CN105226146A - Liquid quantum dot LED and preparation method thereof - Google Patents

Liquid quantum dot LED and preparation method thereof Download PDF

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Publication number
CN105226146A
CN105226146A CN201510624145.3A CN201510624145A CN105226146A CN 105226146 A CN105226146 A CN 105226146A CN 201510624145 A CN201510624145 A CN 201510624145A CN 105226146 A CN105226146 A CN 105226146A
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Prior art keywords
quantum dot
liquid quantum
liquid
led
luminescence chip
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Chinese (zh)
Inventor
张宇
王鹤林
张铁强
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Jilin University
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Jilin University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
    • H01L33/02Semiconductor 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
    • H01L33/04Semiconductor 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
    • H01L33/06Semiconductor 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
    • H01L33/005Processes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
    • H01L33/005Processes
    • H01L33/0062Processes for devices with an active region comprising only III-V compounds
    • H01L33/0075Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
    • H01L33/02Semiconductor 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
    • H01L33/26Materials of the light emitting region
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008Processes
    • H01L2933/0025Processes relating to coatings

Abstract

The invention discloses liquid quantum dot LED and preparation method thereof, described liquid quantum dot LED, using liquid quantum dot as luminescent layer, has better quantum yield, also has higher brightness and luminous efficiency compared with solid state quantum point luminescent layer.The preparation method of this liquid quantum dot LED is: according to the requirement of described liquid quantum dot photoexcitation, select the luminescence chip of respective wavelength as excitation source, the liquid quantum dot prepared is injected luminescent layer by the mode injected by hydraulic pressure, liquid quantum dot LED is made finally by combination installation, the LED structure obtained by the method for the invention is simple, preparation process is easy, and spillage of material is low.

