CN105070796A - Method using water-soluble cadmium telluride quantum dot as light-emitting layer to build water-soluble quantum dot LED - Google Patents
Method using water-soluble cadmium telluride quantum dot as light-emitting layer to build water-soluble quantum dot LED Download PDFInfo
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- CN105070796A CN105070796A CN201510443506.4A CN201510443506A CN105070796A CN 105070796 A CN105070796 A CN 105070796A CN 201510443506 A CN201510443506 A CN 201510443506A CN 105070796 A CN105070796 A CN 105070796A
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- 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
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- 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
- H01L33/0083—Processes for devices with an active region comprising only II-VI compounds
- H01L33/0087—Processes for devices with an active region comprising only II-VI compounds with a substrate not being a II-VI compound
Abstract
The invention discloses a method using a water-soluble cadmium telluride quantum dot as a light-emitting layer to build a water-soluble quantum dot LED. The method comprises the steps that the film layer of ITO conductive glass is etched into strips; ultrasonic cleaning, removing out and drying are carried out; a PEDOT:PSS solution is spin-coated on the ITO conductive glass, and annealing is carried out; PVK is dissolved in toluene to form a solution and is spin-coated on a PEDO:PSS layer, and annealing is carried out; a water-soluble cadmium telluride solution is spin-coated on a PVK layer, and annealing is carried out; Alq3 is dissolved in ethanol and is spin-coated on a water-soluble cadmium telluride quantum dot layer, and annealing is carried out; and aluminizing is carried out on the Alq3 layer in a heat evaporation manner and in the manner of crosswise intersecting with the etched ITO film layer. According to the invention, the quantum dot LED is built based on the water-soluble cadmium telluride quantum dot; the electroluminescent property of the water-soluble quantum dot is verified; and the building method of the water-soluble cadmium telluride quantum dot LED is provided for the first time.
Description
Technical field
The present invention relates to and build technical field containing quantum dot LED, being specifically related to a kind of take water soluble cadmium telluride quantum point as the method that water-soluble quantum dot LED built by luminescent layer.
Background technology
Traditional LED mainly assembles at the fluorescent RE powder of blue-ray LED backlight surface-coated gold-tinted or orange red light.This LED component but has shortcomings, such as show the lower meeting of index and make object cross-color under LED illumination, fluorescent RE powder particle size is uneven, luminescent layer composition is difficult to control and makes LED light source different at different angles color coordinates, and in the whole world, rare earth expensively also have impact on its application in solid-state illumination and backlight industry for limes reacting dose.Compared with fluorescent RE powder, quantum dot advanced luminescent material has the advantages such as absorption region is wide, luminous zone is narrow, photostability is strong, and can obtain by its size of control and composition the various monochromatic light that glow color covers whole visible light wave range, therefore quantum dot can be used for LED field as a kind of novel luminescent material.But synthesize in oil-based system for the quantum dot major part of LED now, there is a large amount of nonconducting organic molecules in its surface, causes the luminous efficiency of device low.Compared with oil phase method, Aqueous phase has numerous advantage.Such as, do nontoxic solvent environmental protection with water and significantly reduce costs, the preparation temperature of milder makes the character of quantum dot have good controllability and repeatability, preparation process equal proportion amplification can carry out producing in batches thus more meets Product industrialization requirement, and the quantum dot surface preparing gained has a large amount of functional group and has good processability.Therefore, in aqueous phase, directly prepare the quantum dot with emissivities and be applied in LED field and have great importance, this by provide for solid-state illumination field a kind of low toxicity, stability is strong, machinability good, can be mass-produced, lower-cost New LED device.
Summary of the invention
The object of this invention is to provide a kind of take water soluble cadmium telluride quantum point as the method that water-soluble quantum dot LED built by luminescent layer, there is a large amount of nonconducting organic molecules to solve its surface of oil phase quantum dot adopted in traditional oils phase quantum dot LED, cause the problem that the luminous efficiency of device is low.
