CN108807609B - Preparation method of metal nanoparticle modified patterned substrate L ED - Google Patents
Preparation method of metal nanoparticle modified patterned substrate L ED Download PDFInfo
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- CN108807609B CN108807609B CN201810415268.XA CN201810415268A CN108807609B CN 108807609 B CN108807609 B CN 108807609B CN 201810415268 A CN201810415268 A CN 201810415268A CN 108807609 B CN108807609 B CN 108807609B
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- 239000000758 substrate Substances 0.000 title claims abstract description 78
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 239000010409 thin film Substances 0.000 claims abstract description 19
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000002105 nanoparticle Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 24
- 229910052594 sapphire Inorganic materials 0.000 claims description 23
- 239000010980 sapphire Substances 0.000 claims description 23
- 239000010408 film Substances 0.000 claims description 18
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 10
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000005566 electron beam evaporation Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- CQYBWJYIKCZXCN-UHFFFAOYSA-N diethylaluminum Chemical compound CC[Al]CC CQYBWJYIKCZXCN-UHFFFAOYSA-N 0.000 claims description 3
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical group C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 3
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 claims description 3
- UXFDJNIGYGTLAX-UHFFFAOYSA-N diethylindium Chemical compound CC[In]CC UXFDJNIGYGTLAX-UHFFFAOYSA-N 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 230000000903 blocking effect Effects 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 9
- 238000005229 chemical vapour deposition Methods 0.000 abstract 1
- 235000012431 wafers Nutrition 0.000 description 11
- 229910052774 Proactinium Inorganic materials 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005530 etching Methods 0.000 description 3
- 208000012868 Overgrowth Diseases 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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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- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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 having potential barriers 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 having potential barriers 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 having potential barriers 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 having potential barriers 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 having potential barriers 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 having potential barriers 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 having potential barriers 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
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Abstract
The invention discloses a preparation method of a patterned substrate L ED modified by metal nanoparticles, which comprises the following steps of 1) forming a layer of metal thin film on the patterned substrate, rapidly heating to 750-1200 ℃, annealing for 1-10min, and forming the metal nanoparticles on the patterned substrate, 2) transferring the patterned substrate to an MOCVD (metal organic chemical vapor deposition) growth chamber to grow a buffer layer, 3) growing u-type GaN, n-type GaN, InGaN/GaN quantum wells, AlGaN electron barrier layers and p-type GaN to obtain the patterned substrate L ED. modified by the metal nanoparticles.
Description
Technical Field
The invention belongs to the technical field of L ED, and particularly relates to a preparation method of a metal nanoparticle modified patterned substrate L ED.
Background
In order to improve the epitaxial effect of epitaxially growing a GaN thin film on a patterned sapphire substrate, the following steps are generally performed: (1) by using thicker AlN or AlGaN buffer layers; (2) firstly growing an AlN buffer layer, and then carrying out pattern alignment on the AlN buffer layer; (3) an AlN or SiN insertion layer is introduced into the buffer layer. However, these methods have certain disadvantages, for example, the methods (1) and (3) have disadvantages that the thickness of the buffer layer is large, the required raw material is increased, and the cost is increased; the method (2) has the defects of complex process, and when AlN is subjected to alignment, a sample needs to be taken out and then put in for growth after etching is finished; and the etching process is also relatively complex, and steps such as gluing, photoetching, cleaning, ICP etching, cleaning and the like are required, so that the processing cost is greatly increased.
Therefore, it is necessary to develop a patterned substrate L ED modified with metal nanoparticles that can be processed with simple process steps, low cost, reduced buffer layer thickness, reduced dislocation density, and improved epitaxy effect.
Disclosure of Invention
The invention aims to provide a patterned substrate L ED modified by metal nanoparticles, which has simple processing procedures and low cost, can reduce the thickness of a buffer layer, reduce the dislocation density and improve the epitaxial effect.
The invention adopts the technical scheme that the preparation method of the metal nanoparticle modified patterned substrate L ED comprises the following steps:
1) forming a layer of metal film on the patterned substrate, rapidly heating to 750-1200 ℃, and annealing for 1-10min to form metal nanoparticles on the patterned substrate;
2) transferring the substrate to an MOCVD growth chamber, and growing an AlN or AlGaN buffer layer;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned substrate L ED modified by the metal nanoparticles.
