CN104576849B - Method for improving ultraviolet light intensity of ZnO micron line/nano wire - Google Patents
Method for improving ultraviolet light intensity of ZnO micron line/nano wire Download PDFInfo
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- CN104576849B CN104576849B CN201410812473.1A CN201410812473A CN104576849B CN 104576849 B CN104576849 B CN 104576849B CN 201410812473 A CN201410812473 A CN 201410812473A CN 104576849 B CN104576849 B CN 104576849B
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- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 41
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 41
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 41
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 41
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 41
- 239000002131 composite material Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 239000010408 film Substances 0.000 claims description 17
- 238000010894 electron beam technology Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000010409 thin film Substances 0.000 claims description 9
- 230000002708 enhancing effect Effects 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 abstract description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 4
- 239000012528 membrane Substances 0.000 abstract 2
- YTCQFLFGFXZUSN-BAQGIRSFSA-N microline Chemical compound OC12OC3(C)COC2(O)C(C(/Cl)=C/C)=CC(=O)C21C3C2 YTCQFLFGFXZUSN-BAQGIRSFSA-N 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 2
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 111
- 239000011787 zinc oxide Substances 0.000 description 60
- 238000004020 luminiscence type Methods 0.000 description 12
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- 229910000510 noble metal Inorganic materials 0.000 description 2
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- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 241000764238 Isis Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- H01L33/005—Processes
- H01L33/0083—Processes for devices with an active region comprising only II-VI compounds
- H01L33/0087—Processes for devices with an active region comprising only II-VI compounds with a substrate not being a II-VI compound
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- Luminescent Compositions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for improving the ultraviolet light intensity of a ZnO micron line/nano wire, and relates to application of an optoelectronic system and a light emitting device based on a ZnO micron/nano structure in fields such as semiconductor techniques, biomedicine and energy environment. The method comprises the following steps: washing a substrate, namely, performing ultrasonic washing on a substrate which takes single crystal silicon wafer as a composite base by using acetone and ethanol respectively; growing an Au membrane layer with the thickness of 60-70nm on a Si substrate; growing a SiO2 film layer as a medium layer on the Au membrane, thereby obtaining a Si-Au-SiO2 composite base, wherein the thickness of the SiO2 film is 5-100nm, the thickness of the SiO2 film with the most remarkable ultraviolet intensification effect is 5-10nm (or the thickness of the SiO2 film is 5-10nm); putting the micron line/nano wire with the ＜0001＞ orientation into an ethanol solution or distilled water, performing ultrasonic dispersion for 3-5 minutes, and dropping on the Si-Au-SiO2 composite base by using a dropper. The ultraviolet light intensity of the ZnO micro line/nano wire on the composite base is remarkably improved when being compared with that of a ZnO micro line/nano wire without a composite base.
Description
Technical field
The present invention is to adopt Si-Au-SiO2Composite substrate, strengthens the ultra-violet light-emitting intensity of ZnO micro wire and nano wire
A kind of design, preparation technology and detection technique, the Au film thickness in composite substrate is 60～70nm, SiO2Film thickness
For 5～10nm.The present invention promotes electro-optical system based on ZnO micro-nano structure and luminescent device in semiconductor technology, biomedical,
The application in the fields such as energy environment.
Background technology
Zinc oxide (ZnO) is the direct wide band gap semiconducter of hexagonal wurtzite structure, and energy gap is 3.37eV, corresponding purple
Outer luminescence band, exciton bind energy is up to 60meV.The preparation process is simple of ZnO nano-wire, low cost, there is strong exciton effect
Should.Based on the functional device of ZnO nano-wire, such as nano laser, photoelectron detector, field effect transistor, biosensor, light is urged
Change, solaode etc. becomes the focus material of optoelectronic areas research, there is important application showing and be widely applied
Prospect.
ZnO material easily produces the crystal defects such as Lacking oxygen in growth so as to radiative transistion probability and luminescent properties drop
Low.How to improve its luminous efficiency is problem demanding prompt solution in application.By improving structure and the technique of material, can improve
The quality of ZnO material/device and luminous efficiency, but it is subject to material band structure itself, and growing technology and substrate etc. limit,
It is difficult to make the luminous efficiency of ZnO to increase substantially.
