CN108336196A - A kind of preparation method of UV LED chip - Google Patents
A kind of preparation method of UV LED chip Download PDFInfo
- Publication number
- CN108336196A CN108336196A CN201810080422.2A CN201810080422A CN108336196A CN 108336196 A CN108336196 A CN 108336196A CN 201810080422 A CN201810080422 A CN 201810080422A CN 108336196 A CN108336196 A CN 108336196A
- Authority
- CN
- China
- Prior art keywords
- layer
- ingan
- superlattices
- layers
- deep ultraviolet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
-
- 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
- H01L33/04—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 quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—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 quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of group III and group V of the periodic system
- H01L33/32—Materials of the light emitting region containing only elements of group III and group V of the periodic system containing nitrogen
-
- 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
- H01L33/48—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 body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/005—Processes relating to semiconductor body packages relating to encapsulations
Abstract
The invention discloses a kind of preparation method of UV LED chip, this method uses the silicon substrate of special process cleaning；The method of the present invention does not need large area etching removal GaN layer, reduces the difficulty of technique, further improves the light extraction efficiency of GaN layer；In the growth course of the epitaxial structure of the present invention, the high quality quaternary AlInGaN materials that component is uniform, defect concentration is low are prepared, form InGaN/AlxInyGa1‑x‑yN multi-quantum pit structure layers, the lattice constant of the potential barrier and Potential well layer materials that make quantum well structure, which reaches, to be exactly matched；The present invention uses red, blue, the green three fluorescence colloid of ultraviolet excitation as the protective layer of LED chip; colloid used is not easy to be decomposed by ultraviolet light and ozone; no double bond exists; the chemical bond of molecule is not broken at high temperature; it is in water white transparency colloid after colloid solidification; there are certain adherency and leakproofness good PPA and metal, there is excellent electrical insulation properties and good leakproofness.
Description
Technical field
The present invention relates to the preparation methods of LED, and in particular to a kind of preparation method of UV LED chip.
Background technology
Light emitting diode (Light-Emitting Diode, LED) is as a kind of novel energy-conserving, environmentally friendly solid-state lighting light
Source has many advantages, such as high efficiency, small, light-weight, fast response time and long lifespan, it is made to have been obtained extensively in many fields
General application.
Nowadays, III-V race's semi-conducting material flourishes, and is entered in people’s lives in many fields,
Middle GaN has even more attracted the eyeball of many people as the important materials for preparing efficient LED.Compared with traditional material, GaN conducts
The representative of third generation semi-conducting material has excellent physics, chemical property, such as：Energy gap is wider, and thermal stability is good,
Electron mobility is very high, and a kind of still direct band-gap semicondictor material.
It is and traditional at present ultraviolet with the development of ultraviolet LED technology, the decline of production cost, the promotion of output performance
Light source is compared, and ultraviolet LED has theoretical long lifespan, cold light source, high efficient and reliable, irradiation brightness uniformly and without noxious material etc.
Advantage, in the increasingly wider of the fields applications such as biologic medical, sterilizing, printing lithographic, photocuring production and communication detecting
It is general, it is also more and more paid close attention to by semiconductor lighting industry in recent years.
The maximum bottlenecks of deep ultraviolet LED are luminous efficiencies at present, are primarily limited to three aspects：（1）Injection efficiency has
Effect is injected into the ratio of the carrier of light-emitting zone；（2）Internal quantum efficiency, the compound generation photon of light-emitting zone electrons and holes
Ratio；（3）Light extraction efficiency, the photon generated in light-emitting zone, extracts the ratio of available photon from chip.And
Deep ultraviolet band, the efficiency in terms of above three are all relatively low.On the one hand, need to further increase the crystal matter of AlGaN material
Amount, obtains higher internal quantum efficiency, on the other hand, since the current deep ultraviolet LED overwhelming majority uses flip-chip packaged by substrate
The interface of the mode of face light extraction, substrate and air becomes one of the key for influencing light extraction efficiency.When growing AlGaN material, one
As take the method for the film of growing AIN on substrate as transition zone, the fault in material of the AlN of growth is generally 107-11/
cm2The order of magnitude.
