CN104868023A - III-nitride semiconductor/quantum dot hybrid white light LED device and preparing method thereof - Google Patents
III-nitride semiconductor/quantum dot hybrid white light LED device and preparing method thereof Download PDFInfo
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- CN104868023A CN104868023A CN201510237489.9A CN201510237489A CN104868023A CN 104868023 A CN104868023 A CN 104868023A CN 201510237489 A CN201510237489 A CN 201510237489A CN 104868023 A CN104868023 A CN 104868023A
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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
- H01L33/04—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 quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—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 quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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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
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Abstract
The invention discloses an III-nitride semiconductor/quantum dot hybrid white light LED device. According to the invention, an ordered nano-pore array is arranged outside the regions of a p type electrode and an n type electrode. The nano-pore array penetrates from the surface of the device through a quantum well active layer to the inner part of an n type nitride layer. The nano-pore array is internally filled with II-VI quantum dots. The invention further discloses a preparing method of the III-nitride semiconductor/quantum dot hybrid white light LED device. Non-radiative composite energy transferring between an indium gallium nitrogen (InGaN) quantum well and excitons in the II-VI quantum dots is utilized by the device to improved the light emitting efficiency of the device; in addition, by changing the types and the ratio of the filling quantum dots, the wavelength and the intensity of emitted light is adjusted, and the white light LED device with the nitride/quantum dot hybrid structure is capable of realizing a superhigh color rendering index.
Description
Technical field
The present invention relates to a kind of III nitride semiconductor/quantum dot mixed white light LED component with and preparation method thereof, belong to field of semiconductor illumination.
Background technology
III-nitride material is direct gap semiconductor, and its band gap covers from infrared visible ray to ultraviolet band, is the ideal material realizing solid-state illumination and low power consumption display.Solid-state illumination is a brand-new lighting field, and it is mainly light emitting source with semiconductor chip, and directly convert electrical energy into luminous energy, conversion efficiency is high.LED is as the core component of solid-state illumination semiconductor light sources, and having that energy consumption is low, the life-span is long, volume is little, environmental protection, use safety, can to work under various adverse circumstances, is the lighting source of new generation after incandescent lamp, fluorescent lamp.Along with the development of light-emitting diode (LED), solid state illumination technology will progressively replace existing lighting technology, welcome the new illumination epoch.
Current white light LEDs element major technique is blue-ray LED+yellow fluorescent powder (as: YAG) or ultraviolet LED+three-color phosphor, because its process costs is lower, is extensively adopted by industrial quarters.But the inevitable shortcoming of this fluorescent material scheme comprises: self-absorption, long-time decay, yellow fluorescence pink colour conversion efficiency are low.What is more important, the existing LED chip based on the conversion of fluorescent material light, along with the increase of injected current density, radiation recombination efficiency does not improve, and non-radiative recombination increases, as auger recombination, defect compound etc., therefore, under large injection condition, the luminous efficiency of LED progressively declines, and in experiment, this phenomenon is called droop effect.
Although researchers have employed a lot of method, as the mqw active layer, AlGaN potential barrier barrier layer, GaN isoepitaxial growth etc. of non-polar plane growth, can partial reduction or eliminate quantum limit Stokes effect, but droop effect still still cannot overcome.In order to weaken quantum limit Stokes effect and droop effect further, improve the luminous efficiency of light-emitting diode, preparation nano-pillar (hole) type light-emitting diode is a kind of effective implementation method.In this ordered nano post (hole) type light LED material structure, the stress of active layer structure is discharged, thus reduce the internal electric field of active layer inside, the Spatial Wave Function being conducive to electron hole is overlapping, reduces quantum limit Stokes effect; Add the combined efficiency of electron hole, and this nano-pillar (hole) reduces defect recombination probability simultaneously, be expected to overcome droop effect.
At present, on market, white light LEDs great majority adopt monochromatic light excitated fluorescent powder, utilize photochromic principle to produce white light.Wherein more ripe and business-like be utilize the gallium nitrate based chip of blue light to excite yellow fluorescent powder to obtain white light.But the luminous efficiency of fluorescent material is lower, and spectrum is shaped like narrow, and color rendering is poor, and colour temperature is higher.Therefore, this white light source is not soft, inharmonious to eyes.Another kind of comparatively common LED structure excites red, blue, green three primary colors fluorescent powder to obtain white light by ultraviolet light or purple light chip, and principle is ditto similar.Although can improve color rendering, regulate colour temperature, because the method employs fluorescent material equally, there is the effective transformation efficiency of light low, particularly the efficiency of red fluorescence powder needs significantly to improve.Meanwhile, the poor stability of fluorescent material, affects its useful life greatly.Therefore, the White light LED technology of unstressed configuration powder more and more comes into one's own.From current disclosed unstressed configuration powder White light LED technology (see Chinese patent CN201210052040.1, CN201410422581.8), there is no the nano-pore mixed white light LED device using quantum dot to realize light conversion.