For achieving the above object, the present invention is by the following technical solutions:
Take water soluble cadmium telluride quantum point as the method that water-soluble quantum dot LED built by luminescent layer, it is characterized in that: comprise the steps:
Step one, the rete of ITO electro-conductive glass is etched into strip;
Step 2, cleaned by the ITO electro-conductive glass after etching, respectively with acetone, isopropyl alcohol, the ultrasonic each cleaning 15-30 minute of deionized water, taking-up nitrogen dries up;
Step 3, PEDOT:PSS solution sol evenning machine is spin-coated on ITO electro-conductive glass, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 4, PVK is dissolved in toluene is configured to solution, with sol evenning machine, PVK solution is spin-coated on PEDOT:PSS layer, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 5, water soluble cadmium telluride solution sol evenning machine is spin-coated on PVK layer, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 6, Alq3 is dissolved in ethanol, with sol evenning machine so that Alq3 solution is spin-coated on water soluble cadmium telluride quantum point layer, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 7, with the mode of thermal evaporation on Alq3 layer with etching after the mode of ito film layer right-angled intersection aluminize.
Preferably, in step 3, described PEDOT:PSS solution need first filter; During spin coating, sol evenning machine rotating speed is 2000rpm/s, and spin-coating time is 40s; Annealing temperature 150 DEG C, time 15min.
Preferably, in step 4, the concentration of described PVK solution is 10mg/mL; During spin coating, sol evenning machine rotating speed is 1000rpm/s, and spin-coating time is 40s; Annealing temperature 120 DEG C, time 35min.
Preferably, in step 5, described water soluble cadmium telluride solution is concentrated into through purifying the solution that concentration is 0.035mol/L; During spin coating, sol evenning machine rotating speed is 1000rpm/s, and spin-coating time is 40s; Annealing temperature 60 DEG C, time 35min.
Preferably, in step 6, described Alq3 solution is be solvent with ethanol, and concentration is 200mL/g, and the solution after filtering; During spin coating, sol evenning machine rotating speed is 1000rpm/s, and spin-coating time is 40s; Annealing temperature 60 DEG C, time 30min.
Preferably, in step 7, the aluminum layer thickness of aluminizing is 200nm.
The invention has the beneficial effects as follows:
1) the present invention is that luminescent layer is built the method validation of water-soluble quantum dot LED water-soluble quantum dot and had electroluminescence characters with water soluble cadmium telluride quantum point.
2) the present invention take water soluble cadmium telluride quantum point as the building method that the method that water-soluble quantum dot LED built by luminescent layer has initiated water soluble cadmium telluride quantum point LED, has successfully lighted water soluble cadmium telluride quantum point LED.
3) the present invention take water soluble cadmium telluride quantum point as the luminescent layer method of building water-soluble quantum dot LED for solid-state illumination field provide a kind of low toxicity, stability is strong, machinability good, can be mass-produced, lower-cost New LED device.
Accompanying drawing explanation
Fig. 1 is embodiments of the invention take water soluble cadmium telluride quantum point as the pictorial diagram that water-soluble quantum dot LED built by luminescent layer.
Fig. 2 is embodiments of the invention is that the illumination effect figure of water-soluble quantum dot LED when making alive 8V built by luminescent layer with water soluble cadmium telluride quantum point.
Fig. 3 is embodiments of the invention take water soluble cadmium telluride quantum point as the I-V curve chart that water-soluble quantum dot LED built by luminescent layer.
Fig. 4 for embodiments of the invention with water soluble cadmium telluride quantum point for the luminescence generated by light spectrogram of the ruddiness cadmium telluride quantum dot material that luminescent layer in water-soluble quantum dot LED adopts built by luminescent layer.
Fig. 5 is embodiments of the invention take water soluble cadmium telluride quantum point as the electroluminescence spectrogram that water-soluble quantum dot LED built by luminescent layer.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.The following example only for illustration of the present invention, but is not used for limiting practical range of the present invention.
Following examples caddy used, mercaptopropionic acid, NaOH, tellurium powder, sodium borohydride, PEDOT:PSS solution, PVK, Alq
3analytical reagent is Deng raw material.With deionized water rinse three times final vacuum dryings before glass apparatus used in experimentation uses.