Invention content
The present invention provides a kind of preparation method of UV LED chip, and this method uses the silicon substrate of special process cleaning, should
Silicon substrate has many advantages, such as to easily remove, radioresistance, thermal conductivity height, high temperature resistant, chemical property are relatively stablized, intensity is higher, has
Very high reliability, the UV LED chip based on silicon substrate are widely used in high-temperature device；The method of the present invention does not need big face
Product etching removal GaN layer, reduces the difficulty of technique, prevents the damage to epitaxial wafer electric property and protective layer in etching process
Wound, while the present invention to GaN layer after dry etching is thinned be roughened, and further improves the light extraction efficiency of GaN layer, both
Epitaxial structure can be protected by GaN layer, while increasing light extraction function；The growth of the epitaxial structure of the present invention
Cheng Zhong prepares the high quality quaternary AlInGaN materials that component is uniform, defect concentration is low, and is successfully applied to InGaN/
AlxInyGa1-x-yThe abarrier layer material of N multi-quantum pit structures, and the alternating growth on AlInGaN superlattices template layers
AlxInyGa1-x-yN superlattices barrier layer and InGaN potential well layers, to form InGaN/AlxInyGa1-x-yN multi-quantum pit structure layers,
The lattice constant of the potential barrier and Potential well layer materials that make quantum well structure, which reaches, to be exactly matched；Present invention ultraviolet excitation is red, it is blue,
Protective layer of the green three fluorescence colloid as LED chip, colloid used are not easy to be decomposed by ultraviolet light and ozone, and no double bond is deposited
, the chemical bond of molecule is not broken at high temperature, colloid solidification after be in water white transparency colloid, have to PPA and metal certain
Adherency and leakproofness are good, have excellent electrical insulation properties and good leakproofness.
To achieve the goals above, the present invention provides a kind of preparation method of UV LED chip, which includes such as
Lower step：
（1）Preparing substrate
It is 1 that silicon substrate, which is put into volume ratio,:Ultrasound 3-5 minutes in 15 hydrofluoric acid and deionized water mixed solution, removal silicon lining
Bottom surface oxide and pickup particle place into ultrasound 3-5 minutes in deionized water, surface impurity are removed, with dry nitrogen air-blowing
It is dry；
（2）Buffer layer is generated from substrate
Using Metal Organic Chemical Vapor Deposition method, at 540-560 DEG C, reaction cavity pressure 350mbar- is kept
450mbar is passed through the NH that flow is 10000sccm-16000sccm3, 60sccm-80sccm TMGa, 140L/min-160L/
The H of min2, on substrate growth thickness be 20nm-30nm buffer layer GaN；
（3）The back growth deep ultraviolet epitaxial structure on the surface of the buffer layer GaN；
（4）Two cuts are marked on deep ultraviolet epitaxial structure with laser scribing, and the middle part of buffer layer GaN is made to disconnect, then
Deep ultraviolet epitaxial structure between two cuts is removed using dry etching technology, to form the first deep ultraviolet epitaxial structure, the
Two deep ultraviolet epitaxial structures and the second gap；
（5）It is anti-that first is made respectively in the upper surface of the upper surface of the first deep ultraviolet epitaxial structure and the second deep ultraviolet epitaxial structure
Light microscopic layer and the second mirror layer；
（6）In the surface of substrate, the first deep ultraviolet epitaxial structure surface, the second deep ultraviolet epitaxy junction by the way of low temperature depositing
The surface on the surface of structure, the surface of the first mirror layer and the second mirror layer makes protective layer, then removes the first reflective mirror
The protective layer on layer surface and the second mirror layer surface, to form the first epitaxial structure protective layer, the second epitaxial structure protective layer,
Obtain UV LED chip.
Preferably, in step（3）In, specifically deep ultraviolet epitaxial structure is formed using following steps：
Using metal-organic chemical vapor deposition equipment method, InGaN insert layers, AlInGaN superlattices on the surface of buffer layer GaN
Template layer and InGaN/AlInGaN multi-quantum pit structure layers.
Preferably, the AlInGaN superlattices template layer is by 25-30 layers of short cycle InGaN/AlGaN superlattices of growth
Structure sheaf is formed；Growing the InGaN/AlxInyGa1-x-yWhen N multi-quantum pit structure layers, first in AlInGaN superlattices templates
One layer of Al is grown on layerxInyGa1-x-yN superlattices barrier layers, then again in AlxInyGa1-x-yOne is grown on N superlattices barrier layers
Layer InGaN potential well layers, so alternately grow AlxInyGa1-x-yN superlattices barrier layer and InGaN potential well layers, until last raw
Long AlxInyGa1-x-yN superlattices barrier layers, the AlxInyGa1-x-yThe ratio of x and y is in N superlattices barrier layers（3.75-
3.88）: 1, and x is 0.15-0.3.
Preferably, when growing the short cycle InGaN/AlGaN super lattice structure layers, growth heating is 840-850 DEG C,
NH3Flow is 17500-18500sccm, and the flow of triethyl-gallium is 72-75 μm of ol/min, and the flow of trimethyl aluminium is 102-
The flow of 105 μm of ol/min, trimethyl indium are 40-42 μm of ol/min.
Preferably, the Al is being grownxInyGa1-x-yWhen N superlattices barrier layers, every layer of AlxInyGa1-x-yN superlattices potential barriers
Layer is made of the InGaN/AlGaN superlattices that periodicity is 12-15, the InGaN/AlGaN superlattice thickness difference in each period
For 1nm.Since each layer thickness of InGaN/AlGaN superlattices is below its critical thickness so that InGaN, AlGaN superlattice layer pair
InGaN bottoms can be respectively at compressive strain, tensile strain state, therefore the short cycle InGaN/AlGaN Jing Guo optimization design is super brilliant
Lattice can be used as stress compensation structure, realize the balance lattice exactly matched with InGaN bottoms, caused by effective compensation lattice mismatch
Stress, and then realize the High Efficiency Luminescence of quantum well structure.
