CN108807609A - The preparation method of the patterned substrate LED of metal nanoparticle modification - Google Patents
The preparation method of the patterned substrate LED of metal nanoparticle modification Download PDFInfo
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- CN108807609A CN108807609A CN201810415268.XA CN201810415268A CN108807609A CN 108807609 A CN108807609 A CN 108807609A CN 201810415268 A CN201810415268 A CN 201810415268A CN 108807609 A CN108807609 A CN 108807609A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01L33/10—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 light reflecting structure, e.g. semiconductor Bragg reflector
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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
- H01L33/12—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 stress relaxation structure, e.g. buffer layer
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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
Abstract
The invention discloses the preparation methods of the patterned substrate LED of metal nanoparticle modification a kind of, include the following steps：1) one layer of metallic film is formed in patterned substrate, is rapidly heated to 750-1200 DEG C, and anneal 1-10min, you can metal nanoparticle is formed in patterned substrate；2) it is transferred in mocvd growth chamber, grown buffer layer；3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain the patterned substrate LED of metal nanoparticle modification.The present invention improves the epitaxial lateral overgrowth of buffer layer using metal nanoparticle as mask, reduces dislocation density, achievees the effect that improve epitaxy；Using metal nanoparticle, be conducive to the thickness for reducing buffer layer；Au or Ag nano-particles have preferable reflection characteristic to light, and the reflected light emitting of light and LED surface that active layer issues is gone out, the light extraction efficiency of LED component is improved.
Description
Technical field
The invention belongs to LED technology fields, and in particular to a kind of patterned substrate LED's of metal nanoparticle modification
Preparation method.
Background technology
In order to improve the epitaxy effect of graphical sapphire substrate epitaxial growth GaN film, typically：(1) by using
Thicker AlN AlGaN buffer layers；(2) one layer of AlN buffer layer is first grown, however alignment pattern is carried out to AlN buffer layers；
(3) one layer of AlN SiN insert layer is introduced in buffer layer.But these methods all have some disadvantages, such as method
(1) and the deficiency of (3) be buffer layer thickness it is larger, required raw material increase, and can increase cost；The deficiency of method (2) is
Complex process needs to take out in sample when to AlN alignments, completes the growth that puts in again after etching；And the technique of etching
More complicated, need by gluing, photoetching, cleaning, ICP etching, cleaning and etc., this significantly increases be processed into
This.
Therefore, it is necessary to research and develop one kind can manufacturing procedure it is simple, it is at low cost, reduce buffering thickness and reduce dislocation it is close
Degree improves the patterned substrate LED of the metal nanoparticle modification of epitaxy effect.
Invention content
It is at low cost the object of the present invention is to provide a kind of manufacturing procedure is simple, can reduce buffering thickness and reduce dislocation
Density improves the patterned substrate LED of the metal nanoparticle modification of epitaxy effect.
The technical solution adopted by the present invention is：A kind of preparation method of the patterned substrate LED of metal nanoparticle modification,
Include the following steps：
1) one layer of metallic film is formed in patterned substrate, is rapidly heated to 750-1200 DEG C, and anneal 1-10min, i.e.,
Metal nanoparticle can be formed in patterned substrate；
2) it is transferred in mocvd growth chamber, growing AIN or AlGaN buffer layers；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The patterned substrate LED of metal nanoparticle modification.
Preferably, the metallic film is Ag films, Au films, In films or Al films；The metal nanoparticle is
Ag nano-particles, Au nano-particles, In nano-particles or Al nano-particles.
Preferably, in step 1), the specific method of metal nanoparticle form is：Using electron beam evaporation equipment, scheming
Layer of Au film or Ag films, evaporation current 100-150A are deposited on shape substrate, vacuum is 1 × 10-6 -1×10-3Pa,
In N2It under protective atmosphere, is rapidly heated to 750-1200 DEG C, anneal 0.5-5min, you can Au nanometers are formed in patterned substrate
Particle or Ag nano-particles.It is furthermore preferred that evaporation current is 120A, vacuum is 1 × 10-4Pa, in N2Under protective atmosphere, quickly
800 DEG C are warming up to, annealing time 1min.
Preferably, in step 1), the specific method of metal nanoparticle form is：Patterned substrate is placed on MOCVD lifes
In long room, at 400-600 DEG C, In metallorganics or Al metallorganics is passed through with the flow of 350-600sccm, spread one layer
Then In films or Al films are more than 10 in vacuum degree-3It under conditions of Pa, is rapidly heated to 750-1200 DEG C, anneal 1-
10min, you can In nano-particles or Al nano-particles are formed in patterned substrate.