At present, patent documentation CN103383980A discloses one and utilizes the soft nanometer embossing of ultraviolet (UV-NIL) to prepare the method for orderly gallium nitride nanohole array.The method adopts PMMA and the soft impression of ultra-violet curing glue double-layer glue technology ultraviolet to prepare the gallium nitride nano-pillar (hole) of large area, low defect, and utilize reactive ion etching (RIE) technology to realize the adjustable nano-pillar of dielectric layer mask diameter (hole) array, thus realize the adjustable gallium nitride nano-pillar (hole) of diameter.
Summary of the invention
The object of this invention is to provide a kind of white light LED part without the need to fluorescent material.
For reaching goal of the invention, the technical solution used in the present invention is: a kind of white light LED part based on III nitride semiconductor/quantum dot mixing nanostructure, the region of described white light LED part outside p-type electrode and n-type electrode is provided with orderly nanohole array, the degree of depth of nanohole array passes mqw active layer from device surface, until N-shaped nitride layer is inner, in described nanohole array, be filled with II-VI group quantum dot.
Preferably, described device comprises:
One substrate;
N-shaped gallium nitride (GaN) layer of one growth on substrate;
The one indium gallium nitrogen/gallium nitride (In of growth in n-type gallium nitride layer
xga
1-xn/GaN) mqw active layer;
The p-type GaN layer of one growth on mqw active layer;
Tin indium oxide (ITO) layer of one growth on p-type gallium nitride layer;
One p-type electrode, makes on the ito layer;
One n-type electrode, is produced in n-type GaN layer;
One orderly nanohole array, described nanohole array is arranged at ITO layer surface, avoid p-type electrode zone, the degree of depth of nanohole array passes mqw active layer from device surface, until n-type GaN layer is inner, be filled with II-VI group quantum dot in described nanohole array, wherein the color matching formula of quantum dot and white light LED part is:
S
white(λ)＝S
MQW(λ)+k
NC1·S
NC1(λ)+k
NC2·S
NC2(λ)+…，
Wherein S represents Energy distribution; Subscript white, MQW, NC1, NC2 represent white light LEDs, Multiple Quantum Well, the first quantum dot, the second quantum dot respectively; K represents this kind of quantum dot with the peak intensity values after the strong normalization in quantum well radiation peak.
Preferably, described substrate is Sapphire Substrate, described x scope: 0.12≤x≤0.25, and mqw active layer emission wavelength is at 430nm to 480nm, and the periodicity of quantum well 10 ~ 15, the thickness 300 ~ 500nm of p-type GaN layer, ITO layer thickness is 100 ~ 200nm.
Preferably, the diameter of described nanohole array is 100 ~ 260nm, and the cycle is 300 ~ 700nm.
Preferably, described II-VI group quantum dot is from CdSe/ZnS quantum dot, the CdSe of nucleocapsid structure
ys
1-Y/ ZnS quantum dot, and the CdSe quantum dot of mononuclear structure, Zn
zcd
1-Zselect arbitrarily in Te quantum dot, nuclear radius is 1.3 ~ 2.5nm, and shell thickness is 1.4 ~ 2.8nm, and the emission wavelength of quantum dot is 520nm to 650nm, is carried out the emission wavelength of adjusting means by the kind and proportioning regulating filling quantum dot.