Preferably, the Al is being grownxInyGa1-x-yWhen N superlattices barrier layers, growth temperature is 810-825 DEG C, NH3Stream
Amount is 17500-18500sccm, and the flow of triethyl-gallium is 66-69 μm of ol/min, and the flow of trimethyl aluminium is 98-101 μm of ol/
The flow of min, trimethyl indium are 39-42 μm of ol/min.
Preferably, when growing the InGaN insert layers, growth temperature is 780-790 DEG C, NH3Flow is 16000-
The flow of 17000sccm, triethyl-gallium are 65-68 μm of ol/min, and the flow of trimethyl indium is 76-78 μm of ol/min.
Preferably, in the step（6）In, the protective layer is formed by three coloured light powder colloidal deposition, is specifically included as follows
Step：
（61）By the silica gel that viscosity is 10000mPas at 25 DEG C and the silica gel that viscosity is 4500mPas at 25 DEG C, in 80-
It is mixed 5-10 minutes under 100 revs/min of rotating speed, vacuum defoamation 10-15 minutes obtains phosphor gel；
（62）Red fluorescence powder, green emitting phosphor, blue colour fluorescent powder and curing agent are added according to the ratio, in 100-150 revs/min turn
Speed lower stirring 20-30 minutes, obtains three-color phosphor colloid；
（63）Three-color phosphor colloid 40-60 minute is toasted at 70-80 DEG C, then is warming up to 100-120 DEG C to toast 1.5-2.5 small
When；
（64）By the three-color phosphor colloidal deposition after solidification in the surface of substrate, the first deep ultraviolet epitaxial structure surface, second
The surface on the surface of deep ultraviolet epitaxial structure, the surface of the first mirror layer and the second mirror layer.
Preferably, wherein red fluorescence powder, green emitting phosphor, blue colour fluorescent powder are respectively：
Red quantum dot fluorescent powder：Coat the CdSe of shell structurexTe1-xQuantum dot, 0≤x<1；
Green quantum dot fluorescent powder：Coat one kind in CdSe, CuInS, InP quantum dot of shell structure；
Blue light fluorescent powder：Rare earth blue light fluorescent powder.
Preferably, red quantum dot fluorescent powder：Green quantum dot fluorescent powder：Blue light fluorescent powder=（0.5-1.5）：（0.8-
1.2）：1.
The invention has the advantages that：
（1）The present invention uses the silicon substrate of special process cleaning, the silicon substrate have easily remove, radioresistance, thermal conductivity are high, resistance to
The advantages that high temperature, chemical property are relatively stablized, intensity is higher has very high reliability, the UV LED chip based on silicon substrate wide
It is general to be applied to high-temperature device.
（2）The method of the present invention does not need large area etching removal GaN layer, reduces the difficulty of technique, prevents etched
To the damage of epitaxial wafer electric property and protective layer in journey, while the present invention to GaN layer after dry etching is thinned be roughened, into
The light extraction efficiency for improving GaN layer of one step, can both protect epitaxial structure by GaN layer, while increasing light
Extract function.
（3）In the growth course of the epitaxial structure of the present invention, the high quality quaternary that component is uniform, defect concentration is low is prepared
AlInGaN materials, and it is successfully applied to InGaN/AlxInyGa1-x-yThe abarrier layer material of N multi-quantum pit structures.And
Alternating growth Al on AlInGaN superlattices template layersxInyGa1-x-yN superlattices barrier layer and InGaN potential well layers, to be formed
InGaN/AlxInyGa1-x-yN multi-quantum pit structure layers, the lattice constant of the potential barrier and Potential well layer materials that make quantum well structure reach
It exactly matches.The InGaN/Al for the Lattice Matching that the present invention preparesxInyGa1-x-yN multi-quantum pit structure layers reach following ginseng
Number index：1. Quantum Well surface V-type defect concentration<4.2×105/cm2；2. Quantum Well surface roughness RMS<1nm；3. interior quantum
Efficiency>79%.
（4）The present invention uses red, blue, the green three fluorescence colloid of ultraviolet excitation as the protective layer of LED chip, colloid used
It is not easy to be decomposed by ultraviolet light and ozone, no double bond exists, and the chemical bond of molecule is not broken at high temperature, is in nothing after colloid solidification
Color transparent jelly has certain adherency and leakproofness good PPA and metal, with excellent electrical insulation properties and well
Leakproofness.
Specific implementation mode
Embodiment one
It is 1 that silicon substrate, which is put into volume ratio,:Ultrasound 3 minutes in 15 hydrofluoric acid and deionized water mixed solution, remove silicon substrate
Oxide on surface and pickup particle place into ultrasound 3 minutes in deionized water, remove surface impurity, dried up with drying nitrogen.