In step 2), using metal nanoparticle as mask, technique growing AIN routinely or AlGaN buffer layers.It carries
The epitaxial lateral overgrowth of high buffer layer reduces dislocation density, to achieve the purpose that improve epitaxy effect.
Preferably, the In metallorganics are trimethyl indium or diethyl indium；The Al metallorganics are front three
Base aluminium or diethyl aluminum.
Preferably, the thickness of the metallic film is 6-30nm.It is furthermore preferred that the thickness of metallic film is 10nm.Buffering
The thickness of layer is 2-20nm.
Preferably, a diameter of 2-6nm of metal nanoparticle.
Preferably, the patterned substrate is graphical sapphire substrate.
The beneficial effects of the invention are as follows：The present invention improves buffer layer lateral out using metal nanoparticle as mask
Prolong outgrowth, reduce dislocation density, to achieve the purpose that improve epitaxy effect；Using metal nanoparticle, be conducive to reduce
The thickness of buffer layer reduces production cost；Au or Ag nano-particles have preferable reflection characteristic to light, can send out active layer
The reflected light emitting of light and LED surface out is gone out, to improve the light extraction efficiency of LED component；The gold of the present invention
Preparation method is simple with belonging to the patterned substrate of Nanoparticle Modified, and use scope is wide.
Description of the drawings
Fig. 1 is the forming process schematic diagram of metal nanoparticle, wherein 11 be graphical sapphire substrate, and 12 be metal
Nano-particle.
Fig. 2 is that AlGaN buffer layers grow schematic diagram on the graphical sapphire substrate LED that metal nanoparticle is modified,
Wherein 11 be graphical sapphire substrate, and 12 be metal nanoparticle, and 13 be buffer layer.
Fig. 3 is the X-ray rocking curve (XRC) of LED epitaxial wafer；For in the prior art without metal nano wherein in (a)
The X-ray rocking curve (XRC) of the LED epitaxial wafer of particle；(b) X-ray of the LED epitaxial wafer prepared for embodiment 1 waves song
Line.
Fig. 4 is luminescence generated by light (PL) collection of illustrative plates of LED epitaxial wafer prepared by embodiment 1.
Specific implementation mode
The present invention provides the preparation methods of the patterned substrate LED of metal nanoparticle modification a kind of, including following step
Suddenly：
1) one layer of metallic film is formed in patterned substrate, is rapidly heated to 750-1200 DEG C, and anneal 1-10min, i.e.,
Metal nanoparticle can be formed in patterned substrate；
2) it is transferred in mocvd growth chamber, grown buffer layer；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The patterned substrate LED of metal nanoparticle modification.
Preferably, the specific method of metal nanoparticle form is：Using electron beam evaporation equipment, in patterned substrate
Layer of Au film or Ag films, evaporation current 100-150A is deposited, vacuum is 1 × 10-6-1×10-3Pa, in N2Protective atmosphere
Under, it is rapidly heated to 750-1200 DEG C, anneal 0.5-5min, you can Au nano-particles or Ag nanometers are formed in patterned substrate
Particle.
Preferably, the specific method of metal nanoparticle form is：Patterned substrate is placed in mocvd growth chamber,
At 400-600 DEG C, In metallorganics or Al metallorganics are passed through with the flow of 350-600sccm, spread one layer of In film or
Then Al films are more than 10 in vacuum degree-3It under conditions of Pa, is rapidly heated to 750-1200 DEG C, anneal 1-10min, you can
In nano-particles or Al nano-particles are formed in patterned substrate.