In recent years, people begin attempt to metallic surface plasma excimer (Surface plasmon polarition,
SPP) coupling strengthens photoemissive characteristic, strengthens the light emission effciency of semiconductive luminescent materials.SPP is the freely electricity of metal surface
Interaction after son occurs collective oscillation under light or electron irradiation, and light wave electromagnetic field between.Using metal surface etc. from
The local fields of excimer and coupling effect, can improve the Photon state density at semiconductor light emitting center, strengthen semiconductor microactuator micro-nano structure
Local electromagnetic field, improves the radiative transistion probability of material.Therefore, sent out using the light that SPP structure has become enhancing semi-conducting material
Penetrate, and change the effective means of the band structure/wavelength of semi-conducting material, cause the great interest of people and extensive pass
Note.
According to document report, using the noble metals such as Au and Ag local surface plasma (include nano-particle, island,
Cellular and raster-like thin film) resonance coupling, ZnO film and nano-wire array can be strengthened, the mono- quantum of GaAs, InGaN quantum
Trap, Si quantum dot, the fluorescence of LED and Schottky diode or electroluminescent intensity, and modulate the wavelength of the nano wires such as CdS.
For avoiding emitting semiconductor and Au, the noble metal SPP structure such as Ag, Pt, Cu closely causes energy transfer to quench very much because of distance
Go out, sealing coat can be added between quasiconductor and metal film SPP, such as semi-conducting material GaN, organic material PMMA, or dielectric
Material SiO2Deng, make carrier the interface of dielectric layer and semiconductor microactuator micro-nano structure accumulate, thus further enhance metal SPP knot
The free electron of structure and the interaction of photon, form high local fields and the close coupling of metal surface phasmon, produce resonance,
Strengthen the light emitting performance of semi-conducting material.
Content of the invention
The present invention prepares a kind of Si-Au-SiO2Composite substrate, strengthens the design of ZnO micro wire and nano wire luminous intensity
Scheme and preparation method.
A kind of method of enhancing ZnO micro wire/nano wire ultra-violet light-emitting intensity is it is characterised in that enter according to following steps
OK：
One. the cleaning of substrate：It is the substrate in composite substrate using monocrystalline silicon piece, be respectively adopted acetone and ethanol is surpassed
Sound wave cleans；
The preparation of two .Au thin film：Using magnetron sputtering technique, growth a layer thickness is the Au of 60～70nm on a si substrate
Film；
Three .SiO2The preparation of dielectric layer：One layer of SiO is grown on Au film2Thin film, as dielectric layer, obtains Si-Au-SiO2
Composite substrate, SiO2Film thickness is 5～100nm；
The selection of four .ZnO nano wires：Using having<0001>The ZnO nano-wire of orientation or micro wire, diameter is respectively 1
～3 μm and 200～500nm, length is 20～600 μm；
Five. ZnO micro wire/nano wire is put in ethanol solution or distilled water, disperses through ultrasound wave after 3～5min, use
Dropper drops in Si-Au-SiO2In composite substrate.
Further, SiO2The thickness of thin film is 5～100nm.When thickness is 5～10nm, obtains ultra-violet light-emitting the strongest and increase
Potent fruit.
Further, excite the ultra-violet light-emitting peak of ZnO nano-wire, accelerating potential is 3～30kV, wherein accelerating potential is 10kV
When, obtain ultra-violet light-emitting reinforced effects the strongest.
Further, excite the ultra-violet light-emitting peak of ZnO micro wire, accelerating potential is 3～30kV, wherein accelerating potential is 15kV
When, obtain ultra-violet light-emitting reinforced effects the strongest.