Preferably, the metal film is an Ag film, an Au film, an In film or an Al film; the metal nanoparticles are Ag nanoparticles, Au nanoparticles, In nanoparticles or Al nanoparticles.
Preferably, in the step 1), the specific method for forming the metal nanoparticles is to evaporate an Au thin film or an Ag thin film on the patterned substrate by using an electron beam evaporation device, wherein the evaporation current is 100-150A, and the vacuum is 1 × 10-6-1×10-3Pa, in N2Under the protection atmosphere, rapidly heating to 750-1200 ℃, annealing for 0.5-5min, and then Au nanoparticles or Ag nanoparticles can be formed on the patterned substrate, more preferably, the evaporation current is 120A, and the vacuum is 1 × 10-4Pa, in N2Under the protective atmosphere, the temperature is rapidly raised to 800 ℃, and the annealing time is 1 min.
Preferably, in step 1), the specific method for forming the metal nanoparticles is as follows: placing the patterned substrate In an MOCVD growth chamber, introducing an In metal organic substance or an Al metal organic substance at the temperature of 400-600 ℃ and the flow rate of 350-600sccm, laying an In thin film or an Al thin film, and then, keeping the vacuum degree to be more than 10-3Under the condition of Pa, rapidly heating to 750-1200 ℃, and annealing for 1-10min to form In nanoparticles or Al nanoparticles on the patterned substrate.
In the step 2), the AlN or AlGaN buffer layer is grown by using the metal nanoparticles as a mask according to a conventional process. The transverse epitaxial overgrowth of the buffer layer is improved, and the dislocation density is reduced, so that the purpose of improving the epitaxial effect is achieved.
Preferably, the In metallorganic is trimethyl indium or diethyl indium; the Al metal organic matter is trimethyl aluminum or diethyl aluminum.
Preferably, the thickness of the metal thin film is 6 to 30 nm. More preferably, the thickness of the metal thin film is 10 nm. The thickness of the buffer layer is 2-20 nm.
Preferably, the metal nanoparticles have a diameter of 2 to 6 nm.
Preferably, the patterned substrate is a patterned sapphire substrate.
The metal nano particle modified patterned substrate has the beneficial effects that the metal nano particle is used as a mask, the transverse epitaxial overgrowth of the buffer layer is improved, the dislocation density is reduced, the purpose of improving the epitaxial effect is achieved, the metal nano particle is beneficial to reducing the thickness of the buffer layer and reducing the production cost, the Au or Ag nano particle has good reflection characteristics on light, light emitted by the active layer and reflected by the L ED surface can be emitted, the light emitting efficiency of a L ED device is improved, the preparation method of the patterned substrate modified by the metal nano particle is simple, and the application range is wide.
Drawings
Fig. 1 is a schematic view of a process for forming metal nanoparticles, wherein 11 is a patterned sapphire substrate and 12 is a metal nanoparticle.
Fig. 2 is a schematic view of AlGaN buffer layer grown on a patterned sapphire substrate L ED decorated with metal nanoparticles, wherein 11 is the patterned sapphire substrate, 12 is the metal nanoparticles, and 13 is the buffer layer.
Fig. 3 is an X-ray rocking curve (XRC) for L ED epitaxial wafers, where (a) is the X-ray rocking curve (XRC) for L ED epitaxial wafers without metal nanoparticles of the prior art, and (b) is the X-ray rocking curve for L ED epitaxial wafers prepared in example 1.
Fig. 4 is a photoluminescence (P L) spectrum of L ED epitaxial wafers prepared in example 1.
Detailed Description
The invention provides a preparation method of a patterned substrate L ED modified by metal nanoparticles, which comprises the following steps:
1) forming a layer of metal film on the patterned substrate, rapidly heating to 750-1200 ℃, and annealing for 1-10min to form metal nanoparticles on the patterned substrate;
2) transferring the substrate to an MOCVD growth chamber, and growing a buffer layer;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned substrate L ED modified by the metal nanoparticles.