Fig. 1 is the forming process schematic diagram of Ag metal nanoparticles, wherein 11 be graphical sapphire substrate, and 12 be gold
Belong to nano-particle；One layer of Ag metallic film is first deposited on graphical sapphire substrate, then in N2Under protective atmosphere, high temperature is fast
Fast annealing both can get Ag metal nanoparticles.
Fig. 2 is that AlGaN grows schematic diagram on the graphical sapphire substrate LED that metal nanoparticle is modified, and 11 be figure
Shape Sapphire Substrate, 12 be metal nanoparticle, and 13 be buffer layer.Metal nanoparticle can play the role of mask, carry
The epitaxial lateral overgrowth for crossing buffer layer, to achieve the purpose that improve epitaxy effect.
Embodiment 1
A kind of preparation method of the patterned substrate LED of metal nanoparticle modification, includes the following steps：
1) electron beam evaporation equipment is utilized, the Ag films that a layer thickness is 10nm are deposited on graphical sapphire substrate,
Evaporation current is 120A, and vacuum is 1 × 10-4Pa, in N2It under protective atmosphere, is rapidly heated to 800 DEG C, anneal 1min, you can
The Ag nano-particles of a diameter of 3nm are formed in patterned substrate；
2) it is transferred in mocvd growth chamber, growth thickness is the AlGaN buffer layers of 5nm；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The graphical sapphire substrate LED of metal nanoparticle modification.
Fig. 3 shows the X-ray rocking curve of LED epitaxial wafer, wherein in the prior art without metal nanoparticle in (a)
LED epitaxial wafer X-ray rocking curve (XRC)；(b) the X-ray rocking curve of the LED epitaxial wafer prepared for embodiment 1.Such as
Shown in (b) of Fig. 3, the XRC half-peak breadths of LED epitaxial wafer prepared by embodiment 1 are 201arcsec, and being better than does not have Ag nanoparticles
The LED epitaxial wafer (244arcse c) of son.
Fig. 4 is the PL collection of illustrative plates of LED epitaxial wafer prepared by embodiment 1, and intensity is the LED epitaxial wafers of no Ag nano-particles
1.5-2 times, light extraction efficiency improves 3-5%.
Embodiment 2
A kind of preparation method of the patterned substrate LED of metal nanoparticle modification, includes the following steps：
1) electron beam evaporation equipment is utilized, the Au films that a layer thickness is 6nm are deposited on graphical sapphire substrate, steam
Power generation stream is 100A, and vacuum is 1 × 10-3Pa, in N2It under protective atmosphere, is rapidly heated to 750 DEG C, anneal 5min, you can is scheming
The Au nano-particles of a diameter of 2nm are formed on shape substrate；
2) it is transferred in mocvd growth chamber, growth thickness is the AlN buffer layers of 2nm；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The graphical sapphire substrate LED of metal nanoparticle modification.
Embodiment 3
A kind of preparation method of the patterned substrate LED of metal nanoparticle modification, includes the following steps：
1) electron beam evaporation equipment is utilized, the Au films that a layer thickness is 15nm are deposited on graphical sapphire substrate,
Evaporation current is 150A, and vacuum is 1 × 10-5Pa, in N2It under protective atmosphere, is rapidly heated to 1000 DEG C, anneal 2min, you can
The Au nano-particles of a diameter of 5nm are formed on graphical sapphire substrate；
2) it is transferred in mocvd growth chamber, growth thickness is the AlN buffer layers of 8nm；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The graphical sapphire substrate LED of metal nanoparticle modification.
Embodiment 4
A kind of preparation method of the patterned substrate LED of metal nanoparticle modification, includes the following steps：
1) graphical sapphire substrate is placed in mocvd growth chamber, at 400 DEG C, three is passed through with the flow of 350sccm
Methyl indium, paving a layer thickness are 12nm In films, then, are more than 10 in vacuum degree-3Under conditions of Pa, it is rapidly heated to 900
DEG C, anneal 1min, you can the In nano-particles of a diameter of 3nm are formed in patterned substrate；
2) it is transferred in mocvd growth chamber, growth thickness is the AlN buffer layers of 5nm；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The graphical sapphire substrate LED of metal nanoparticle modification.