Present invention also offers a kind of preparation method of above-mentioned white light LED part, its step comprises:
1) evaporation one deck ITO layer on the InGaN/GaN quantum well LED substrate of emission wavelength 430 ~ 480nm;
2) at ITO layer superficial growth one layer insulating, at surface of insulating layer growth layer of metal rete, SU8 glue and ultra-violet curing glue are spin-coated on metal film layer surface successively, insulating barrier adopts the fine and close insulating material with high-k, and the work function that the metal that metallic diaphragm adopts contacts with gold-half of p-type GaN is mated;
3) utilize UV-NIL technology, use soft template on ultra-violet curing glue, form the ordered nano hole array of gross area;
4) utilize RIE technology, pass into CHF
3and O
2the remnant layer of mist etching ultra-violet curing glue, then with ultra-violet curing glue for mask, utilize RIE technology, pass into O
2sU8 layer is etched, nano-pore array structure is transferred to SU8 layer;
5) adopt inductively coupled plasma etching (ICP) technology, pass into Ar gas etching metallic diaphragm, nano-pore array structure is transferred to metallic diaphragm, removes the SU8 glue of metallic diaphragm nanohole array surface;
6) adopt photoetching technique to make the LED component unit of standard at device surface, remove the metallic diaphragm in the region beyond photoresist, then remove photoresist;
7) photoetching, makes p-type electrode zone at device surface, adopts RIE technology, passes into CF
4and O
2mist etching insulating layer, make the nanohole array of metallic diaphragm be transferred to insulating barrier, remove photoresist;
8) adopt ICP technology, pass into Cl
2mist etching ITO layer with Ar, is transferred to ITO layer by nano-pore array structure from insulating medium layer;
9) adopt ICP technology, pass into Cl
2with the mist of Ar, anisotropic etching p-type gallium nitride layer, mqw active layer, n-type gallium nitride layer, formation runs through ITO layer, p-type gallium nitride layer, mqw active layer, be deep to the nanohole array of n-type gallium nitride layer, sample is placed on inorganic acid, etching injury is removed in aqueous slkali water-bath, then remove remaining insulating barrier;
10) photoetching technique is adopted, evaporation p-type electrode and n-type electrode;
11) the certain density II-VI group quantum dot of proportioning, is spin-coated on device surface.
Preferably, described insulating barrier selects SiO2 or SiNx, and metallic diaphragm selects Ni, Cr or Al.
Preferably, the thickness of insulating layer of growth is 30 ~ 300nm, and metallic diaphragm thickness is 10 ~ 50nm, SU8 glue thickness is 200 ~ 600nm, and ultra-violet curing glue thickness is 30 ~ 300nm.
The present invention utilizes the non-radiative recombination energy trasfer in indium gallium nitrogen (InGaN) quantum well and II-VI quantum dot between exciton, improves device light emitting efficiency; By changing the kind and proportioning of filling quantum dot, emission wavelength and intensity can be regulated, the white light LED part of the nitride/quantum dot mixed structure of superelevation color rendering index can be realized.Adopt the soft stamping technique preparation of ultraviolet, can realize the preparation of large area low cost, overcome the shaggy defect of nitride quantum well LED, nanohole array shape, diameter are adjustable.The nanohole array that the inventive method obtains can keep consistent with the specification of original design template substantially.In addition, this device architecture and technique extend to inorganic/organic mixed hybridization light emitting semiconductor device, and completely compatible with current standard blue light LED component chip fabrication technique, are highly susceptible to being integrated into existing LED and produce line production.
Accompanying drawing explanation
Fig. 1 is step 1 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 2 is step 2 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 3 is step 3 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 4 is step 4 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 5 is step 5 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 6 is step 6 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 7 is step 7 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 8 is step 9 in embodiment 1) the white light LED part structural representation that obtains.
Fig. 9 is step 10 in embodiment 1) the white light LED part structural representation that obtains.
Figure 10 is step 11 in embodiment 1) the white light LED part structural representation that obtains.
Figure 11 is the plan structure schematic diagram of white light LED part.
Figure 12 is the scanning electron microscopy picture of the ordered nano hole array not being mixed into quantum dot in embodiment 1.
Figure 13 is the cross sectional scanning electron micro-image of the white light LED part after being mixed into quantum dot in embodiment 1.
Figure 14 is the transmission electron microscope image on white light LED part surface in embodiment 1, and wherein amplifier section is quantum dot.
Figure 15 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 1.
Figure 16 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 2.
Figure 17 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 3.
Figure 18 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 4.
Figure 19 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 5.
Figure 20 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 6.
Figure 21 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 7.
Figure 22 is the electroluminescence spectrum of the mixed white light LED of high color rendering index (CRI) in embodiment 8.
Figure 23 is the chromaticity coordinates figure of the mixed white light LED of high color rendering index (CRI).