Using Metal Organic Chemical Vapor Deposition method, at 540 DEG C, reaction cavity pressure 350mbar is kept, stream is passed through
Amount is the NH of 10000sccm3, 60sccm TMGa, 140L/min H2, on substrate growth thickness be 20nm buffer layer
GaN。
The back growth deep ultraviolet epitaxial structure on the surface of the buffer layer GaN；Specifically depth is formed using following steps
Ultraviolet epitaxial structure：Using metal-organic chemical vapor deposition equipment method, on the surface of buffer layer GaN InGaN insert layers,
AlInGaN superlattices template layer and InGaN/AlInGaN multi-quantum pit structure layers.
The AlInGaN superlattices template layer is formed by the short cycle InGaN/AlGaN super lattice structure layers for growing 25 layers；
Growing the InGaN/AlxInyGa1-x-yWhen N multi-quantum pit structure layers, first one is grown on AlInGaN superlattices template layers
Layer AlxInyGa1-x-yN superlattices barrier layers, then again in AlxInyGa1-x-yOne layer of InGaN potential well is grown on N superlattices barrier layers
Layer, so alternately grows AlxInyGa1-x-yN superlattices barrier layer and InGaN potential well layers, until last growth AlxInyGa1-x- yN superlattices barrier layers, the AlxInyGa1-x-yThe ratio of x and y is 3.88: 1 in N superlattices barrier layers, and x is 0.15.
When growing the short cycle InGaN/AlGaN super lattice structure layers, growth heating is 840 DEG C, NH3Flow is
The flow of 17500sccm, triethyl-gallium are 72 μm of ol/min, and the flow of trimethyl aluminium is 102 μm of ol/min, the stream of trimethyl indium
Amount is 40 μm of ol/min.
Growing the AlxInyGa1-x-yWhen N superlattices barrier layers, every layer of AlxInyGa1-x-yN superlattices barrier layers are by week
The InGaN/AlGaN superlattices that issue is 12 are constituted, and the InGaN/AlGaN superlattice thickness in each period is respectively 1nm.Due to
Each layer thickness of InGaN/AlGaN superlattices is below its critical thickness so that InGaN, AlGaN superlattice layer are to InGaN bottoms
It can be respectively at compressive strain, tensile strain state, therefore the short cycle InGaN/AlGaN superlattices Jing Guo optimization design can be used as and answer
Force compensating structure, realizes the balance lattice exactly matched with InGaN bottoms, stress caused by effective compensation lattice mismatch, in turn
Realize the High Efficiency Luminescence of quantum well structure.
Growing the AlxInyGa1-x-yWhen N superlattices barrier layers, growth temperature is 810 DEG C, NH3Flow is
The flow of 17500sccm, triethyl-gallium are 66 μm of ol/min, and the flow of trimethyl aluminium is 98 μm of ol/min, the stream of trimethyl indium
Amount is 39 μm of ol/min.
When growing the InGaN insert layers, growth temperature is 780 DEG C, NH3Flow is 16000sccm, triethyl-gallium
Flow is 65 μm of ol/min, and the flow of trimethyl indium is 76 μm of ol/min.
Two cuts are marked on deep ultraviolet epitaxial structure with laser scribing, and the middle part of buffer layer GaN is made to disconnect, then
Deep ultraviolet epitaxial structure between two cuts is removed using dry etching technology, to form the first deep ultraviolet epitaxial structure, the
Two deep ultraviolet epitaxial structures and the second gap.
First is made respectively in the upper surface of the upper surface of the first deep ultraviolet epitaxial structure and the second deep ultraviolet epitaxial structure
Mirror layer and the second mirror layer.
In the surface of substrate, the first deep ultraviolet epitaxial structure surface, the second deep ultraviolet extension by the way of low temperature depositing
The surface on the surface of structure, the surface of the first mirror layer and the second mirror layer makes protective layer, and it is reflective then to remove first
The protective layer on mirror layer surface and the second mirror layer surface, to form the first epitaxial structure protective layer, the second epitaxial structure is protected
Layer, obtains UV LED chip.
The protective layer is formed by three coloured light powder colloidal deposition, is specifically comprised the following steps：
By the silica gel that viscosity is 10000mPas at 25 DEG C and the silica gel that viscosity is 4500mPas at 25 DEG C, at 80 revs/min
Rotating speed under be mixed 5 minutes, vacuum defoamation 10 minutes obtains phosphor gel；
Red fluorescence powder, green emitting phosphor, blue colour fluorescent powder and curing agent are added according to the ratio, is stirred under 100 revs/min of rotating speed
20 minutes, obtain three-color phosphor colloid；
Three-color phosphor colloid is toasted at 70 DEG C 40 minutes, then be warming up to 100 DEG C and toast 1.5 hours；
By the three-color phosphor colloidal deposition after solidification on the surface of substrate, the first deep ultraviolet epitaxial structure surface, second dark purple
The surface on the surface of outer epitaxial structure, the surface of the first mirror layer and the second mirror layer.