Preferably, the specific method of the metal nanoparticle form is to use an electron beam evaporation device to evaporate an Au thin film or an Ag thin film on the patterned substrate, wherein the evaporation current is 100-150A, and the vacuum is 1 × 10-6-1×10-3Pa, in N2Under the protective atmosphere, rapidly heating to 750-And 5-5min, forming Au nano particles or Ag nano particles on the patterned substrate.
Preferably, the specific method for the metal nanoparticle form is: placing the patterned substrate In an MOCVD growth chamber, introducing an In metal organic substance or an Al metal organic substance at the temperature of 400-600 ℃ and the flow rate of 350-600sccm, laying an In thin film or an Al thin film, and then, keeping the vacuum degree to be more than 10-3Under the condition of Pa, rapidly heating to 750-1200 ℃, and annealing for 1-10min to form In nanoparticles or Al nanoparticles on the patterned substrate.
Fig. 1 is a schematic view of a process for forming Ag metal nanoparticles, wherein 11 is a patterned sapphire substrate, and 12 is a metal nanoparticle; firstly, a layer of Ag metal film is deposited on a patterned sapphire substrate, and then N is deposited2And (3) under a protective atmosphere, performing high-temperature rapid annealing to obtain the Ag metal nanoparticles.
Fig. 2 is a schematic view of AlGaN growing on a patterned sapphire substrate L ED modified by metal nanoparticles, 11 is the patterned sapphire substrate, 12 is the metal nanoparticles, and 13 is a buffer layer.
Example 1
A method for preparing a patterned substrate L ED decorated by metal nano-particles comprises the following steps:
1) evaporating an Ag film with a thickness of 10nm on the patterned sapphire substrate by using an electron beam evaporation device, wherein the evaporation current is 120A, and the vacuum is 1 × 10-4Pa, in N2Rapidly heating to 800 ℃ under the protective atmosphere, and annealing for 1min to form Ag nano particles with the diameter of 3nm on the patterned substrate;
2) transferring the AlGaN buffer layer to an MOCVD growth chamber, and growing the AlGaN buffer layer with the thickness of 5 nm;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned sapphire substrate L ED modified by the metal nanoparticles.
FIG. 3 shows the X-ray rocking curves of L ED epitaxial wafers, where (a) is the X-ray rocking curve (XRC) of L ED epitaxial wafers without metal nanoparticles of the prior art and (b) is the X-ray rocking curve of L ED epitaxial wafers prepared in example 1 As shown in (b) of FIG. 3, the half-peak XRC width of L ED epitaxial wafers prepared in example 1 is 201arcsec, which is superior to L ED epitaxial wafers without Ag nanoparticles (244 arcsec c).
Fig. 4 is a P L spectrum of L ED epitaxial wafer prepared in example 1, which has strength 1.5-2 times higher than that of L ED epitaxial wafer without Ag nanoparticles, and light extraction efficiency is improved by 3-5%.
Example 2
A method for preparing a patterned substrate L ED decorated by metal nano-particles comprises the following steps:
1) evaporating an Au thin film with the thickness of 6nm on the patterned sapphire substrate by using electron beam evaporation equipment, wherein the evaporation current is 100A, and the vacuum is 1 × 10-3Pa, in N2Under the protective atmosphere, rapidly heating to 750 ℃, and annealing for 5min to form Au nanoparticles with the diameter of 2nm on the patterned substrate;
2) transferring the substrate to an MOCVD growth chamber, and growing an AlN buffer layer with the thickness of 2 nm;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned sapphire substrate L ED modified by the metal nanoparticles.
Example 3
A method for preparing a patterned substrate L ED decorated by metal nano-particles comprises the following steps:
1) evaporating an Au thin film with the thickness of 15nm on the patterned sapphire substrate by using an electron beam evaporation device, wherein the evaporation current is 150A, and the vacuum is 1 × 10-5Pa, in N2Under the protective atmosphere, rapidly heating to 1000 ℃, and annealing for 2min to form Au nano particles with the diameter of 5nm on the patterned sapphire substrate;
2) transferring the substrate to an MOCVD growth chamber, and growing an AlN buffer layer with the thickness of 8 nm;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned sapphire substrate L ED modified by the metal nanoparticles.