Wherein 1 represent Sapphire Substrate, 2 represent n-type GaN layer, and 3 represent mqw active layer, 4 represent p-type GaN layer, 5 represent ITO layer, and 6 represent insulating barrier, and 7 represent metallic diaphragm, 8 represent SU8 glue, 9 represent ultra-violet curing glue, and 10 represent p-type electrode, and 11 represent n-type electrode, 12 represent nano-pore, and 13 represent quantum dot.
Below in conjunction with accompanying drawing, embodiments of the present invention are further elaborated.
Embodiment
Embodiment 1
As shown in figs. 1-11, the preparation method of this white light LED part, its step comprises:
1) x is selected to be 0.12, emission wavelength is 430nm, the periodicity of quantum well is 10, the InGaN/GaN quantum well LED substrate of the thickness 300nm of p-type GaN, utilize electron beam evaporation technique evaporation one deck ITO layer thereon, thickness is 100nm, then sample is carried out high annealing at quick anneal oven (RTA), annealing temperature 450 DEG C, time 2min;
2) using plasma strengthens chemical vapor deposition method at ITO layer superficial growth one deck SiO
2layer, thickness is 30nm, adopts physical vapor deposition at SiO
2layer superficial growth layer of Ni metallic diaphragm, thickness is 10nm, and SU8 glue thick for 200nm and the thick ultra-violet curing glue of 30nm are spin-coated on Ni metal film layer surface successively;
3) UV-NIL technology is utilized, to prepare in advance and did soft template and the device ultra-violet curing film surface close contact of release treatment, under uviol lamp, fully exposure makes ultra-violet curing adhesive curing, the demoulding subsequently, soft template is separated with device surface, the ultra-violet curing glue-line of device surface is formed the ordered nano hole array of gross area, and nanohole array diameter is 260nm, and the cycle is 600nm;
4) utilize RIE technology, pass into CHF
3and O
2the remnant layer of mist etching ultra-violet curing glue, then with ultra-violet curing glue for mask, utilize RIE technology, pass into O
2sU8 layer is etched, nano-pore array structure is transferred to SU8 layer;
5) adopt ICP technology, pass into Ar gas etching N i metallic diaphragm, nano-pore array structure is transferred to Ni metallic diaphragm, adopt photoresist to remove photoresist liquid or continue to use reactive ion etching technology, remove the SU8 glue of metallic diaphragm nanohole array surface;
6) with acetone, isopropyl alcohol and washed with de-ionized water device, adopt photoetching technique to make the LED component unit of standard at device surface, sample is soaked 30 seconds in mineral acid, removes the Ni metallic diaphragm in the region beyond photoresist, adopt acetone to remove photoresist, pass into O by RIE technology
2remove residual gum, clean, dry;
7) photoetching, makes p-type electrode zone at device surface, adopts RIE technology, passes into CF
4and O
2mist etching SiO
2layer, makes the nanohole array of Ni metallic diaphragm be transferred to SiO
2layer, now p-type electrode zone has photoresist to protect, and is not etched, reactive ion etching condition: the flow CF of reactive ion etching gas
4: 30sccm; O
2: 4sccm, power 30W, pressure 1.0Pa, etch period 1min; Photoresist is removed by method above;
8) adopt ICP technology, pass into Cl
2mist etching ITO layer with Ar, is transferred to ITO layer by nano-pore array structure from insulating barrier, etching condition: Cl
215 ± 10sccm and 50 ± 25sccm is respectively, cavity air pressure: 10 ± 5mTorr, DC bias voltage: 550 ± 60V, RF power, 150 ± 30w, ICP power: 300 ± 200W, frequency 13.56MHz, etch period: 2min with Ar flow;
9) adopt ICP technology, pass into Cl
2with the mist of Ar, anisotropic etching p-type gallium nitride layer, mqw active layer, n-type gallium nitride layer, formed and run through ITO layer, p-type gallium nitride layer, mqw active layer, be deep to the nanohole array of n-type gallium nitride layer, etching parameters: Cl
225 ± 10sccm and 10 ± 3sccm is respectively, cavity air pressure: 10 ± 5mTorr, DC bias voltage: 300 ± 60V, RF power, 50 ± 30w, ICP power: 200 ± 100W, frequency 13.56MHz, etch period: 5min with Ar flow; Sample is placed on inorganic acid, aqueous slkali 40 C water bath heats 5min and remove etching injury, then use hydrofluoric acid to remove remaining insulating barrier;
10) photoetching technique is adopted, evaporation p-type electrode and n-type electrode;
11) matched proportion density is that two amounts of the CdSe/ZnS nucleocapsid structure of 10mg/mL is put in toluene solution, radius/the thickness of its core/shell is 1.3nm/1.4nm and 2.2nm/2.5nm, the emission wavelength of quantum dot is respectively 518nm and 600nm, is spin-coated on device surface.