Embodiment 5
A kind of preparation method of the patterned substrate LED of metal nanoparticle modification, includes the following steps：
1) graphical sapphire substrate is placed in mocvd growth chamber, at 500 DEG C, three is passed through with the flow of 500sccm
Then aluminium methyl, the Al films that paving a layer thickness is 15nm are more than 10 in vacuum degree-3Under conditions of Pa, it is rapidly heated to 1000
DEG C, anneal 5min, you can the Al nano-particles of a diameter of 5nm are formed in patterned substrate；
2) it is transferred in mocvd growth chamber, growth thickness is the AlGaN buffer layers of 10nm；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The graphical sapphire substrate LED of metal nanoparticle modification.
Embodiment 6
A kind of preparation method of the patterned substrate LED of metal nanoparticle modification, includes the following steps：
1) graphical sapphire substrate is placed in mocvd growth chamber, at 600 DEG C, two is passed through with the flow of 600sccm
Then aluminium ethide, the Al films that paving a layer thickness is 20nm are more than 10 in vacuum degree-3Under conditions of Pa, it is rapidly heated to 1200
DEG C, anneal 8min, you can the Al nano-particles of a diameter of 6nm are formed in patterned substrate；
2) it is transferred in mocvd growth chamber, growth thickness is the AlN buffer layers of 12nm；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain
The graphical sapphire substrate LED of metal nanoparticle modification.
Claims (9)
1. a kind of preparation method of the patterned substrate LED of metal nanoparticle modification, which is characterized in that include the following steps：
1) one layer of metallic film is formed in patterned substrate, is rapidly heated to 750-1200 DEG C, and anneal 1-10min, you can
Metal nanoparticle is formed in patterned substrate；
2) it is transferred in mocvd growth chamber, grown buffer layer；
3) growth u-shaped GaN, N-shaped GaN, InGaN/GaN Quantum Well, AlGaN electronic barrier layers and p-type GaN, you can obtain metal
The patterned substrate LED of Nanoparticle Modified.
2. preparation method according to claim 1, which is characterized in that the metallic film is Ag films, Au films, In thin
Film or Al films；The metal nanoparticle is Ag nano-particles, Au nano-particles, In nano-particles or Al nano-particles.
3. preparation method according to claim 2, which is characterized in that in step 1), metal nanoparticle form it is specific
Method is：Using electron beam evaporation equipment, layer of Au film or Ag films, evaporation current 100- are deposited in patterned substrate
150A, vacuum are 1 × 10-6-1×10-3Pa, in N2Under protective atmosphere, it is rapidly heated to 750-1200 DEG C, anneal 0.5-5min,
Au nano-particles or Ag nano-particles can be formed in patterned substrate.
4. preparation method according to claim 2, which is characterized in that in step 1), metal nanoparticle form it is specific
Method is：Patterned substrate is placed in mocvd growth chamber, at 400-600 DEG C, In is passed through with the flow of 350-600sccm
Metallorganic or Al metallorganics spread one layer of In film or Al films, then, are more than 10 in vacuum degree-3Under conditions of Pa,
It is rapidly heated to 750-1200 DEG C, anneal 1-10min, you can In nano-particles or Al nanoparticles are formed in patterned substrate
Son.
5. preparation method according to claim 4, which is characterized in that the In metallorganics are trimethyl indium or two
Ethyl indium；The Al metallorganics are trimethyl aluminium or diethyl aluminum.
6. preparation method according to claim 1, which is characterized in that in step 2), buffer layer be AlN buffer layers or
AlGaN buffer layers；The thickness of buffer layer is 2-20nm.
7. preparation method according to claim 1, which is characterized in that the thickness of the metallic film is 6-30nm.
8. preparation method according to claim 1, which is characterized in that a diameter of 2-6nm of metal nanoparticle.
9. preparation method according to claim 1, which is characterized in that the patterned substrate is graphic sapphire lining
Bottom.
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| CN110120448A (en) * | 2019-05-07 | 2019-08-13 | 厦门大学 | A kind of nitride LED production method based on metal mask substrate |
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