Wherein red fluorescence powder, green emitting phosphor, blue colour fluorescent powder are respectively：
Red quantum dot fluorescent powder：Coat the CdSe of shell structure0.1Te0.9Quantum dot.
Green quantum dot fluorescent powder：Coat the CdSe quantum dot of shell structure.
Blue light fluorescent powder：Rare earth blue light fluorescent powder.
Red quantum dot fluorescent powder：Green quantum dot fluorescent powder：Blue light fluorescent powder=0.5：0.8：1.
Embodiment two
It is 1 that silicon substrate, which is put into volume ratio,:Ultrasound 5 minutes in 15 hydrofluoric acid and deionized water mixed solution, remove silicon substrate
Oxide on surface and pickup particle place into ultrasound 5 minutes in deionized water, remove surface impurity, dried up with drying nitrogen.
Using Metal Organic Chemical Vapor Deposition method, at 560 DEG C, reaction cavity pressure 450mbar is kept, stream is passed through
Amount is the NH of 16000sccm3, 60sccm-80sccm TMGa, 140L/min-160L/min H2, growth thickness on substrate
For the buffer layer GaN of 30nm.
The back growth deep ultraviolet epitaxial structure on the surface of the buffer layer GaN；Specifically depth is formed using following steps
Ultraviolet epitaxial structure：Using metal-organic chemical vapor deposition equipment method, on the surface of buffer layer GaN InGaN insert layers,
AlInGaN superlattices template layer and InGaN/AlInGaN multi-quantum pit structure layers.
The AlInGaN superlattices template layer is formed by the short cycle InGaN/AlGaN super lattice structure layers for growing 30 layers；
Growing the InGaN/AlxInyGa1-x-yWhen N multi-quantum pit structure layers, first one is grown on AlInGaN superlattices template layers
Layer AlxInyGa1-x-yN superlattices barrier layers, then again in AlxInyGa1-x-yOne layer of InGaN potential well is grown on N superlattices barrier layers
Layer, so alternately grows AlxInyGa1-x-yN superlattices barrier layer and InGaN potential well layers, until last growth AlxInyGa1-x- yN superlattices barrier layers, the AlxInyGa1-x-yThe ratio of x and y is 3.75: 1 in N superlattices barrier layers, and x is 0.3.
When growing the short cycle InGaN/AlGaN super lattice structure layers, growth heating is 850 DEG C, NH3Flow is
The flow of 17500-18500sccm, triethyl-gallium are 75 μm of ol/min, and the flow of trimethyl aluminium is 105 μm of ol/min, trimethyl
The flow of indium is 42 μm of ol/min.
Growing the AlxInyGa1-x-yWhen N superlattices barrier layers, every layer of AlxInyGa1-x-yN superlattices barrier layers are by week
The InGaN/AlGaN superlattices that issue is 15 are constituted, and the InGaN/AlGaN superlattice thickness in each period is respectively 1nm.Due to
Each layer thickness of InGaN/AlGaN superlattices is below its critical thickness so that InGaN, AlGaN superlattice layer are to InGaN bottoms
It can be respectively at compressive strain, tensile strain state, therefore the short cycle InGaN/AlGaN superlattices Jing Guo optimization design can be used as and answer
Force compensating structure, realizes the balance lattice exactly matched with InGaN bottoms, stress caused by effective compensation lattice mismatch, in turn
Realize the High Efficiency Luminescence of quantum well structure.
Growing the AlxInyGa1-x-yWhen N superlattices barrier layers, growth temperature is 825 DEG C, NH3Flow is
The flow of 18500sccm, triethyl-gallium are 69 μm of ol/min, and the flow of trimethyl aluminium is 101 μm of ol/min, the stream of trimethyl indium
Amount is 42 μm of ol/min.
When growing the InGaN insert layers, growth temperature is 790 DEG C, NH3Flow is 17000sccm, triethyl-gallium
Flow is 68 μm of ol/min, and the flow of trimethyl indium is 78 μm of ol/min.
Two cuts are marked on deep ultraviolet epitaxial structure with laser scribing, and the middle part of buffer layer GaN is made to disconnect, then
Deep ultraviolet epitaxial structure between two cuts is removed using dry etching technology, to form the first deep ultraviolet epitaxial structure, the
Two deep ultraviolet epitaxial structures and the second gap.
First is made respectively in the upper surface of the upper surface of the first deep ultraviolet epitaxial structure and the second deep ultraviolet epitaxial structure
Mirror layer and the second mirror layer.
In the surface of substrate, the first deep ultraviolet epitaxial structure surface, the second deep ultraviolet extension by the way of low temperature depositing
The surface on the surface of structure, the surface of the first mirror layer and the second mirror layer makes protective layer, and it is reflective then to remove first
The protective layer on mirror layer surface and the second mirror layer surface, to form the first epitaxial structure protective layer, the second epitaxial structure is protected
Layer, obtains UV LED chip.