As shown in figures 10-14, its electroluminescence spectrum as shown in Figure 15 for obtained white light LED part.
Embodiment 2
As shown in figs. 1-11, the preparation method of this white light LED part, its step comprises:
1) x is selected to be 0.25, emission wavelength is 480nm, the periodicity of quantum well is 15, the InGaN/GaN quantum well LED substrate of the thickness 500nm of p-type GaN, utilize electron beam evaporation technique evaporation one deck ITO layer thereon, thickness is 200nm, then sample is carried out high annealing at quick anneal oven (RTA), annealing temperature 600 DEG C, time 10min;
2) using plasma strengthens chemical vapor deposition method in ITO layer superficial growth layer of sin
xlayer, thickness is 300nm, adopts physical vapor deposition at Si
3n
4layer superficial growth one deck Cr metallic diaphragm, thickness is 50nm, and SU8 glue thick for 600nm and the thick ultra-violet curing glue of 300nm are spin-coated on Cr metal film layer surface successively;
3) UV-NIL technology is utilized, to prepare in advance and did soft template and the device ultra-violet curing film surface close contact of release treatment, under uviol lamp, fully exposure makes ultra-violet curing adhesive curing, the demoulding subsequently, soft template is separated with device surface, the ultra-violet curing glue-line of device surface is formed the ordered nano hole array of gross area, and nanohole array diameter is 100nm, and the cycle is 300nm;
4) utilize RIE technology, pass into CHF
3and O
2the remnant layer of mist etching ultra-violet curing glue, then with ultra-violet curing glue for mask, utilize RIE technology, pass into O
2sU8 layer is etched, nano-pore array structure is transferred to SU8 layer;
5) adopt ICP technology, pass into Ar gas etching N i metallic diaphragm, nano-pore array structure is transferred to Ni metallic diaphragm, adopt photoresist to remove photoresist liquid or continue to use reactive ion etching technology, remove the SU8 glue of metallic diaphragm nanohole array surface;
6) with acetone, isopropyl alcohol and washed with de-ionized water device, adopt photoetching technique to make the LED component unit of standard at device surface, sample is soaked 120 seconds in mineral acid, removes the Cr metallic diaphragm in the region beyond photoresist, adopt acetone to remove photoresist, pass into O by RIE technology
2remove residual gum, clean, dry;
7) photoetching, makes p-type electrode zone at device surface, adopts RIE technology, passes into CF
4and O
2mist etching SiO
2layer, makes the nanohole array of Cr metallic diaphragm be transferred to SiO
2layer, now p-type electrode zone has photoresist to protect, and is not etched, reactive ion etching condition: the flow CF of reactive ion etching gas
4: 100sccm; O
2: 20sccm, power 100W, pressure 10Pa, etch period 20min; Photoresist is removed by method above;
8) adopt ICP technology, pass into Cl
2mist etching ITO layer with Ar, is transferred to ITO layer by nano-pore array structure from insulating barrier, etching condition: Cl
215 ± 10sccm and 50 ± 25sccm is respectively, cavity air pressure: 10 ± 5mTorr, DC bias voltage: 550 ± 60V, RF power, 150 ± 30w, ICP power: 300 ± 200W, frequency 13.56MHz, etch period: 6min with Ar flow;
9) adopt ICP technology, pass into Cl
2with the mist of Ar, anisotropic etching p-type gallium nitride layer, mqw active layer, n-type gallium nitride layer, formed and run through ITO layer, p-type gallium nitride layer, mqw active layer, be deep to the nanohole array of n-type gallium nitride layer, etching parameters: Cl
225 ± 10sccm and 10 ± 3sccm is respectively, cavity air pressure: 10 ± 5mTorr, DC bias voltage: 300 ± 60V, RF power, 50 ± 30w, ICP power: 200 ± 100W, frequency 13.56MHz, etch period: 10min with Ar flow; Sample is placed on inorganic acid, aqueous slkali 90 C water bath heats 10min and remove etching injury, then use hydrofluoric acid to remove remaining insulating barrier;
10) photoetching technique is adopted, evaporation p-type electrode and n-type electrode;
11) matched proportion density is that two amounts of the CdSe/ZnS nucleocapsid structure of 10mg/mL is put in toluene solution, radius/the thickness of its core/shell is 1.4nm/1.4nm and 2.5nm/2.8nm, the emission wavelength of quantum dot is respectively 546nm and 621nm, is spin-coated on device surface.