Description

Liquid quantum dot LED and preparation method thereof
Technical field
The present invention relates to a kind of liquid quantum dot LED and preparation method thereof, belong to illumination and display field.
Background technology
Along with the raising of development in science and technology and people's environmental consciousness, increasing new material is applied to lighting field.Quantum dot, as novel luminescent material, has the characteristics such as high-quantum efficiency, the adjustable band-gap of Size dependence, outstanding emission spectrum halfwidth, has good application prospect.
In recent years, along with going deep into of quanta point material research, quantum dot had become outstanding luminescent material, for the preparation of light-emitting diode (Light-EmittingDiode writes a Chinese character in simplified form LED).Compared with the luminescent material of traditional LED, quantum dot has the advantages such as luminous efficiency is higher, long service life, color rendering are higher, purity that is color is better.
The emitting layer material of existing quantum dot LED mainly adopts solid state quantum dot fluorescent powder and solid state quantum point film etc., but solid state quantum point is compared with quantum dot solution, its fluorescence efficiency is often lower, in addition, due to self aggregation effect, there will be in process of setting " coffee ring ", affect the homogeneity of fluorescent material distribution.Therefore, compared to solid state quantum point, liquid quantum dot has better quantum yield, avoids the loaded down with trivial details technique in quantum dot fluorescence powder, quantum dot film manufacturing process and spillage of material simultaneously.
Based on above-mentioned background, development luminous efficiency is high, technique is simple, spillage of material is low, stablize the novel liquid quantum dot LED of advantages such as getting well, contributes to promoting further developing of Lighting Industry.Through searching, use liquid quantum dot solution as luminescent layer, by the design of structure, liquid quantum dot LED preparing high-luminous-efficiency and preparation method thereof, both at home and abroad there are no relevant report.
Summary of the invention
In order to overcome the material and technical problem that exist in existing quantum dot LED, the present invention adopts liquid quantum dot solution as luminescent layer, pass through structural design, provide a kind of liquid quantum dot LED and preparation method thereof, the liquid quantum dot mixed white light LED or single wavelength quantum dot LED of multi-wavelength can be made.
The present invention adopts following technical scheme, and accompanying drawings is as follows:
Liquid quantum dot LED, primarily of luminescence chip base and luminescent layer composition, described luminescence chip base comprises heat radiation substrate and exciting light active layer, and described luminescent layer is liquid quantum dot.
Described liquid quantum dot is cadmium sulfide (CdS), cadmium selenide (CdSe), cadmium telluride (CdTe), copper indium sulphur (CuInS 2), copper indium diselenide (CuInSe 2), indium phosphide (InP), vulcanized lead (PbS), selenizing sulphur (PbSe), lead telluride (PbTe), zinc sulphide (ZnS), zinc selenide (ZnSe), zinc telluridse (ZnTe), polymer quantum dot or carbon quantum dot.
Luminescence chip in described exciting light active layer is gallium nitride (GaN) chip or UV LED chip.
The preparation method of liquid quantum dot LED, according to the requirement of described liquid quantum dot photoexcitation, select the luminescence chip of respective wavelength as excitation source, the liquid quantum dot prepared is injected luminescent layer by the mode injected by hydraulic pressure, and concrete steps are as follows:
Step one: prepare liquid quantum dot;
Step 2: the photoexcitation requirement of liquid quantum dot prepared by step one, selects luminescence chip, carries out ultrasonic cleaning, UV treatment;
Step 3: use gold thread to be connected with electrode by luminescence chip;
Step 4: by epoxy resin or silicone filler to the surface of luminescence chip, make airtight glass partition at epoxy resin or Silica Surface subsequently, namely complete the making of luminescence chip base;
Step 5: make glass envelope;
Step 6: machining small in glass envelope, in the glove box being full of nitrogen, is injected in glass envelope by liquid quantum dot, after being filled, uses silica gel or epoxy resin to be sealed by aperture;
Step 7: place plastic uptake acrylic board outside glass envelope, and filling gel or epoxy resin in space between glass envelope and plastic uptake acrylic board, namely complete the making of liquid quantum dot light emitting layer;
