CN110491973A - C surface GaN film and preparation method thereof based on SiC graph substrate - Google Patents
C surface GaN film and preparation method thereof based on SiC graph substrate Download PDFInfo
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- CN110491973A CN110491973A CN201910635705.3A CN201910635705A CN110491973A CN 110491973 A CN110491973 A CN 110491973A CN 201910635705 A CN201910635705 A CN 201910635705A CN 110491973 A CN110491973 A CN 110491973A
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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
- H01L33/0075—Processes for devices with an active region comprising only III-V compounds 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
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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
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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
Abstract
The invention discloses a kind of c surface GaN film and preparation method based on SiC graph substrate, mainly solve the problems, such as that existing GaN film dislocation density is high, crystal quality is low.Comprising: SiC substrate layer (1), GaN nucleating layer (3) and the face c GaN layer (4), wherein SiC graph substrate surface, which is equipped with, is arranged regularly and evenly spaced coniform pattern, is covered with SiN on the coniform patternxLayer (2), remaining region of substrate are exposed；GaN nucleating layer (3) is distributed between cone cell pattern；The face c GaN layer (4) is located at GaN nucleating layer (3) and SiNxOn layer (2).Present invention reduces the dislocation densities of GaN film, improve the performance of device, can be used for making the photoelectricity and electronic device of c surface GaN base.
Description
Technical field
The invention belongs to microelectronics technology, in particular to a kind of c surface GaN film, can be used for making blue green light,
Microwave power and power electronic devices.
Technical background
It is manufacture light emitting diode, two pole of laser by III-V race's wide band gap nitrides semiconductor material of representative of GaN
Pipe, the important semiconductor material of microwave power device and power electronic devices.Especially InGaN material system is in blue light emitting
Achieve immense success on diode, Shuji Nakamura in 2014, day open country be great, this red rugged brave three people is because in blue light-emitting diode
Tremendous contribution obtains Nobel Prize in physics.
Although GaN base semiconductor devices achieves such huge success, it is currently widely used hetero-epitaxy GaN
About 10 in film8cm-2High dislocation density limit the further promotion of GaN base light emitting device performance.This is because
Dislocation in material is considered as non-radiative recombination center, and the nonequilibrium carrier in material is difficult to avoid that ground fault in place is compound
And photon outgoing will not be generated, greatly reduce luminous efficiency.Therefore to improve device performance, it is thin to further decrease GaN epitaxy
Dislocation density in film is very necessary.
It is the direct epitaxial growth polarity in SiC planar substrate that the method based on SiC substrate growth GaN is widely used at present
C face GaN film, or based on epitaxial growth c surface GaN film direct in SiC graph substrate.Based on graph substrate extension
Though growing obtained GaN film to decrease compared to SiC planar substrate dislocation density, its dislocation density is still higher, limitation
The development of high performance device.
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 combination of SiC graph substrate
SiNxGaN film of exposure mask and preparation method thereof improves the crystal of GaN epitaxial layer to reduce the dislocation density in GaN epitaxial layer
Quality.
Realizing the technical thought of the object of the invention is: cannot be in SiN using GaN layerxThe characteristics of upper nucleation, passes through photoetching work
Skill makes SiNxIt is merely present on the cone cell figure in SiC graph substrate.By inhibiting nucleation of the GaN on cone cell figure raw
It is long, it grows GaN only at inter-pattern space, introduces transversal epitaxial growth process, reduce dislocation density using horizontal extension process
Feature improve GaN epitaxial layer crystal quality.
To achieve the above object, the present invention is based on the GaN films of SiC graph substrate, comprising: SiC substrate layer, GaN nucleation
Layer and the face c GaN layer, it is characterised in that:
The surface of the SiC graph substrate layer is equipped with regularly arranged coniform figure, is covered on the cone cell figure
SiNxLayer, remaining region of substrate are exposed；
The GaN nucleating layer is distributed between cone cell pattern；
The face c GaN layer is located at GaN nucleating layer and SiNxOn layer.