The electroluminescence spectrum of obtained white light LED part as shown in figure 16.
Embodiment 3
As shown in figs. 1-11, the preparation method of this white light LED part, its step comprises:
1) x is selected to be 0.18, emission wavelength is 450nm, the periodicity of quantum well is 12, the InGaN/GaN quantum well LED substrate of the thickness 400nm of p-type GaN, utilize electron beam evaporation technique evaporation one deck ITO layer thereon, thickness is 150nm, then sample is carried out high annealing at quick anneal oven (RTA), annealing temperature 500 DEG C, time 6min;
2) using plasma strengthens chemical vapor deposition method in ITO layer superficial growth layer of sin
xlayer, thickness is 160nm, adopts physical vapor deposition at Si
3n
4layer superficial growth one deck Al metallic diaphragm, thickness is 30nm, and SU8 glue thick for 450nm and the thick ultra-violet curing glue of 160nm are spin-coated on Al metal film layer surface successively;
3) UV-NIL technology is utilized, to prepare in advance and did soft template and the device ultra-violet curing film surface close contact of release treatment, under uviol lamp, fully exposure makes ultra-violet curing adhesive curing, the demoulding subsequently, soft template is separated with device surface, the ultra-violet curing glue-line of device surface is formed the ordered nano hole array of gross area, and nanohole array diameter is 180nm, and the cycle is 700nm;
4) utilize RIE technology, pass into CHF
3and O
2the remnant layer of mist etching ultra-violet curing glue, then with ultra-violet curing glue for mask, utilize RIE technology, pass into O
2sU8 layer is etched, nano-pore array structure is transferred to SU8 layer;
5) adopt ICP technology, pass into Ar gas etching Al metallic diaphragm, nano-pore array structure is transferred to Ni metallic diaphragm, adopt photoresist to remove photoresist liquid or continue to use reactive ion etching technology, remove the SU8 glue of metallic diaphragm nanohole array surface;
6) with acetone, isopropyl alcohol and washed with de-ionized water device, adopt photoetching technique to make the LED component unit of standard at device surface, sample is soaked 80 seconds in mineral acid, removes the Ni metallic diaphragm in the region beyond photoresist, adopt acetone to remove photoresist, pass into O by RIE technology
2remove residual gum, clean, dry;
7) photoetching, makes p-type electrode zone at device surface, adopts RIE technology, passes into CF
4and O
2mist etching SiO
2layer, makes the nanohole array of Al metallic diaphragm be transferred to SiO
2layer, now p-type electrode zone has photoresist to protect, and is not etched, reactive ion etching condition: the flow CF of reactive ion etching gas
4: 60sccm; O
2: 10sccm, power 60W, pressure 5Pa, etch period 10min; Photoresist is removed by method above;
8) adopt ICP technology, pass into Cl
2mist etching ITO layer with Ar, is transferred to ITO layer by nano-pore array structure from insulating barrier, etching condition: Cl
215 ± 10sccm and 50 ± 25sccm is respectively, cavity air pressure: 10 ± 5mTorr, DC bias voltage: 550 ± 60V, RF power, 150 ± 30w, ICP power: 300 ± 200W, frequency 13.56MHz, etch period: 4min with Ar flow;
9) adopt ICP technology, pass into Cl
2with the mist of Ar, anisotropic etching p-type gallium nitride layer, mqw active layer, n-type gallium nitride layer, formed and run through ITO layer, p-type gallium nitride layer, mqw active layer, be deep to the nanohole array of n-type gallium nitride layer, etching parameters: Cl
225 ± 10sccm and 10 ± 3sccm is respectively, cavity air pressure: 10 ± 5mTorr, DC bias voltage: 300 ± 60V, RF power, 50 ± 30w, ICP power: 200 ± 100W, frequency 13.56MHz, etch period: 8min with Ar flow; Sample is placed on inorganic acid, aqueous slkali 60 C water bath heats 8min and remove etching injury, then use hydrofluoric acid to remove remaining insulating barrier;
10) photoetching technique is adopted, evaporation p-type electrode and n-type electrode;
11) matched proportion density is that two amounts of the CdSe mononuclear structure of 10mg/mL is put in toluene solution, and its nuclear radius is 1.3nm and 2.2nm, and the emission wavelength of quantum dot is respectively 520nm and 620nm, is spin-coated on device surface.
