinding to the face c SiC substrate, polish the candy strip for being parallel to SiC substrate true edge or vertical
In the zigzag candy strip of SiC substrate true edge；
(2) substrate cleans
The face c SiC substrate after polishing is first put into ultrasonic cleaning 1-10min in HF acid or HCl acid, is then placed in acetone
Ultrasonic cleaning 1-10min in solution reuses ethanol solution ultrasonic cleaning 1-10min, then clear with deionized water ultrasound
1-10min is washed, finally with being dried with nitrogen；
(3) it is heat-treated
The face c SiC substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, is first vacuumized
Make the pressure of reaction chamber less than 2 × 10-2Torr；The mixed gas of hydrogen and ammonia is passed through to reaction chamber again, in MOCVD reaction chamber
Pressure is reached under the conditions of 20-760Torr, is 900-1200 DEG C by silicon to temperature, and keep 5-15min, completion pair
The heat treatment of substrate base；
(4) AlN layers of the face extension c
Growth is raw using metal organic chemical vapor deposition MOCVD technique in the face the c SiC substrate of (4a) after heat treatment
The long GaN nucleating layer with a thickness of 10-120nm；
(4b) uses MOCVD technique growth thickness for the Al content gradually variational of 1000-6000nm on GaN nucleating layer
AlGaN layer, growth temperature are 950-1100 DEG C；
(4c) uses MOCVD technique growth thickness for the AlN of 500-3000nm on the AlGaN layer of Al content gradually variational
Layer.
The present invention has the advantage that
1. the present invention in the SiC substrate of the face c due to polishing parallel benchmark edge direction or vertical base using diamond sand paper
The zigzag candy strip of quasi- edge direction prepares graph substrate, so that simplify technique stream while improving quality of materials
Journey shortens fabrication cycle and has saved cost.
2. the gradual change AlGaN layer that the present invention is continuously improved due to using Al component, greatly reduces material stress.
Technical solution of the present invention can be further illustrated by the following drawings and embodiment.
Detailed description of the invention
Fig. 1 is c surface AlN film profile schematic diagram of the present invention；
Fig. 2 is the face the c SiC graph substrate sectional view polished in Fig. 1 by diamond sand paper；
Fig. 3 is the flow chart of present invention production c surface AlN film.
Specific embodiment
Below in conjunction with attached drawing, present invention is further described in detail:
Referring to Fig.1, c surface AlN film of the invention, comprising: the face c SiC substrate layer, GaN nucleating layer, gradual change AlGaN
AlN layers of layer and the face c.
The face the c SiC substrate layer, surface is equipped with the substrate striped to be formed of polishing by diamond sand paper, such as Fig. 2 institute
Show, which is the pattern for being parallel to SiC substrate true edge or the saw-tooth like pattern perpendicular to SiC substrate true edge, is used
In the quality to improve AlN material；
The GaN nucleating layer is located on the SiC substrate layer of the face c, with a thickness of 10-120nm；
The gradual change AlGaN layer: it is located on GaN nucleating layer, uses Al component from 5% gradual change to 100%, to drop
The stress of low material, the gradual change AlGaN layer is with a thickness of 1000-6000nm；
Described the face c AlN layers, it is located on gradual change AlGaN layer, with a thickness of 500-3000nm.
Referring to Fig. 3, the present invention provides three kinds of embodiments of preparation c surface AlN film.
Embodiment 1 prepares GaN nucleating layer with a thickness of 60nm, and gradual change AlGaN layer is with a thickness of the face 3000nm and c AlN thickness degree
For the AlN film based on the face c SiC graph substrate of 1700nm.
Step 1, the face c SiC substrate is ground.
The face c SiC substrate is horizontally arranged, the diamond sand paper that particle diameter is 9 μm is placed on substrate surface, in Buddha's warrior attendant
The power for applying 10 newton on stone sand paper makes sand paper be parallel to the true edge polishing substrate of SiC substrate, grinds saw on sic substrates
Dentate stripe pattern, as shown in Figure 2.
Step 2, the SiC substrate that opposite grinding makes is cleaned.
The SiC substrate ground is first put into ultrasonic cleaning 5min in HF acid, is then placed into ultrasonic in acetone soln
Wave cleans 5min, is next equally cleaned by ultrasonic 5min using ethanol solution, is finally cleaned by ultrasonic again with deionized water
5min, then with being dried with nitrogen.