Further, it is characterised in that: SiNxLayer with a thickness of 10-20nm.
Further, it is characterised in that: GaN nucleating layer with a thickness of 10-90nm.
Further, it is characterised in that: the face c GaN layer with a thickness of 1000-3000nm.
To achieve the above object, the present invention is based on the preparation method of the c surface GaN film of SiC graph substrate, features
It is, includes the following steps:
1) SiC graph substrate HF acid, acetone soln, ethanol solution, deionized water is sequentially placed into be cleaned by ultrasonic
5min, finally with being dried with nitrogen；
2) the SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, in SiC
The SiN of 10-20nm is deposited in graph substratex；
3) SiN will be depositedxAfter substrate afterwards is cleaned, spin coating photoresist, followed by photoetching process in pattern light
Processing is exposed under the exposure mask cut blocks for printing；
4) SiN will be removed in the SiC graph substrate after photoetching treatmentxAnd photoresist；
5) the SiC graph substrate after removal photoresist is sequentially placed into HF acid, acetone soln, ethanol solution, gone
Ionized water is cleaned by ultrasonic 5-10min, finally with being dried with nitrogen；
6) the SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, will be reacted
The vacuum degree of room drops below 2 × 10-2Torr；The mixed gas of hydrogen and ammonia is passed through to reaction chamber again, is reacted in MOCVD
Chamber pressure is reached under the conditions of 20-760Torr, is 900-1200 DEG C by silicon to temperature, and keep 5-10min, is completed
Heat treatment to substrate；
7) metal organic chemical vapor deposition MOCVD is used between the cone cell pattern of SiC graph substrate after heat treatment
Technique growth thickness is the GaN nucleating layer of 10-90nm；Again in GaN nucleating layer and SiNxOn layer, using metal organic-matter chemical
Vapor deposition MOCVD technique growth thickness is the GaN layer of 1000-3000nm, completes the preparation to film.
The invention has the following advantages over the prior art:
1. the present invention deposits SiN in the cone shaped pattern due to being equipped with cone shaped pattern in SiC graph substratex, inhibit
Growth of GaN, avoids the upward extension of thin film growth process Dislocations at this.
2. the present invention promotes in thin film growth process due to only growing GaN nucleating layer in substrate cone shaped pattern gap location
The transverse direction of dislocation is buried in oblivion, and the dislocation density in GaN film is effectively reduced.
Detailed description of the invention
Fig. 1 is the schematic diagram of the section structure of c surface GaN film of the present invention；
Fig. 2 is the flow diagram that the present invention prepares c face GaN film.
Specific embodiment
Below in conjunction with attached drawing, present invention is further described in detail:
Referring to Fig.1, c surface GaN film of the invention, comprising: SiC substrate layer 1, SiNxIlluvium 2, GaN nucleating layer 3
With c surface GaN layer 4.
The SiC graph substrate layer 1, surface is equipped with and is arranged regularly and evenly spaced coniform pattern, to drop
The dislocation density of low GaN film；
The SiNxLayer 2, is covered on the coniform pattern of SiC substrate, with a thickness of 10-20nm, to inhibit GaN thin
Film growth course Dislocations upwardly extend；
The GaN nucleating layer 3, is distributed between coniform pattern, with a thickness of 10-90nm, to promote GaN film horizontal
To burying in oblivion for growth Dislocations, dislocation density is further decreased；
The face c GaN layer 4 is located at GaN nucleating layer 3 and SiNxOn layer 2, with a thickness of 1000-3000nm.
Referring to Fig. 2, the present invention provides three kinds of embodiments of preparation c surface GaN film.
Embodiment 1 prepares GaN nucleating layer with a thickness of 50nm, SiNxLayer with a thickness of the face 10nm and c GaN layer with a thickness of
The GaN film based on SiC graph substrate of 1500nm.
Step 1, substrate cleans.