The electroluminescence spectrum of obtained white light LED part as shown in figure 17.
Embodiment 4
This embodiment step and embodiment 3 basically identical, its difference is that quantum dot selects the sub-point of the two amounts of CdSeS/ZnS nucleocapsid structure, radius/the thickness of its core/shell is 1.3nm/1.4nm and 2.7nm/2.9nm, and the emission wavelength of quantum dot is respectively 520nm and 650nm, is spin-coated on device surface.
The electroluminescence spectrum of obtained white light LED part as shown in figure 18.
Embodiment 5
This embodiment step and embodiment 3 basically identical, its difference is that quantum dot selects the sub-point of the two amounts of ZnCdTe mononuclear structure, and the radius of its core is 1.5nm and 2.5nm, and the emission wavelength of quantum dot is respectively 530nm and 610nm, is spin-coated on device surface.
The electroluminescence spectrum of obtained white light LED part as shown in figure 19.
Embodiment 6
This embodiment step and embodiment 3 basically identical, its difference is that the x of InGaN/GaN quantum well LED substrate is 0.22, emission wavelength is 465nm, the periodicity of quantum well is 10, the thickness of p-type GaN is 200nm, and quantum dot selects the sub-point of the two amounts of ZnCdTe mononuclear structure and CdSeS/ZnS nucleocapsid structure, and wherein the nuclear radius of ZnCdTe is 1.5nm, emission wavelength is 530nm, the nuclear radius of CdSeS/ZnS is 2.7nm, shell radius is 2.9nm, emission wavelength is 650nm, is spin-coated on device surface.
The electroluminescence spectrum of obtained white light LED part as shown in figure 20.
Embodiment 7
This embodiment step and embodiment 6 basically identical, its difference is that quantum dot selects three kinds of quantum dots of CdSe, ZnCdTe mononuclear structure and CdSe/ZnS nucleocapsid structure, wherein the nuclear radius of CdSe is 1.3nm, emission wavelength is 520nm, the nuclear radius of ZnCdTe is 2.5nm, emission wavelength is 610nm, the nuclear radius of CdSe/ZnS is 1.8nm, shell radius is 2.2nm, emission wavelength is 586nm, is spin-coated on device surface.
The electroluminescence spectrum of obtained white light LED part as shown in figure 21.
Embodiment 8
This embodiment step and embodiment 3 basically identical, its difference is that the x of InGaN/GaN quantum well LED substrate is 0.16, emission wavelength is 440nm, the periodicity of quantum well is 10, the thickness of p-type GaN is 200nm, quantum dot selects the quantum dot of CdSeS/ZnS and CdSe/ZnS two kinds of nucleocapsid structures, the nuclear radius of CdSeS/ZnS is 1.3nm, shell radius is 1.4nm, emission wavelength is 520nm, the nuclear radius of CdSe/ZnS is 2.2nm, shell radius is 2.5nm, emission wavelength is 600nm, is spin-coated on device surface.The electroluminescence spectrum of obtained white light LED part as shown in figure 22.
Claims (8)
1. III nitride semiconductor/quantum dot mixed white light LED component, it is characterized in that: the region of described white light LED part outside p-type electrode and n-type electrode is provided with orderly nanohole array, the degree of depth of nanohole array passes mqw active layer from device surface, until N-shaped nitride layer is inner, in described nanohole array, be filled with II-VI group quantum dot.
2. white light LED part according to claim 1, is characterized in that: described device comprises:
One substrate;
The n-type GaN layer of one growth on substrate;
One In of growth in n-type gallium nitride layer
xga
1-xn/GaN mqw active layer;
The p-type GaN layer of one growth on mqw active layer;
The ITO layer of one growth on p-type gallium nitride layer;
One p-type electrode, makes on the ito layer;
One n-type electrode, is produced in n-type GaN layer;
One orderly nanohole array, described nanohole array is arranged at ITO layer surface, avoid p-type electrode zone, the degree of depth of nanohole array passes mqw active layer from device surface, until n-type GaN layer is inner, be filled with II-VI group quantum dot in described nanohole array, wherein the color matching formula of quantum dot and white light LED part is:
S
white(λ)＝S
MQW(λ)+k
NC1·S
NC1(λ)+k
NC2·S
NC2(λ)+…，
Wherein S represents Energy distribution; Subscript white, MQW, NC1, NC2 represent white light LEDs, Multiple Quantum Well, the first quantum dot, the second quantum dot respectively; K represents this kind of quantum dot with the peak intensity values after the strong normalization in quantum well radiation peak.