Following examples sodium hydrogen telluride (NaHTe) solution is now with the current, and compound method comprises the steps: sodium borohydride to dissolve in deionized water, then adds rapidly tellurium powder; Seal reaction vessel with plug, plug communicates so that the hydrogen that produces of release reaction with a little pin hole with the external world; In course of reaction, system ice-water bath cools, and the tellurium powder of black disappears and produces the Boratex crystal of white afterwards, and the lavender solution of upper strata clarification is sodium hydrogen telluride solution.
Embodiment 1
Take water soluble cadmium telluride quantum point as the method that water-soluble quantum dot LED built by luminescent layer
1) the ito glass scotch tape adhesion of 2cm*2cm is gone out the strip region of two 0.4cm*2cm, again ito glass is put into concentrated hydrochloric acid and soak half an hour, take out, remove adhesive tape, with glue remaining on erased by rubber slice, thin piece, and clean up with liquid detergent.
2) ito glass etched is put into beaker, pour acetone soln, aqueous isopropanol and deionized water solution successively into, each ultrasonic cleaning 30 minutes.Take out, dry up with nitrogen, put into clean dry culture dish.
3), after being filtered with filtering head by PEDOT:PSS solution, be spin-coated on ito glass on the speed of 2000rpm/s by PEDOT:PSS solution with sol evenning machine, corotation is coated with 40s, then slice, thin piece is put into 15min that roasting Jiao Tai anneals at 150 DEG C.
4) PVK50mg is got, toluene 5mL, is configured to after concentration is the solution of 10mg/mL, be spin-coated on PEDOT:PSS thin layer with sol evenning machine with the speed of 1000rpm/s by PVK solution by ultrasonic for PVK being dissolved in toluene, corotation is coated with 40s, then slice, thin piece is put into 35min that roasting Jiao Tai anneals at 120 DEG C.
5) preparation of water-soluble CdTe quantum dots: add 40ml in the deionized water of 953ml, concentration is the CdCl of 0.1mol/L
2the mercaptopropionic acid (MPA) of solution and 835ul, fully stirring rear concentration is that 5mol/LNaOH regulates mixed solution pH to 9.0, uses N
2deoxidation, after 30 minutes, injects mixed solution with the NaHTe solution that syringe gets 1.2ml, concentration is 0.667mol/L.Stir after 10 minutes, heat 8 hours at 100 DEG C, obtain CdTe red quantum point solution.In final solution, the total concentration of Cd is 4 × 10
-3mol/L.The molar ratio of Cd/MPA/NaHTe is 1/2.4/0.2.
6) to add isopropyl alcohol centrifugal for water-soluble cadmium telluride quantum dot solution 35mL, and the powder obtained adds 4mL deionized water ultrasonic dissolution, just can purify and concentrate out the water soluble cadmium telluride solution that concentration is 0.035mol/L.Be spin-coated on PVK thin layer on the speed of 1000rpm/s by water soluble cadmium telluride solution with sol evenning machine, corotation is coated with 40s, then slice, thin piece is put into 35min that roasting Jiao Tai anneals at 60 DEG C.
7) 1gAlq is got
3, be dissolved under the state adding hot reflux in 200mL ethanol, be configured to 200mL/g solution and filter after, with sol evenning machine with the speed of 1000rpm/s by Alq
3solution is spin-coated on water soluble cadmium telluride quantum point thin layer, and corotation is coated with 40s, then slice, thin piece is put into 30min that roasting Jiao Tai anneals at 60 DEG C.
8) in the mode of thermal evaporation at Alq
3on layer with etching after the mode of ito film layer right-angled intersection plate two aluminium aluminum layer thickness for 200nm.As shown in Figure 1.
9) with voltage source to slice, thin piece making alive, ito thin film connects positive pole, and Al connects negative pole.When reaching cut-in voltage 7-8V, the part that on slice, thin piece, ito film layer and Al intersect can send ruddiness, and this is the light of red cadmium telluride quantum dot, as shown in Figure 2.