Step 8: the liquid quantum dot light emitting layer made by step 7 is mounted on the luminescence chip base of step 4 making, namely completes the preparation of liquid quantum dot LED.
The glow color of the liquid quantum dot LED of the present invention is determined by the liquid quantum dot light emitting character chosen, and can realize the luminescence of panchromatic system or monochrome.
Compared with the prior art, the invention has the beneficial effects as follows:
1, liquid quantum dot LED of the present invention and preparation method thereof, the fluorescence quantum yield of the liquid quantum dot adopted is high;
2, liquid quantum dot LED of the present invention and preparation method thereof, prepared New LED brightness, luminous efficiency are high;
3, liquid quantum dot LED of the present invention and preparation method thereof, designed New LED structure is simple, preparation is easy, spillage of material is low.
Accompanying drawing explanation
Fig. 1 is liquid quantum dot LED structure schematic diagram of the present invention;
Fig. 2 is liquid quantum dot LED green glow of the present invention, ruddiness CdSe quantum dots solution emission spectrum and abosrption spectrogram;
Fig. 3 is the liquid quantum spot white light LED photo of cadmium selenide of gallium nitride chip in liquid quantum dot LED of the present invention, green glow CdSe quantum dots, ruddiness CdSe quantum dots utilizing emitted light spectrogram and insertion;
Fig. 4 is the emission spectrum of the liquid quantum spot white light LED of cadmium selenide under different voltage in liquid quantum dot LED of the present invention.
In figure:
1-electrode, 2-gold thread, 3-luminescence chip, 4-first epoxide-resin glue or silica gel, 5-glass partition, the liquid quantum dot light emitting layer of 6-, 7-hemisphere glass envelope, 8-second epoxide-resin glue or silica gel, 9-plastic uptake acrylic plate.
Embodiment
In conjunction with Figure of description, the specific embodiment of the present invention is described below:
Consult Fig. 1, the invention provides a kind of liquid quantum dot LED, primarily of luminescence chip base and luminescent layer composition, described luminescence chip base comprises heat radiation substrate and exciting light active layer, wherein, exciting light active layer comprises electrode 1, luminescence chip 3, wherein, luminescence chip selects gallium nitride (GaN) chip or UV LED chip, described electrode 1 is all fixed on heat radiation substrate with luminescence chip 3, and connected by gold thread 2, luminescence chip surface is filled with the first silica gel or epoxy resin 4, outside described first silica gel or epoxy resin 4, airtight glass partition 5 is housed, realize the sealing to exciting light active layer.Described luminescent layer 6 is liquid quantum dot layer, liquid quantum dot is filled in hemispheric glass envelope 7, the size of glass envelope 7 is depending on actual conditions, glass envelope 7 is outer places hemispheric plastic uptake acrylic plate 9, and be filled with silica gel or epoxy resin at glass envelope 7 and plastic uptake acrylic plate 9, realize sealing.
Consult Fig. 1 and Fig. 2, the preparation method of liquid quantum dot LED, according to the requirement of liquid quantum dot photoexcitation, selects the luminescence chip of respective wavelength as excitation source, the liquid quantum dot solution prepared is injected luminescent layer by the mode injected by hydraulic pressure, and concrete steps are as follows:
Step one, prepare the liquid quantum dot mixed solution of specific dimensions and kind;
Step 2, selection GaN luminescence chip or UV LED chip 3, carry out ultrasonic washing, UV treatment;
Step 3, luminescence chip 3 to be connected by gold thread 2 with electrode 1;
Step 4, epoxy resin/silica gel 4 is filled into chip surface, makes airtight glass partition 5 on epoxy resin/silica gel X surface, namely complete the making of luminescence chip base subsequently;
Step 5, making hemisphere glass envelope 7, the diameter of spherical glass shell is selected according to the actual requirements;
Step 6, open an aperture in hemisphere glass envelope 7, in the glove box being full of nitrogen, quantum dot solution is injected in hemisphere glass envelope, after being filled, and uses silica gel or epoxy resin to be sealed by aperture;
Step 7, place hemisphere plastic uptake acrylic plate 9 at spherical glass can 7, fill certain thickness second silica gel or epoxy resin 8 therebetween, thickness is determined by concrete condition, and silica gel or epoxy resin play the effect of packaging protection, completes the making of liquid quantum dot light emitting layer 6;