The protective layer is formed by three coloured light powder colloidal deposition, is specifically comprised the following steps：
By the silica gel that viscosity is 10000mPas at 25 DEG C and the silica gel that viscosity is 4500mPas at 25 DEG C, 100 turns/
It is mixed 10 minutes under the rotating speed divided, vacuum defoamation 15 minutes obtains phosphor gel；
Red fluorescence powder, green emitting phosphor, blue colour fluorescent powder and curing agent are added according to the ratio, is stirred under 150 revs/min of rotating speed
30 minutes, obtain three-color phosphor colloid；
Three-color phosphor colloid is toasted at 80 DEG C 60 minutes, then be warming up to 120 DEG C and toast 2.5 hours；
By the three-color phosphor colloidal deposition after solidification on the surface of substrate, the first deep ultraviolet epitaxial structure surface, second dark purple
The surface on the surface of outer epitaxial structure, the surface of the first mirror layer and the second mirror layer.
Wherein red fluorescence powder, green emitting phosphor, blue colour fluorescent powder are respectively：
Red quantum dot fluorescent powder：Coat the CdSe of shell structure0.8Te0.2Quantum dot
Green quantum dot fluorescent powder：Coat the InP quantum dots of shell structure.
Blue light fluorescent powder：Rare earth blue light fluorescent powder.
Red quantum dot fluorescent powder：Green quantum dot fluorescent powder：Blue light fluorescent powder=1.5：1.2：1.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, other various forms of variations can also be made on the basis of the above description.
There is no necessity and possibility to exhaust all the enbodiments.And obvious changes or variations extended from this are still
Among protection scope of the present invention.
Claims (10)
1. a kind of preparation method of UV LED chip, the preparation method include the following steps：
（1）Preparing substrate
It is 1 that silicon substrate, which is put into volume ratio,:Ultrasound 3-5 minutes in 15 hydrofluoric acid and deionized water mixed solution, removal silicon lining
Bottom surface oxide and pickup particle place into ultrasound 3-5 minutes in deionized water, surface impurity are removed, with dry nitrogen air-blowing
It is dry；
（2）Buffer layer is generated from substrate
Using Metal Organic Chemical Vapor Deposition method, at 540-560 DEG C, reaction cavity pressure 350mbar- is kept
450mbar is passed through the NH that flow is 10000sccm-16000sccm3, 60sccm-80sccm TMGa, 140L/min-160L/
The H of min2, on substrate growth thickness be 20nm-30nm buffer layer GaN；
（3）The back growth deep ultraviolet epitaxial structure on the surface of the buffer layer GaN；
（4）Two cuts are marked on deep ultraviolet epitaxial structure with laser scribing, and the middle part of buffer layer GaN is made to disconnect, then
Deep ultraviolet epitaxial structure between two cuts is removed using dry etching technology, to form the first deep ultraviolet epitaxial structure, the
Two deep ultraviolet epitaxial structures and the second gap；
（5）It is anti-that first is made respectively in the upper surface of the upper surface of the first deep ultraviolet epitaxial structure and the second deep ultraviolet epitaxial structure
Light microscopic layer and the second mirror layer；
（6）In the surface of substrate, the first deep ultraviolet epitaxial structure surface, the second deep ultraviolet epitaxy junction by the way of low temperature depositing
The surface on the surface of structure, the surface of the first mirror layer and the second mirror layer makes protective layer, then removes the first reflective mirror
The protective layer on layer surface and the second mirror layer surface, to form the first epitaxial structure protective layer, the second epitaxial structure protective layer,
Obtain UV LED chip.
2. the method as described in claim 1, which is characterized in that in step（3）In, specifically deep ultraviolet is formed using following steps
Epitaxial structure：
Using metal-organic chemical vapor deposition equipment method, InGaN insert layers, AlInGaN superlattices on the surface of buffer layer GaN
Template layer and InGaN/AlInGaN multi-quantum pit structure layers.
3. method as claimed in claim 2, which is characterized in that the AlInGaN superlattices template layer is by growing 25-30 layers
Short cycle InGaN/AlGaN super lattice structure layers are formed；Growing the InGaN/AlxInyGa1-x-yN multi-quantum pit structure layers
When, one layer of Al is first grown on AlInGaN superlattices template layersxInyGa1-x-yN superlattices barrier layers, then exist again
AlxInyGa1-x-yOne layer of InGaN potential well layer is grown on N superlattices barrier layers, so alternately grows AlxInyGa1-x-yN superlattices
Barrier layer and InGaN potential well layers, until last growth AlxInyGa1-x-yN superlattices barrier layers, the AlxInyGa1-x-yN is super brilliant
The ratio of x and y is in lattice barrier layer（3.75-3.88）: 1, and x is 0.15-0.3.