Example 4
A method for preparing a patterned substrate L ED decorated by metal nano-particles comprises the following steps:
1) placing the graphical sapphire substrate In an MOCVD growth chamber, introducing trimethyl indium at the temperature of 400 ℃ at the flow rate of 350sccm, laying an In film with the thickness of 12nm, and then, under the vacuum degree of more than 10-3Under the condition of Pa, rapidly heating to 900 ℃, and annealing for 1min to form In nano particles with the diameter of 3nm on the patterned substrate;
2) transferring the substrate to an MOCVD growth chamber, and growing an AlN buffer layer with the thickness of 5 nm;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned sapphire substrate L ED modified by the metal nanoparticles.
Example 5
A method for preparing a patterned substrate L ED decorated by metal nano-particles comprises the following steps:
1) placing the graphical sapphire substrate in an MOCVD growth chamber, introducing trimethylaluminum at the temperature of 500 ℃ at the flow rate of 500sccm, laying an Al thin film with the thickness of 15nm, and then, under the vacuum degree of more than 10-3Under the condition of Pa, rapidly heating to 1000 ℃, and annealing for 5min to form Al nano particles with the diameter of 5nm on the patterned substrate;
2) transferring the AlGaN buffer layer to an MOCVD growth chamber, and growing the AlGaN buffer layer with the thickness of 10 nm;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned sapphire substrate L ED modified by the metal nanoparticles.
Example 6
A method for preparing a patterned substrate L ED decorated by metal nano-particles comprises the following steps:
1) placing the graphical sapphire substrate in an MOCVD growth chamber, introducing diethyl aluminum at 600 ℃ at a flow rate of 600sccm, laying an Al thin film with the thickness of 20nm, and then, under the vacuum degree of more than 10-3Under the condition of Pa, quickly raising the temperature to 1200 ℃, and removingFiring for 8min to form Al nano particles with the diameter of 6nm on the patterned substrate;
2) transferring the substrate to an MOCVD growth chamber, and growing an AlN buffer layer with the thickness of 12 nm;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum well, AlGaN electron barrier layer and p-type GaN to obtain the patterned sapphire substrate L ED modified by the metal nanoparticles.
Claims (5)
1. A method for preparing a patterned substrate L ED decorated by metal nano-particles is characterized by comprising the following steps:
1) forming a layer of metal film on the patterned substrate, rapidly heating to 750-1200 ℃, and annealing for 1-10min to form metal nanoparticles with the diameter of 2-6nm on the patterned substrate;
2) transferring the substrate to an MOCVD growth chamber, and growing a buffer layer with the thickness of 2-20 nm;
3) growing u-type GaN, n-type GaN, InGaN/GaN quantum wells, AlGaN electron blocking layers and p-type GaN to obtain a patterned substrate L ED modified by metal nanoparticles;
the metal film is an Ag film, an Au film, an In film or an Al film; the metal nanoparticles are Ag nanoparticles, Au nanoparticles, In nanoparticles or Al nanoparticles;
in the step 1), the specific method of the metal nano particle form is to use electron beam evaporation equipment to evaporate a layer of Au film or Ag film on the patterned substrate, wherein the evaporation current is 100-150A, and the vacuum is 1 × 10-6-1×10-3Pa, rapidly heating to 750-1200 ℃ under the protection of N, and annealing for 0.5-5min to form Au nanoparticles or Ag nanoparticles on the patterned substrate;
in the step 1), the specific method for the metal nanoparticle form is as follows: placing the patterned substrate In an MOCVD growth chamber, introducing an In metal organic substance or an Al metal organic substance at the temperature of 400-600 ℃ and the flow rate of 350-600sccm, laying an In thin film or an Al thin film, and then, keeping the vacuum degree to be more than 10-3Under the condition of Pa, rapidly heating to 750-1200 ℃, annealing for 1-10min, and then forming In nano particles or Al nano particles on the patterned substrateParticles.
2. The method according to claim 1, wherein the In metallorganics are trimethyl indium or diethyl indium; the Al metal organic matter is trimethyl aluminum or diethyl aluminum.
3. The production method according to claim 1, wherein in the step 2), the buffer layer is an AlN buffer layer or an AlGaN buffer layer.
4. The production method according to claim 1, wherein the thickness of the metal thin film is 6 to 30 nm.
5. The method of manufacturing according to claim 1, wherein the patterned substrate is a patterned sapphire substrate.
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