Using the cathode-luminescence spectrometer (CL) of configuration in scanning electron microscope (SEM), check Si-Au-SiO2Composite substrate is to ZnO
The reinforced effects of the ultraviolet light of micro wire/nano wire, the incident electron beam accelerating voltage of SEM is 3～30kV, and incident electron stream is
10-8～10-10A, operating distance be 12.5～13mm, enlargement ratio be 4000 ×～20,000 ×～, lens isis be 40～
100 μm, electric current beam spot is 3～5；Photomultiplier tube detectors (PMT) voltage of CL spectrometer is 500～1500V, fluorescence detection ripple
A length of 200～960nm, diffraction grating is 1200mm/l, and slit is 3～5mm, and spectrometer resolution is 0.66nm；Using above-mentioned SEM
With CL test parameter, strong radiative transistion probability, radioluminescence and high detection effect can be produced with excitation nano line/micro wire
Rate, wherein, works as SiO2Thickness is the ultra-violet light-emitting intensity of ZnO micro wire in the composite substrate of 5～10nm and nano wire, than no
The luminous intensity of complex matrix substantially increases, and the ZnO micro wire in the composite substrate of 5nm and the ultra-violet light-emitting intensity of nano wire are divided
Not increased 5 times and 20 times；
Brief description
Fig. 1 is the Si-Au-SiO being prepared by step one to step 42Composite substrate, and the ZnO micron depositing thereon
The schematic diagram of line/nano wire, wherein Au film thickness are 60～70nm, SiO2Film thickness is 5～100nm.ZnO micro wire
A diameter of 1～3 μm, a diameter of 200～500nm of ZnO nano-wire, the length of micro wire and nano wire is 20～600 μm；
The scanning electron microscope (SEM) that Fig. 2 adopts and cathode-luminescence spectrometer (CL) test system (SEM-CL) schematic diagram.In Fig. 2,
1 electron beam, 2 electromagnetic lenses, 3 sample rooms, 4 sample stages, 5 samples, 6 cathode-luminescence spectrometers.
Fig. 3 is located in Si-Au-SiO2ZnO micro wire in composite substrate and the scanning electron microscope secondary electron of nano wire
(SE) as with corresponding cathode-luminescence (CL) as.Fig. 3 (a) and (b) are a diameter of 2.48 μm of SE picture and CL pictures, (c) and (d)
It is SE picture and the CL picture of a diameter of 500nm.
Fig. 4 compares and is placed on Si-Au-SiO2300nm-ZnO nano wire in composite substrate and in monocrystalline substrate
Cathode-luminescence is composed.Fig. 5 compares and is placed on Si-Au-SiO21.6 μm of-ZnO micro wires in composite substrate and in monocrystalline substrate
Cathode-luminescence spectrum.
Fig. 6 is using different SEM incident electron beam energies, excites the ultra-violet light-emitting peak of 300nm-ZnO nano wire.
Fig. 7 is using different SEM incident electron beam energies, excites the ultra-violet light-emitting peak of 1.6 μm of-ZnO micro wires.
Specific embodiment
One. the cleaning of substrate：Using<100>The n-type monocrystalline silicon piece of orientation is the substrate in composite substrate, is respectively adopted
Acetone and ethanol, carry out ultrasound wave and clean each 5min；
The preparation of two .Au thin film：Using magnetron sputtering technique, growth a layer thickness is the Au of 60～70nm on a si substrate
Film, sputtering power is 250W, and speed is 0.46nm/s, vacuum is 10mtorr, and Ar throughput is 40scum；
3rd, SiO2The preparation of dielectric layer：Using PECVD technique, one layer of SiO of regrowth on Au film2Thin film is as medium
Layer, obtains Si-Au-SiO2Composite substrate, SiO2Film thickness is respectively 5nm, and 10nm, 20nm and 100nm are thick.
4th, the selection of ZnO nano-wire：Using having<0001>The ZnO nano-wire of orientation and micro wire, diameter is respectively 1
～3 μm and 200～500nm, length is 20～600 μm；
5th, ZnO micro wire/nano wire is put in ethanol solution or distilled water, disperse through ultrasound wave after 3～5min, use
Dropper drops in Si-Au-SiO2In composite substrate；
Fig. 1 is the Si-Au-SiO being prepared by step one to step 42Composite substrate, and the ZnO micron depositing thereon
The schematic diagram of line/nano wire, wherein Au film thickness are 60～70nm, SiO2Film thickness is 5～100nm.ZnO micro wire
A diameter of 1～3 μm, a diameter of 200～500nm of ZnO nano-wire, the length of micro wire and nano wire is 20～600 μm；
The scanning electron microscope (SEM) that Fig. 2 adopts and cathode-luminescence spectrometer (CL) test system (SEM-CL) schematic diagram.Scanning electricity
The electron beam launched in mirror electron gun, after electromagnetic lenses focusing, incides sample surfaces, excites solid luminescent material to produce
Bear substantial amounts of electron-hole pair, electron-hole composed emission photon, photon is by the parabola of CL spectrometer front end or semielliptical
Face mirror receives, then through reflecting mirror and diffraction grating light splitting, is received by photomultiplier tube (PMT) or charge-coupled device (CCD) probe
Collection, is finally shown in the form of CL picture or spectrum.In Fig. 2,1 electron beam, 2 electromagnetic lenses, 3 sample rooms, 4 samples
Platform, 5 samples, 6 cathode-luminescence spectrometers
Fig. 3 is located in Si-Au-SiO2ZnO micro wire in composite substrate and the scanning electron microscope secondary electron of nano wire
(SE) as with corresponding cathode-luminescence (CL) as.Fig. 3 (a) and (b) are a diameter of 2.48 μm of SE picture and CL pictures, (c) and (d)
It is SE picture and the CL picture of a diameter of 500nm.