4. method as claimed in claim 3, which is characterized in that growing the short cycle InGaN/AlGaN superlattice structures
When layer, growth heating is 840-850 DEG C, NH3Flow is 17500-18500sccm, and the flow of triethyl-gallium is 72-75 μm of ol/
The flow of min, trimethyl aluminium are 102-105 μm of ol/min, and the flow of trimethyl indium is 40-42 μm of ol/min.
5. method as described in claim 3 or 4, which is characterized in that growing the AlxInyGa1-x-yN superlattices barrier layers
When, every layer of AlxInyGa1-x-yN superlattices barrier layer is made of the InGaN/AlGaN superlattices that periodicity is 12-15, Ge Gezhou
The InGaN/AlGaN superlattice thickness of phase is respectively 1nm；
Since each layer thickness of InGaN/AlGaN superlattices is below its critical thickness so that InGaN, AlGaN superlattice layer pair
InGaN bottoms can be respectively at compressive strain, tensile strain state, therefore the short cycle InGaN/AlGaN Jing Guo optimization design is super brilliant
Lattice can be used as stress compensation structure, realize the balance lattice exactly matched with InGaN bottoms, caused by effective compensation lattice mismatch
Stress, and then realize the High Efficiency Luminescence of quantum well structure.
6. method as described in claim 3 or 4, which is characterized in that growing the AlxInyGa1-x-yN superlattices barrier layers
When, growth temperature is 810-825 DEG C, NH3Flow is 17500-18500sccm, and the flow of triethyl-gallium is 66-69 μm of ol/
The flow of min, trimethyl aluminium are 98-101 μm of ol/min, and the flow of trimethyl indium is 39-42 μm of ol/min.
7. method as described in claim 3 or 4, which is characterized in that when growing the InGaN insert layers, growth temperature is
780-790 DEG C, NH3Flow is 16000-17000sccm, and the flow of triethyl-gallium is 65-68 μm of ol/min, the stream of trimethyl indium
Amount is 76-78 μm of ol/min.
8. the method as described in claim 1-7 is any, which is characterized in that in the step（6）In, the protective layer is by three colors
Light powder colloidal deposition forms, and specifically comprises the following steps：
（61）By the silica gel that viscosity is 10000mPas at 25 DEG C and the silica gel that viscosity is 4500mPas at 25 DEG C, in 80-
It is mixed 5-10 minutes under 100 revs/min of rotating speed, vacuum defoamation 10-15 minutes obtains phosphor gel；
（62）Red fluorescence powder, green emitting phosphor, blue colour fluorescent powder and curing agent are added according to the ratio, in 100-150 revs/min turn
Speed lower stirring 20-30 minutes, obtains three-color phosphor colloid；
（63）Three-color phosphor colloid 40-60 minute is toasted at 70-80 DEG C, then is warming up to 100-120 DEG C to toast 1.5-2.5 small
When；
（64）By the three-color phosphor colloidal deposition after solidification in the surface of substrate, the first deep ultraviolet epitaxial structure surface, second
The surface on the surface of deep ultraviolet epitaxial structure, the surface of the first mirror layer and the second mirror layer.
9. method as claimed in claim 8, which is characterized in that wherein red fluorescence powder, green emitting phosphor, blue colour fluorescent powder point
It is not：
Red quantum dot fluorescent powder：Coat the CdSe of shell structurexTe1-xQuantum dot, 0≤x<1；
Green quantum dot fluorescent powder：Coat one kind in CdSe, CuInS, InP quantum dot of shell structure；
Blue light fluorescent powder：Rare earth blue light fluorescent powder.