This example uses the substrate for being formed with the SiC figure of conical pattern, and it is clear to put it into ultrasonic wave in HF acid
5min is washed, acetone soln ultrasonic cleaning 5min is then placed in, then uses ethanol solution ultrasonic cleaning 5min, then make
With deionized water ultrasonic cleaning 5min, finally with being dried with nitrogen.
Step 2, SiN is deposited on substratex。
The SiC graph substrate of conical pattern after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction
In room, deposition thickness is the SiN of 10nmxLayer completes the SiN in SiC graph substratexDeposit, such as Fig. 2 (b).
Step 3, to SiNxCarry out photoetching.
3.1) to being deposited with SiNxSiC graph substrate cleaned after, spin coating photoresist on it, such as Fig. 2 (c)；
3.2) processing is exposed under the exposure mask of reticle using photoetching process, so that being distributed in SiC graph substrate circle
Photoresist between cone cell pattern is removed, and exposes the SiN deposited in advance between coniform patternxLayer, such as Fig. 2 (d).
Step 4, SiN is removedxWith photoresist.
4.1) the SiC graph substrate after photoetching treatment is performed etching, is distributed between the coniform pattern of substrate with removal
SiNx, such as Fig. 2 (e)；
4.2) photoresist covered on the coniform pattern of SiC graph substrate is removed, expose coniform pattern it
On the SiN that deposits in advancex, such as Fig. 2 (f).
Step 5, the SiC graph substrate after cleaning removal photoresist.
SiC graph substrate after removal photoresist is put into ultrasonic cleaning 5min in HF acid, is then placed in acetone soln
Ultrasonic cleaning 5min then uses ethanol solution ultrasonic cleaning 5min, reuses deionized water ultrasonic cleaning
5min, finally with being dried with nitrogen.
Step 6, substrate is heat-treated.
SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, it first will reaction
The vacuum degree of room drops below 2 × 10-2Torr；The mixed gas of hydrogen and ammonia is passed through to reaction chamber again, makes to react chamber pressure
Power is 40Torr, by silicon to 1100 DEG C, carries out the heat treatment that the time is 8min to substrate base.
Step 7, the GaN nucleating layer of 50nm thickness is grown.
Underlayer temperature after heat treatment is reduced to 960 DEG C, is passed through the gallium that flow is 20 μm of ol/min simultaneously to reaction chamber
The ammonia that source, flow are 1200sccm hydrogen and flow is 4000sccm, growth is thick under conditions of keeping pressure to be 40Torr
Degree is the GaN nucleating layer of 50nm, such as Fig. 2 (g).
Step 8, the c surface GaN layer of 1500nm thickness is grown.
The underlayer temperature that grown GaN nucleating layer is maintained at 1000 DEG C, being passed through flow simultaneously to reaction chamber is 30 μ
The ammonia that the gallium source of mol/min, flow are 1200sccm hydrogen and flow is 2000sccm is keeping pressure to be the item of 40Torr
Growth thickness is the GaN layer of 1500nm under part, such as Fig. 2 (h).
Step 9, the c surface GaN material grown by the above process is taken out from MOCVD reaction chamber, completes polarity c
The preparation of face GaN film.
Embodiment 2 prepares GaN nucleating layer with a thickness of 30nm, SiNxLayer with a thickness of the face 15nm and c GaN layer with a thickness of
The GaN film based on SiC graph substrate of 1000nm.
Step 1, substrate cleaning.
The specific implementation of this step is identical as the step 1 of embodiment 1.
Step 2 deposits SiN on substratex。
SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, deposition thickness
For the SiN of 15nmxLayer, such as Fig. 2 (b).
Step 3, to SiNxCarry out photoetching treatment.
The specific implementation of this step is identical as the step 3 of embodiment 1.
Step 4 removes SiNxWith photoresist.
The specific implementation of this step is identical as the step 4 of embodiment 1.
Step 5, cleaning remove the SiC graph substrate after photoresist.