Fig. 4 compares and is placed on Si-Au-SiO2300nm-ZnO nano wire in composite substrate and in monocrystalline substrate
Cathode-luminescence is composed.Si-Au-SiO2SiO in composite substrate2Thickness of dielectric layers is respectively 5,10,20 and 100nm, and test negative electrode is glimmering
The test parameter of spectrum：Accelerating potential is 10kV, and incident current is 10-9A, beam spot is 5, and operating distance is 12.6mm.Obtained by Fig. 4
Know：(1) the intrinsic peak of the ultraviolet emission of ZnO nano-wire is 387nm；(2)SiO2Thickness of dielectric layers is in the composite substrate of 5nm
Lighting of ZnO nano-wire is the strongest, compared with Si substrate, 5nm, 10nm, 20nm thickness SiO2Composite substrate on ZnO micro wire
Luminous intensity is respectively 20 times, 2.8 times, 1.8 times, 100nm thickness SiO2Composite substrate on the luminous intensity of ZnO nano-wire with
The luminous intensity of the ZnO nano-wire in monocrystalline substrate is essentially identical.Learnt by Fig. 4, using the SiO that 5～10nm is thick2Medium
Layer significantly improves the ultra-violet light-emitting intensity of ZnO nano-wire.
Fig. 5 compares and is placed on Si-Au-SiO21.6 μm of-ZnO micro wires in composite substrate and in monocrystalline substrate
Cathode-luminescence is composed.Si-Au-SiO2SiO in composite substrate2Thickness of dielectric layers is respectively 5,10,20 and 100nm.Accelerating potential is
15kV.Same Fig. 4 of other test parameters of cathode-luminescence spectrum.Learnt by Fig. 5：(1) the intrinsic peak of the ultraviolet emission of ZnO micro wire is
392nm；(2)SiO2Thickness of dielectric layers is the luminous the strongest of ZnO micro wire in the composite substrate of 5nm, compared with Si substrate, 5nm,
10nm, 20nm and 100nm thickness SiO2Composite substrate on ZnO micro wire luminous intensity be respectively 5 times, 4.8 times, 2.5 times
With 1.3 times.Test result shows, using Si-Au-SiO2Composite substrate, makes the ultra-violet light-emitting intensity of ZnO micro wire substantially carry
Height, this is that Au-SPP structure couples the resonance enhancement producing with ZnO micro wire.Using the SiO that 5nm is thick2Dielectric layer is isolated
Metal SPP structure and ZnO micro wire, can be effectively increased the recombination probability of carrier, make the luminescence enhancement effect of ZnO micro wire
The most obvious.The test result of Fig. 4 and Fig. 5 shows, using Si-Au-SiO2Composite substrate, wherein, SiO2The thickness of dielectric layer is 5
～10nm is hence it is evident that improve the ultra-violet light-emitting intensity of ZnO micro wire and nano wire.
Fig. 6 is using different SEM incident electron beam energies, excites the ultra-violet light-emitting peak of 300nm-ZnO nano wire.Accelerate
Voltage is respectively 3,5,10,15,20 and 30kV.When accelerating potential is for 10kV, the ultra-violet light-emitting of ZnO nano-wire is the strongest, lights
Wavelength is 387nm.This shows, the accelerating potential using 10kV excites ZnO nano-wire, be conducive to improving its radiative transistion probability and
Luminous efficiency.Therefore, the CL spectrum of test ZnO micro wire employs the accelerating potential (Fig. 4) of 10kV.