Step 3, substrate base is heat-treated.
The face c SiC substrate is placed in metal organic chemical vapor deposition MOCVD reaction chamber, first vacuumizing makes reaction chamber
Pressure less than 2 × 10-2Then Torr is passed through the mixed gas of hydrogen and ammonia to reaction chamber, reaches chamber pressure
40Torr carries out heat treatment 8min to substrate base by silicon to 1100 DEG C.
Step 4, the GaN nucleating layer of 70nm thickness is grown.
Substrate base temperature after heat treatment is reduced to 1050 DEG C, being passed through flow simultaneously to reaction chamber is 40 μm of ol/min
Gallium source, flow be 1200sccm hydrogen and flow be 6000sccm ammonia, keep pressure be 40Torr under conditions of
Growth thickness is the GaN nucleating layer of 70nm.
Step 5, the gradual change AlGaN layer of 3000nm thickness is grown on GaN nucleating layer.
The underlayer temperature that grown GaN nucleating layer is reduced to 1000 DEG C, the flow for adjusting silicon source and gallium source makes Al
Component grows the gradual change AlGaN layer with a thickness of 3000nm from 5% gradual change to 100% on GaN nucleating layer.
Step 6, AlN layers of c surface of 1700nm thickness are grown.
The underlayer temperature that grown gradual change AlGaN layer is maintained at 1000 DEG C, being passed through flow simultaneously to reaction chamber is
The ammonia that the silicon source of 40 μm of ol/min, flow are 1200sccm hydrogen and flow is 6000sccm is keeping pressure to be 40Torr
Under conditions of growth thickness be 1700nm AlN layer.
Step 7, the c surface AlN material grown by the above process is taken out from MOCVD reaction chamber, completes the face c
The preparation of AlN film.
Embodiment 2 prepares GaN nucleating layer with a thickness of 10nm, and gradual change AlGaN layer is with a thickness of the face 1000nm and c AlN thickness degree
For the face the c AlN film based on the face c SiC graph substrate of 500nm.
Step 1 grinds the face c SiC substrate.
The face c SiC substrate is horizontally arranged, the metal and stone emery paper that particle diameter is 1 μm is placed on substrate surface, in Buddha's warrior attendant
Apply the true edge polishing substrate that the power of 3N makes sand paper perpendicular to SiC substrate on stone sand paper, grinds zigzag item on sic substrates
Line pattern, as shown in Figure 2.
Step 2, the SiC substrate that opposite grinding makes are cleaned.
The SiC substrate ground is first put into ultrasonic cleaning 5min in HF acid, is then placed in ultrasonic wave in acetone soln
5min is cleaned, is next equally cleaned by ultrasonic 5min using ethanol solution, then with after deionized water ultrasonic cleaning 5min, use
It is dried with nitrogen.
Step 3 is heat-treated substrate base.
The face c SiC substrate is placed in metal organic chemical vapor deposition MOCVD reaction chamber, first vacuumizing makes reaction chamber
Pressure less than 2 × 10-2Then Torr is passed through the mixed gas of hydrogen and ammonia to reaction chamber, makes chamber pressure
20Torr carries out the heat treatment of 5min to substrate base by silicon to 900 DEG C.
Step 4 grows the GaN nucleating layer of 10nm thickness.
Substrate base temperature after heat treatment is increased to 1000 DEG C, is passed through gallium source, hydrogen and ammonia simultaneously to reaction chamber
Three kinds of gases, under conditions of keeping pressure is 20Torr, growth thickness is the GaN nucleating layer of 10nm, and wherein gallium source flux is 5
μm ol/min, hydrogen flowing quantity 1200sccm, ammonia flow 3000sccm.
Step 5 grows the gradual change AlGaN layer of 1000nm thickness on GaN nucleating layer.
The underlayer temperature that grown GaN nucleating layer is reduced to 950 DEG C, adjusts the flow of silicon source and gallium source, growth
Al component is from 5% gradual change to 100%, and with a thickness of the gradual change AlGaN layer of 1000nm.
Step 6, AlN layers of c surface of growth 500nm thickness.