SiC graph substrate after removal photoresist is put into ultrasonic cleaning 7min in HF acid, is then placed in acetone soln
Ultrasonic cleaning 7min then uses ethanol solution ultrasonic cleaning 7min, reuses deionized water ultrasonic cleaning
7min, finally with being dried with nitrogen.
Step 6 is heat-treated substrate.
SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, it first will reaction
The vacuum degree of room drops below 2 × 10-2Torr；It is passed through the mixed gas of hydrogen and ammonia to reaction chamber simultaneously again, makes to react
Chamber pressure is 20Torr, by silicon to 1200 DEG C, carries out 5min heat treatment to substrate base.
Step 7 grows the GaN nucleating layer of 30nm thickness.
Underlayer temperature after heat treatment is reduced to 900 DEG C, is passed through the gallium that flow is 10 μm of ol/min simultaneously to reaction chamber
The ammonia that source, flow are 1200sccm hydrogen and flow is 3000sccm, growth is thick under conditions of keeping pressure to be 20Torr
Degree is the GaN nucleating layer of 30nm.
Step 8 grows the face the c GaN layer of 1000nm thickness.
The underlayer temperature that grown GaN nucleating layer is maintained at 950 DEG C, being passed through flow simultaneously to reaction chamber is 15 μ
The ammonia that the gallium source of mol/min, flow are 1200sccm hydrogen and flow is 3000sccm is keeping pressure to be the item of 20Torr
Growth thickness is the GaN layer of 1000nm under part, such as Fig. 2 (h).
The middle c surface GaN material grown by the above process is taken out from MOCVD reaction chamber, completes pole by step 9
The preparation of property c face GaN film.
Embodiment 3 prepares GaN nucleating layer with a thickness of 90nm, SiNxLayer with a thickness of the face 20nm and c GaN layer with a thickness of
The GaN film based on SiC graph substrate of 3000nm.
Step A, substrate cleaning.
The specific implementation of this step is identical as the step 1 of embodiment 1.
Step B, deposits SiN on substratex。
SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, deposition thickness
For the SiNx layer of 20nm, the SiNx deposit in SiC graph substrate is completed, such as Fig. 2 (b).
Step C, to SiNxCarry out photoetching treatment.
The specific implementation of this step is identical as the step 3 of embodiment 1.
Step D removes SiNxWith photoresist.
The specific implementation of this step is identical as the step 4 of embodiment 1.
Step E, cleaning remove the SiC graph substrate after photoresist.
SiC graph substrate after removal photoresist is put into ultrasonic cleaning 10min in HF acid, is then placed in acetone soln
Ultrasonic cleaning 10min then uses ethanol solution ultrasonic cleaning 10min, reuses deionized water ultrasonic cleaning
10min, finally with being dried with nitrogen.
Step F, is heat-treated substrate base.
SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, it first will reaction
The vacuum degree of room drops below 2 × 10-2Torr；The mixed gas of hydrogen and ammonia is passed through to reaction chamber again, makes to react chamber pressure
Power is 760Torr, by silicon to 900 DEG C, carries out the heat treatment that the time is 10min to substrate base.
Step G grows the GaN nucleating layer of 90nm thickness.
Underlayer temperature after heat treatment is reduced to 1000 DEG C, is passed through gallium source, hydrogen and ammonia simultaneously to reaction chamber,
In, the flow in gallium source is 50 μm of ol/min, and the flow of hydrogen is 1200sccm, and the flow of ammonia is 4000sccm；It is keeping pressing
The GaN nucleating layer that growth thickness is 90nm under conditions of power is 760Torr, such as Fig. 2 (g).
Step H grows the c surface GaN layer of 3000nm thickness.
The underlayer temperature that grown GaN nucleating layer is maintained at 1100 DEG C, is passed through gallium source, hydrogen simultaneously to reaction chamber
And ammonia, wherein the flow in gallium source is 100 μm of ol/min, and the flow of hydrogen is 1200sccm and the flow of ammonia is
5000sccm；The GaN layer that growth thickness is 3000nm under conditions of keeping pressure to be 760Torr, such as Fig. 2 (h).