Fig. 7 is using different SEM incident electron beam energies, excites the ultra-violet light-emitting peak of 1.6 μm of-ZnO micro wires.Accelerate
Voltage is respectively 3,5,10,15,20 and 30kV, the same Fig. 4 of other test parameter.When accelerating potential is for 15kV, ZnO micro wire
Ultra-violet light-emitting is the strongest, and emission wavelength is 392nm.This shows：(1) ZnO micro wire is excited using the accelerating potential of 15kV, be conducive to
Improve its radiative transistion probability and luminous efficiency.Therefore, the CL spectrum of test ZnO micro wire employs the accelerating potential (figure of 15kV
5)；(2) compared with ZnO micro wire, the intrinsic emitter peak blue shift of ZnO nano-wire 5nm, this is that the core-shell structure of nano wire is made
Nanowire surface is become to have differences with center portion band gap, surface compression stress makes the band gap of nano wire narrow, spectral peak blue shift.
Claims (5)
1. a kind of method of enhancing ZnO micro wire/nano wire ultra-violet light-emitting intensity is it is characterised in that follow the steps below：
One. the cleaning of substrate：It is the substrate in composite substrate using monocrystalline silicon piece, carry out ultrasound wave cleaning；
The preparation of two .Au thin film：Using magnetron sputtering technique, growth a layer thickness is the Au film of 60～70nm on a si substrate；
Three .SiO2The preparation of dielectric layer：One layer of SiO is grown on Au film2Thin film, as dielectric layer, obtains Si-Au-SiO2Compound
Substrate, SiO2Film thickness is 5～100nm；
The selection of four .ZnO nano wires：Using having<0001>Orientation ZnO nano-wire or micro wire, diameter be respectively 200～
500nm and 1～3 μm, length is 20～600 μm；
Five. ZnO micro wire/nano wire is put in ethanol solution or distilled water, disperses through ultrasound wave after 3～5min, use dropper
Drop in Si-Au-SiO2In composite substrate.
2. the method for a kind of enhancing ZnO micro wire/nano wire ultra-violet light-emitting intensity according to claim 1, its feature exists
In：
SiO2The thickness of thin film is 5～10nm, obtains ultra-violet light-emitting reinforced effects the strongest.
3. the method for a kind of enhancing ZnO micro wire/nano wire ultra-violet light-emitting intensity according to claim 1, its feature exists
In：
The electron beam launched using scanning electron microscope electron rifle, after electromagnetic lenses focusing, is incided sample surfaces, excites ZnO
The ultra-violet light-emitting peak of micro wire/nano wire, accelerating potential is 3～30kV.
4. the method for a kind of enhancing ZnO micro wire/nano wire ultra-violet light-emitting intensity according to claim 3, its feature exists
In：
For ZnO nano-wire, when accelerating potential is 10kV, obtain ultra-violet light-emitting reinforced effects the strongest.
5. the method for a kind of enhancing ZnO micro wire/nano wire ultra-violet light-emitting intensity according to claim 3, its feature exists
In：
For ZnO micro wire, when accelerating potential is 15kV, obtain ultra-violet light-emitting reinforced effects the strongest.
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| CN102477291A (en) * | 2010-11-23 | 2012-05-30 | 海洋王照明科技股份有限公司 | Preparation method of ZnO nano-rod array |
| CN102957086A (en) * | 2012-10-25 | 2013-03-06 | 电子科技大学 | Deep sub-wavelength surface plasma laser |
| US8574948B2 (en) * | 2010-08-27 | 2013-11-05 | Iowa State University Research Foundation, Inc. | Method of improving power conversion efficiencies in dye-sensitized solar cells by facile surface treatment |
| CN103746056A (en) * | 2013-12-28 | 2014-04-23 | 华中科技大学 | Wave length-adjustable light-emitting diode based on gallium-doped zinc oxide nanowire array and manufacturing method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8574948B2 (en) * | 2010-08-27 | 2013-11-05 | Iowa State University Research Foundation, Inc. | Method of improving power conversion efficiencies in dye-sensitized solar cells by facile surface treatment |
| CN102477291A (en) * | 2010-11-23 | 2012-05-30 | 海洋王照明科技股份有限公司 | Preparation method of ZnO nano-rod array |
| CN102957086A (en) * | 2012-10-25 | 2013-03-06 | 电子科技大学 | Deep sub-wavelength surface plasma laser |
| CN103746056A (en) * | 2013-12-28 | 2014-04-23 | 华中科技大学 | Wave length-adjustable light-emitting diode based on gallium-doped zinc oxide nanowire array and manufacturing method thereof |
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