The underlayer temperature that grown gradual change AlGaN layer is maintained at 950 DEG C, is passed through silicon source, hydrogen simultaneously to reaction chamber
Three kinds of gases of gas and ammonia, under conditions of keeping pressure is 20Torr, growth thickness is AlN layers of the face c of 500nm, wherein aluminium
Source flux is 5 μm of ol/min, hydrogen flowing quantity 1200sccm, ammonia flow 3000sccm.
Step 7 takes out the c surface AlN material grown by the above process from MOCVD reaction chamber, completes the face c
The preparation of AlN film.
Embodiment 3 prepares GaN nucleating layer with a thickness of 120nm, and gradual change AlGaN layer is with a thickness of the face 10000nm and c AlN thickness
Degree is the face the c AlN film based on the face c SiC graph substrate of 3000nm.
The face c SiC substrate is horizontally arranged by step A, and the diamond sand paper that particle diameter is 20 μm is placed on substrate table
Face applies the true edge polishing substrate that the power of 20 newton makes sand paper be parallel to SiC substrate, in SiC substrate on diamond sand paper
On grind zigzag candy strip, as shown in Figure 2.
The SiC substrate ground is first put into ultrasonic cleaning 10min in HF acid, is then being put into acetone soln by step B
Next middle ultrasonic cleaning 10min is equally cleaned by ultrasonic 10min using ethanol solution, finally with deionized water ultrasound
10min is cleaned, then with being dried with nitrogen.
The face c SiC substrate is placed in metal organic chemical vapor deposition MOCVD reaction chamber by step C, and first vacuumizing makes
The pressure of reaction chamber is less than 2 × 10-2Then Torr is passed through the mixed gas of hydrogen and ammonia to reaction chamber, makes chamber pressure
Reach 760Torr, by silicon to 1200 DEG C, the heat treatment of 15min is carried out to substrate base.
Substrate base temperature after heat treatment is reduced to 1150 DEG C by step D, and being passed through flow simultaneously to reaction chamber is 100 μ
The ammonia that the hydrogen and flow that the gallium source of mol/min, flow are 1200sccm are 10000sccm is keeping pressure to be 760Torr
Under conditions of, growth thickness is the AlN nucleating layer of 120nm.
The substrate temperature that grown GaN nucleating layer is reduced to 1100 DEG C, adjusts the stream of silicon source and gallium source by step E
Amount, growth Al component is from 5% gradual change to 100%, and with a thickness of the gradual change AlGaN layer of 10000nm.
Step F, is maintained at 1100 DEG C for the underlayer temperature that grown gradual change AlGaN layer, is passed through simultaneously to reaction chamber
Flow is the silicon source of 100 μm of ol/min, the ammonia that flow is 1200sccm hydrogen and flow is 10000sccm, is keeping pressure
Under conditions of 760Torr, growth thickness is AlN layers of the face c of 3000nm.
Step G takes out the c surface AlN material grown by the above process from MOCVD reaction chamber, completes the face c
The preparation of AlN film.
Above description is only three specific examples of the invention, does not constitute any limitation of the invention, it is clear that for this
It, all may be without departing substantially from the principle of the present invention, structure after understand the content of present invention and principle for the professional in field
In the case of, various modifications and variations in form and details are carried out, but these modifications and variations based on inventive concept are still
Within the scope of the claims of the present invention.
Claims (6)
1. a kind of c surface AlN film based on the face c SiC graph substrate, include: from bottom to top the face c SiC substrate layer, GaN at
AlN layers of stratum nucleare, AlGaN layer and the face c, it is characterised in that:
There is the serrated substrate striped polished and formed by diamond sand paper on the surface of the face c SiC substrate layer, which is flat
Pattern of the row in SiC substrate true edge or the saw-tooth like pattern perpendicular to SiC substrate true edge；
AlGaN layer uses Al content gradually variational AlGaN layer, and wherein Al component is from 5% gradual change to 100%.
2. film according to claim 1, it is characterised in that: the GaN nucleating layer is with a thickness of 10-
150nm。
3. film according to claim 1, it is characterised in that: the Al content gradually variational AlGaN layer with a thickness of 1000-
6000nm。
4. film according to claim 1, it is characterised in that: AlN layers of the face c with a thickness of 500-3000nm.