Step 8, the device that the 6th step completes to be mounted on luminescence chip base that the 4th step makes, to complete the preparation of liquid quantum dot LED.
In order to more specifically understand the present invention lucidly, it will be that embodiment is further elaborated technical scheme of the present invention with the manufacturing process of tellurium/cadmium selenide core shell (CdSe/CdS/ZnS) liquid quantum spot white light LED below: the liquid quantum spot white light LED structural design of tellurium/cadmium selenide core shell (CdSe/CdS/ZnS), comprise electrode, 460nm gallium-nitride blue chip, gold thread, glass partition, silica gel or epoxy resin layer, hemisphere glass seal layer, wherein to be filled with emission wavelength be the liquid quantum dot solution of 545nmCdSe/CdS/ZnS green glow and emission wavelength is the liquid quantum dot solution of 615nmCdSe/CdS/ZnS ruddiness, silica gel or epoxy resin and hemispheric plastic uptake acrylic plate.The diameter of the liquid quantum spot white light LED of cadmium selenide is 9.5mm, and height is 5.0mm.When operating voltage is 2.8 ~ 3.2V, luminous efficiency reaches 180 ~ 240lm/W, and corresponding colour temperature is 3000 ~ 9000K.
The present invention is not limited to this embodiment.
The technology of preparing scheme of tellurium/cadmium selenide core shell (CdSe/CdS/ZnS) liquid quantum spot white light LED is as follows:
Step one, prepare emission wavelength and be respectively the green glow CdSe/CdS/ZnS quantum dot solution of 545nm and the ruddiness CdSe/CdS/ZnS quantum dot of 615nm, and be dissolved in chloroformic solution, consult Fig. 2.
Concrete building-up process is: first, loads in the there-necked flask of 25mL, be heated to 77.04mg cadmium oxide (CdO), 677.9mg oleic acid (OA) and 8.1g1-octadecylene (ODE) 230 DEG C, obtain colourless, clear solution; After solution cool to room temperature, add 1.5g hexadecylamine (HAD) and 1.5g trioctyl phosphine oxide (TOPO), then mixture is heated to 280 DEG C; 0.285g selenium (Se), 0.472g tri octyl phosphine (TOP) are mixed with 1.106gODE, prepare Se precursor solution, be injected in above-mentioned reaction solution fast, the temperature of reactant mixture is reduced to 250 DEG C; Reactant mixture is further cooled to room temperature, through purifying and remove unreacted presoma, then is dissolved in n-hexane solvent by the CdSe particle of purifying.Secondly, 0.0448gCdO, 0.5935gOA and 8mLODE are mixed, is heated to 250 DEG C, obtains Cd parenteral solution (0.04M); By 0.0228g zinc oxide (ZnO), 0.3162gOA and 6.64mLODE mixing, be heated to 250 DEG C, obtain Zn parenteral solution (0.04M); Sulphur (S) is dissolved in ODE, is heated to 200 DEG C, obtain S parenteral solution (0.04M); Cd and Zn parenteral solution is cooled to 60 DEG C, by S parenteral solution cool to room temperature.3rd step carries out the growth of shell, is mixed by 5mLCdSe quantum dot, join in the there-necked flask of 25mL with 1500g octadecylamine (ODA), 5000gODE; Utilize mechanical pump, at ambient temperature, n-hexane is shifted out from there-necked flask, then mixture is heated to 180 DEG C; By one of Cd and Zn parenteral solution, join respectively in there-necked flask together with S parenteral solution, the reaction time is respectively 10 minutes.Finally, toluene is injected reactant mixture, cessation reaction, obtain CdSe/CdS/ZnS core-shell quanta dots, and be dissolved in chloroform.
Step 2, choose wavelength be the gallium-nitride blue chip of 460nm as excitaton source, carry out ultrasonic washing, UV treatment.
Step 3, gallium-nitride blue chip to be connected by gold thread with electrode.
Step 4, by epoxy resin filling to chip surface, make airtight glass partition at epoxy resin surface subsequently, namely complete the making of luminescence chip base.
Step 5, making diameter are 5.0mm, thickness is 0.1mm, height 2.5mm hemisphere glass envelope.
Step 6, open an aperture in hemisphere glass envelope, in the glove box being full of nitrogen, quantum dot solution is injected in hemisphere glass envelope, after being filled, and uses epoxy resin to be sealed by aperture.
Step 7, place hemispheric plastic uptake acrylic plate in hemisphere glass envelope, fill the silica gel of 0.05mm thickness therebetween, silica gel plays the effect of packaging protection, namely completes the making of liquid quantum dot light emitting layer.
Step 8, the liquid quantum dot light emitting layer that the 7th step completes to be mounted on luminescence chip base that the 4th step makes, to complete the preparation of liquid quantum dot LED, consult Fig. 3.
Different voltage is applied to cadmium selenide of the present invention (CdSe) liquid quantum spot white light LED, consults Fig. 4, find that it has good stability and luminous efficiency.