The middle c surface GaN material grown by the above process is taken out from MOCVD reaction chamber, completes pole by step I
The preparation of property c face GaN 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 claims in the present invention protection scope.
Claims (7)
1. the c surface GaN film and preparation method thereof based on SiC graph substrate, comprising:
SiC substrate layer (1), GaN nucleating layer (3) and the face c GaN layer (4), it is characterised in that:
The surface of the SiC graph substrate layer (1) is equipped with regularly arranged coniform figure, is covered with SiN on the cone cell figurex
Layer (2), remaining region of substrate are exposed；
The GaN nucleating layer (3) is distributed between cone cell pattern；
The face c GaN layer (4) is located at GaN nucleating layer (3) and SiNxOn layer (2).
2. film according to claim 1, it is characterised in that: SiNxLayer (2) with a thickness of 10-20nm.
3. film according to claim 1, it is characterised in that: GaN nucleating layer (3) with a thickness of 10-90nm.
4. film according to claim 1, it is characterised in that: the face c GaN layer (4) with a thickness of 1000-3000nm.
5. a kind of c surface GaN method for manufacturing thin film based on SiC graph substrate, which comprises the steps of:
1) SiC graph substrate is sequentially placed into HF acid, acetone soln, ethanol solution, deionized water and is cleaned by ultrasonic 5min, most
Afterwards with being dried with nitrogen；
2) the SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, in SiC figure
The SiN of 10-20nm is deposited on substratex；
3) SiN will be depositedxAfter substrate afterwards is cleaned, spin coating photoresist, followed by photoetching process in patterned photo version
Processing is exposed under exposure mask；
4) SiN will be removed in the SiC graph substrate after photoetching treatmentxAnd photoresist；
5) the SiC graph substrate after removal photoresist is sequentially placed into HF acid, acetone soln, ethanol solution, deionization
Water is cleaned by ultrasonic 5-10min, finally with being dried with nitrogen；
6) the SiC graph substrate after cleaning is placed in metal organic chemical vapor deposition MOCVD reaction chamber, by reaction chamber
Vacuum degree drops below 2 × 10-2Torr；The mixed gas of hydrogen and ammonia is passed through to reaction chamber again, reacts chamber pressure in MOCVD
Power is reached under the conditions of 20-760Torr, is 900-1200 DEG C by silicon to temperature, and keep 5-10min, is completed to lining
The heat treatment at bottom；
7) metal organic chemical vapor deposition MOCVD technique is used between the cone cell pattern of SiC graph substrate after heat treatment
Growth thickness is the GaN nucleating layer of 10-90nm；Again in GaN nucleating layer and SiNxOn layer, using metal-organic chemical vapor
The GaN layer that MOCVD technique growth thickness is 1000-3000nm is deposited, the preparation to film is completed.
6. according to the method described in claim 5, wherein using the technique item of MOCVD technique growth GaN nucleating layer in step 7)
Part is as follows:
Chamber pressure is 20-760Torr,
Temperature is 900-1000 DEG C,
Gallium source flux is 10-50 μm of ol/min,
Hydrogen flowing quantity is 1200sccm,
Ammonia flow is 3000-4000sccm.
7. according to the method described in claim 5, wherein using the technique of the face MOCVD technique growth polarity c GaN layer in step 7)
Condition is as follows:
Chamber pressure is 20-760Torr,
Temperature is 950-1100 DEG C,
Hydrogen flowing quantity is 1200sccm,
Gallium source flux is 5-100 μm of ol/min,
Ammonia flow is 2000-5000sccm.
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| CN113990940A (en) * | 2021-08-30 | 2022-01-28 | 华灿光电（浙江）有限公司 | Silicon carbide epitaxial structure and manufacturing method thereof |
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