5. a kind of c surface AlN method for manufacturing thin film based on the face c SiC graph substrate, includes the following steps:
(1) substrate is polished
The face c SiC substrate is horizontally arranged, diamond sand paper is placed on substrate surface, applies 1-20 ox on diamond sand paper
The power paused carries out parallel grinding to SiC substrate, polish the candy strip for being parallel to SiC substrate true edge or serves as a contrast perpendicular to SiC
The saw-tooth like pattern of bottom true edge；
(2) substrate cleans
The face c SiC substrate after polishing is first put into ultrasonic cleaning 1-10min in HF acid or HCl acid, is then placed in acetone soln
Middle ultrasonic cleaning 1-10min reuses ethanol solution ultrasonic cleaning 1-10min, then is cleaned by ultrasonic 1- with deionized water
10min, finally with being dried with nitrogen；
(3) it is heat-treated
The face c SiC substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, first vacuumizing makes instead
Answer the pressure of room less than 2 × 10-2Torr；The mixed gas of hydrogen and ammonia is passed through to reaction chamber again, in MOCVD chamber pressure
It is reached under the conditions of 20-760Torr, underlayer temperature is heated to 900-1200 DEG C, and keep 5-15min, complete to substrate base
The heat treatment of piece；
(4) AlN layers of the face extension c
GaN nucleating layer is grown in the face the c SiC substrate of (4a) after heat treatment:
Chamber pressure is maintained at 20-760Torr, temperature is set as 1000-1150 DEG C, and being passed through flow simultaneously is 5-100 μ
The gallium source of mol/min, the ammonia that the hydrogen and flow that flow is 1200sccm are 3000-10000sccm, c after heat treatment
Growth thickness is the GaN nucleating layer of 10-150nm in the SiC substrate of face,
(4b) grows AlGaN layer on GaN nucleating layer:
Chamber pressure is maintained at 20-760Torr, temperature is set as 950-1100 DEG C, and the flow for changing gallium source and silicon source makes
From 5% gradual change to 100%, growth thickness is the Al content gradually variational AlGaN layer of 1000-6000nm for Al component in AlGaN layer,
(4c) growing AIN layer on the AlGaN layer of gradual change Al component:
Chamber pressure is maintained at 20-760Torr, temperature is set as 950-1100 DEG C, while being passed through flow is 5-100 μm of ol/
The silicon source and flow of min is the ammonia of 3000-10000sccm, and growth thickness is AlN layers of the face c of 500-3000nm.
6. according to the method described in claim 5, the wherein diamond sand paper of step (1), uses particle diameter for 1-20 μm
Sand paper.
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| CN108598234A (en) * | 2018-04-26 | 2018-09-28 | 吉林大学 | In a kind of reduction SiC substrate in GaN film tensile stress epitaxial structure and preparation method thereof |
| CN110491973A (en) * | 2019-07-15 | 2019-11-22 | 西安电子科技大学 | C surface GaN film and preparation method thereof based on SiC graph substrate |
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| CN102856447A (en) * | 2012-08-02 | 2013-01-02 | 浙江优纬光电科技有限公司 | Method for improving luminous efficiency of AlGaN-based ultraviolet LED (Light-Emitting Diode) |
| CN105009310A (en) * | 2013-02-05 | 2015-10-28 | 株式会社德山 | Nitride semiconductor light-emitting element |
| CN105161402A (en) * | 2010-04-30 | 2015-12-16 | 波士顿大学理事会 | High effeciency ultraviolet light emitting diode with band structure potential fluctuations |
| CN105514168A (en) * | 2016-01-12 | 2016-04-20 | 清华大学 | Semiconductor structure, forming method thereof and field effect transistor |
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| CN105161402A (en) * | 2010-04-30 | 2015-12-16 | 波士顿大学理事会 | High effeciency ultraviolet light emitting diode with band structure potential fluctuations |
| CN102856447A (en) * | 2012-08-02 | 2013-01-02 | 浙江优纬光电科技有限公司 | Method for improving luminous efficiency of AlGaN-based ultraviolet LED (Light-Emitting Diode) |
| CN105009310A (en) * | 2013-02-05 | 2015-10-28 | 株式会社德山 | Nitride semiconductor light-emitting element |
| CN106165126A (en) * | 2014-02-22 | 2016-11-23 | 传感器电子技术股份有限公司 | There is stress and reduce the semiconductor structure of buffer structure |
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