Claims (4)

1. liquid quantum dot LED, primarily of luminescence chip base and luminescent layer composition, described luminescence chip base comprises heat radiation substrate and exciting light active layer, it is characterized in that: described luminescent layer is liquid quantum dot.
2. liquid quantum dot LED as claimed in claim 1, is characterized in that: described liquid quantum dot is cadmium sulfide (CdS), cadmium selenide (CdSe), cadmium telluride (CdTe), copper indium sulphur (CuInS 2), copper indium diselenide (CuInSe 2), indium phosphide (InP), vulcanized lead (PbS), selenizing sulphur (PbSe), lead telluride (PbTe), zinc sulphide (ZnS), zinc selenide (ZnSe), zinc telluridse (ZnTe), polymer quantum dot or carbon quantum dot.
3. liquid quantum dot LED as claimed in claim 1, is characterized in that: the luminescence chip in described exciting light active layer is gallium nitride (GaN) chip or UV LED chip.
4. the preparation method of liquid quantum dot LED as claimed in claim 1, it is characterized in that: according to the requirement of described liquid quantum dot photoexcitation, select the luminescence chip of respective wavelength as excitation source, the liquid quantum dot prepared is injected luminescent layer by the mode injected by hydraulic pressure, and concrete steps are as follows:
Step one: prepare liquid quantum dot;
Step 2: the photoexcitation requirement of liquid quantum dot prepared by step one, selects luminescence chip, carries out ultrasonic cleaning, UV treatment;
Step 3: use gold thread to be connected with electrode by luminescence chip;
Step 4: by epoxy resin or silicone filler to the surface of luminescence chip, make airtight glass partition at epoxy resin or Silica Surface subsequently, namely complete the making of luminescence chip base;
Step 5: make glass envelope;
Step 6: machining small in glass envelope, in the glove box being full of nitrogen, is injected in glass envelope by liquid quantum dot, after being filled, uses silica gel or epoxy resin to be sealed by aperture;
Step 7: place plastic uptake acrylic board outside glass envelope, and filling gel or epoxy resin in space between glass envelope and plastic uptake acrylic board, namely complete the making of liquid quantum dot light emitting layer;
Step 8: the liquid quantum dot light emitting layer made by step 7 is mounted on the luminescence chip base of step 4 making, namely completes the preparation of liquid quantum dot LED.
CN201510624145.3A 2015-09-28 2015-09-28 Liquid quantum dot LED and preparation method thereof Pending CN105226146A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106450022A (en) * 2016-11-28 2017-02-22 深圳市华星光电技术有限公司 Organic light-emitting device and manufacturing method thereof
CN107195763A (en) * 2017-05-08 2017-09-22 安徽芯瑞达科技股份有限公司 A kind of cavity lens of quantum dot solution filling and preparation method thereof
CN107247362A (en) * 2017-06-19 2017-10-13 深圳市华星光电技术有限公司 Quantum dot optical module, quantum dot lens and its manufacture method
WO2017193312A1 (en) * 2016-05-11 2017-11-16 Huawei Technologies Co., Ltd. Quantum dot light-emitting device
CN109742220A (en) * 2018-12-25 2019-05-10 华中科技大学鄂州工业技术研究院 White light LEDs of the quantum dot containing liquid and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110240960A1 (en) * 2008-09-03 2011-10-06 Samsung Led Co., Ltd. Quantum dot-wavelength converter, manufacturing method of the same and light emitting device including the same
CN103155179A (en) * 2010-08-11 2013-06-12 Qd视光有限公司 Quantum dot based lighting
CN104755586A (en) * 2012-10-25 2015-07-01 皇家飞利浦有限公司 PDMS-based ligands for quantum dots in silicones

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110240960A1 (en) * 2008-09-03 2011-10-06 Samsung Led Co., Ltd. Quantum dot-wavelength converter, manufacturing method of the same and light emitting device including the same
CN103155179A (en) * 2010-08-11 2013-06-12 Qd视光有限公司 Quantum dot based lighting
CN104755586A (en) * 2012-10-25 2015-07-01 皇家飞利浦有限公司 PDMS-based ligands for quantum dots in silicones

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017193312A1 (en) * 2016-05-11 2017-11-16 Huawei Technologies Co., Ltd. Quantum dot light-emitting device
CN106450022A (en) * 2016-11-28 2017-02-22 深圳市华星光电技术有限公司 Organic light-emitting device and manufacturing method thereof
CN106450022B (en) * 2016-11-28 2018-04-06 深圳市华星光电技术有限公司 The manufacture method of organic luminescent device and organic luminescent device
CN107195763A (en) * 2017-05-08 2017-09-22 安徽芯瑞达科技股份有限公司 A kind of cavity lens of quantum dot solution filling and preparation method thereof
CN107247362A (en) * 2017-06-19 2017-10-13 深圳市华星光电技术有限公司 Quantum dot optical module, quantum dot lens and its manufacture method
CN109742220A (en) * 2018-12-25 2019-05-10 华中科技大学鄂州工业技术研究院 White light LEDs of the quantum dot containing liquid and preparation method thereof

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