10. method as claimed in claim 9, which is characterized in that red quantum dot fluorescent powder：Green quantum dot fluorescent powder：It is blue
Emitting phosphor=（0.5-1.5）：（0.8-1.2）：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810080422.2A CN108336196A (en) | 2018-01-27 | 2018-01-27 | A kind of preparation method of UV LED chip |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810080422.2A CN108336196A (en) | 2018-01-27 | 2018-01-27 | A kind of preparation method of UV LED chip |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108336196A true CN108336196A (en) | 2018-07-27 |
Family
ID=62926707
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810080422.2A Pending CN108336196A (en) | 2018-01-27 | 2018-01-27 | A kind of preparation method of UV LED chip |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108336196A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110911531A (en) * | 2018-09-14 | 2020-03-24 | 合肥彩虹蓝光科技有限公司 | Light emitting diode epitaxial structure and light emitting diode |
| CN110911529A (en) * | 2018-09-14 | 2020-03-24 | 合肥彩虹蓝光科技有限公司 | Growth method of epitaxial structure of light-emitting diode |
| CN113097353A (en) * | 2021-04-02 | 2021-07-09 | 厦门乾照光电股份有限公司 | Ultraviolet LED and manufacturing method thereof |
| CN113284987A (en) * | 2021-03-30 | 2021-08-20 | 华灿光电（浙江）有限公司 | Preparation method of light-emitting diode epitaxial wafer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106981549A (en) * | 2017-04-19 | 2017-07-25 | 华南理工大学 | The gallium nitride nano-pillar LED of growth on a silicon substrate and preparation method thereof |
| CN107452858A (en) * | 2017-08-15 | 2017-12-08 | 苏州轻光材料科技有限公司 | A kind of burst of ultraviolel white light LEDs containing three-color phosphor and preparation method thereof |
| CN107482092A (en) * | 2017-07-26 | 2017-12-15 | 南京大学扬州光电研究院 | A kind of extension processing method of 395nm short wavelength UVs LED structure |
| CN107611233A (en) * | 2017-08-24 | 2018-01-19 | 西安交通大学 | Vertical stratification deep ultraviolet LED component based on composite transferring substrate and preparation method thereof |
-
2018
- 2018-01-27 CN CN201810080422.2A patent/CN108336196A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106981549A (en) * | 2017-04-19 | 2017-07-25 | 华南理工大学 | The gallium nitride nano-pillar LED of growth on a silicon substrate and preparation method thereof |
| CN107482092A (en) * | 2017-07-26 | 2017-12-15 | 南京大学扬州光电研究院 | A kind of extension processing method of 395nm short wavelength UVs LED structure |
| CN107452858A (en) * | 2017-08-15 | 2017-12-08 | 苏州轻光材料科技有限公司 | A kind of burst of ultraviolel white light LEDs containing three-color phosphor and preparation method thereof |
| CN107611233A (en) * | 2017-08-24 | 2018-01-19 | 西安交通大学 | Vertical stratification deep ultraviolet LED component based on composite transferring substrate and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110911531A (en) * | 2018-09-14 | 2020-03-24 | 合肥彩虹蓝光科技有限公司 | Light emitting diode epitaxial structure and light emitting diode |
| CN110911529A (en) * | 2018-09-14 | 2020-03-24 | 合肥彩虹蓝光科技有限公司 | Growth method of epitaxial structure of light-emitting diode |
| CN113284987A (en) * | 2021-03-30 | 2021-08-20 | 华灿光电（浙江）有限公司 | Preparation method of light-emitting diode epitaxial wafer |
| CN113097353A (en) * | 2021-04-02 | 2021-07-09 | 厦门乾照光电股份有限公司 | Ultraviolet LED and manufacturing method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108336196A (en) | A kind of preparation method of UV LED chip | |
| Zhang et al. | Fluorescent nanomaterial-derived white light-emitting diodes: what's going on | |
| CN105405939B (en) | A kind of light emitting diode and its manufacture method | |
| WO2007001098A1 (en) | Nanostructure having a nitride-based quantum well and light emitting diode employing the same | |
| US20140302665A1 (en) | Method for producing an optoelectronic nitride compound semiconductor component | |
| CN101540361B (en) | Preparation method of AlGaInP LED grown on silicon base | |
| CN105449051B (en) | One kind is using MOCVD technologies in GaN substrate or GaN/Al2O3The method that high brightness homogeneity LED is prepared in compound substrate | |
| CN110518101B (en) | UV LED epitaxial structure and growth method thereof | |
| CN105405942B (en) | Si substrate LEDs and preparation method thereof | |
| CN105633235A (en) | GaN-based LED epitaxial structure with n type GaN structure and growing method thereof | |
| TWI338382B (en) | Method and structure for manufacturing long-wavelength light-emitting diode using prestrain effect | |
| CN105762240B (en) | A kind of UV LED epitaxial structure and preparation method thereof | |
| CN105051918A (en) | Semiconductor structures having active regions comprising ingan, methods of forming such semiconductor structures, and light emitting devices formed from such semiconductor structures | |
| CN102347408B (en) | GaN-base double-blue-light wavelength luminescent device and preparation method thereof | |
| CN108630792A (en) | Based on Ga2O3Vertical structure ultraviolet LED of substrate and preparation method thereof | |
| CN107293624A (en) | A kind of light emitting diode epitaxial structure for becoming hole injection layer based on h BN tunnellings | |
| CN103337571B (en) | Improve epitaxial structure and the growing method of wavelength concentration in GaN base epitaxial wafer | |
| CN100369280C (en) | Luminous semiconductor device | |
| CN110401106A (en) | GaN base light emitting semiconductor device and preparation method thereof with AlGaN insert layer | |
| CN106653973A (en) | LED chip and preparation method thereof | |
| WO2017028555A1 (en) | Gan base material based on si substrate and preparation method therefor | |
| KR101081055B1 (en) | Light emitting device package and method for fabricating the same | |
| CN109888071A (en) | A kind of novel GaN base LED epitaxial layer structure and preparation method thereof | |
| CN109148651A (en) | The preparation method of multicolor luminous InGaN Quantum Well epitaxial wafer based on GaN striped template | |
| CN107689405A (en) | Ultraviolet led epitaxial structure and its growing method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180727 |
|
| WD01 | Invention patent application deemed withdrawn after publication |