3. white light LED part according to claim 2, it is characterized in that: described substrate is Sapphire Substrate, described x scope: 0.12≤x≤0.25, mqw active layer emission wavelength is at 430nm to 480nm, the periodicity of quantum well 10 ~ 15, thickness 300 ~ the 500nm of p-type GaN layer, ITO layer thickness is 100 ~ 200nm.
4. white light LED part according to claim 3, is characterized in that: the diameter of described nanohole array is 100 ~ 260nm, and the cycle is 300 ~ 700nm.
5. the white light LED part according to any one of claim 1-4, is characterized in that: described II-VI group quantum dot is from CdSe/ZnS quantum dot, the CdSe of nucleocapsid structure
ys
1-Y/ ZnS quantum dot, and the CdSe quantum dot of mononuclear structure, Zn
zcd
1-Zselect arbitrarily in Te quantum dot, nuclear radius is 1.3 ~ 2.5nm, and shell thickness is 1.4 ~ 2.8nm, and the emission wavelength of quantum dot is 520nm to 650nm, is carried out the emission wavelength of adjusting means by the kind and proportioning regulating filling quantum dot.
6. the preparation method of the white light LED part described in claim 1-5, its step comprises:
1) evaporation one deck ITO layer on the InGaN/GaN quantum well LED substrate of emission wavelength 430 ~ 480nm;
2) at ITO layer superficial growth one layer insulating, at surface of insulating layer growth layer of metal rete, SU8 glue and ultra-violet curing glue are spin-coated on metal film layer surface successively, insulating barrier adopts the fine and close insulating material with high-k, and the work function that the metal that metallic diaphragm adopts contacts with gold-half of p-type GaN is mated;
3) utilize UV-NIL technology, use soft template on ultra-violet curing glue, form the ordered nano hole array of gross area;
4) utilize RIE technology, pass into CHF
3and O
2the remnant layer of mist etching ultra-violet curing glue, then with ultra-violet curing glue for mask, utilize RIE technology, pass into O
2sU8 layer is etched, nano-pore array structure is transferred to SU8 layer;
5) adopt ICP technology, pass into Ar gas etching metallic diaphragm, nano-pore array structure is transferred to metallic diaphragm, removes the SU8 glue of metallic diaphragm nanohole array surface;
6) adopt photoetching technique to make the LED component unit of standard at device surface, remove the metallic diaphragm in the region beyond photoresist, then remove photoresist;
7) photoetching, makes p-type electrode zone at device surface, adopts RIE technology, passes into CF
4and O
2mist etching insulating layer, make the nanohole array of metallic diaphragm be transferred to insulating barrier, remove photoresist;
8) adopt ICP technology, pass into Cl
2mist etching ITO layer with Ar, is transferred to ITO layer by nano-pore array structure from insulating medium layer;
9) adopt ICP technology, pass into Cl
2with the mist of Ar, anisotropic etching p-type gallium nitride layer, mqw active layer, n-type gallium nitride layer, formation runs through ITO layer, p-type gallium nitride layer, mqw active layer, be deep to the nanohole array of n-type gallium nitride layer, sample is placed on inorganic acid, etching injury is removed in aqueous slkali water-bath, then remove remaining insulating barrier;
10) photoetching technique is adopted, evaporation p-type electrode and n-type electrode;
11) the certain density II-VI group quantum dot of proportioning, is spin-coated on device surface.
7. the preparation method of white light LED part according to claim 6, is characterized in that: described insulating barrier selects SiO
2or Si
3n
4, metallic diaphragm selects individual layer or the combination multilayer of Ni, Cr, Al.
8. the preparation method of white light LED part according to claim 7, is characterized in that: the thickness of insulating layer of growth is 30 ~ 300nm, and metallic diaphragm thickness is 10 ~ 50nm, SU8 glue thickness is 200 ~ 600nm, and ultra-violet curing glue thickness is 30 ~ 300nm.
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