Fig. 1 is the present embodiment take water soluble cadmium telluride quantum point as the pictorial diagram that water-soluble quantum dot LED built by luminescent layer.As shown in Figure 1, LED slice, thin piece smooth surface is clean, and this illustrates that each layer has all well been spin-coated on slice, thin piece, and contacts smooth between layers.
Fig. 2 is the present embodiment is that the illumination effect figure of water-soluble quantum dot LED when making alive 8V built by luminescent layer with water soluble cadmium telluride quantum point.As shown in Figure 2, take water soluble cadmium telluride quantum point as the light that luminescent layer builds that water-soluble quantum dot LED can send quantum dot layer after reaching voltage, demonstrate water-soluble quantum dot and also there is electroluminescent characteristic.
Fig. 3 is the present embodiment take water soluble cadmium telluride quantum point as the I-V curve chart that water-soluble quantum dot LED built by luminescent layer.As can be seen from Figure 3, the cut-in voltage of this LED is about 7.5V, and when 10V, electric current is about 3mA.
Fig. 4 for the present embodiment with water soluble cadmium telluride quantum point for the luminescence generated by light spectrogram of the ruddiness cadmium telluride quantum dot material that luminescent layer in water-soluble quantum dot LED adopts built by luminescent layer.As can be seen from Figure 4, its luminous peak position is 650nm.
Fig. 5 is the present embodiment take water soluble cadmium telluride quantum point as the electroluminescence spectrogram that water-soluble quantum dot LED built by luminescent layer.As shown in Figure 5, the electroluminescence peak position of LED is 635nm, contrasts its luminescence generated by light peak position, slightly blue shift, illustrates that the characteristics of luminescence of water soluble cadmium telluride quantum point does not change.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. be the method that water-soluble quantum dot LED built by luminescent layer with water soluble cadmium telluride quantum point, it is characterized in that: comprise the steps:
Step one, the rete of ITO electro-conductive glass is etched into strip;
Step 2, cleaned by the ITO electro-conductive glass after etching, respectively with acetone, isopropyl alcohol, the ultrasonic each cleaning 15-30 minute of deionized water, taking-up nitrogen dries up;
Step 3, PEDOT:PSS solution sol evenning machine is spin-coated on ITO electro-conductive glass, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 4, PVK is dissolved in toluene is configured to solution, with sol evenning machine, PVK solution is spin-coated on PEDOT:PSS layer, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 5, water soluble cadmium telluride solution sol evenning machine is spin-coated on PVK layer, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 6, Alq3 is dissolved in ethanol, with sol evenning machine so that Alq3 solution is spin-coated on water soluble cadmium telluride quantum point layer, then slice, thin piece is put on roasting Jiao Tai and anneal;
Step 7, with the mode of thermal evaporation on Alq3 layer with etching after the mode of ito film layer right-angled intersection aluminize.
2. according to claim 1 is the method that water-soluble quantum dot LED built by luminescent layer with water soluble cadmium telluride quantum point, it is characterized in that: in step 3, and described PEDOT:PSS solution need first filter; During spin coating, sol evenning machine rotating speed is 2000rpm/s, and spin-coating time is 40s; Annealing temperature 150 DEG C, time 15min.
3. according to claim 1 is the method that water-soluble quantum dot LED built by luminescent layer with water soluble cadmium telluride quantum point, it is characterized in that: in step 4, and the concentration of described PVK solution is 10mg/mL; During spin coating, sol evenning machine rotating speed is 1000rpm/s, and spin-coating time is 40s; Annealing temperature 120 DEG C, time 35min.
4. according to claim 1 is the method that water-soluble quantum dot LED built by luminescent layer with water soluble cadmium telluride quantum point, it is characterized in that: in step 5, and described water soluble cadmium telluride solution is concentrated into through purifying the solution that concentration is 0.035mol/L; During spin coating, sol evenning machine rotating speed is 1000rpm/s, and spin-coating time is 40s; Annealing temperature 60 DEG C, time 35min.
5. according to claim 1 is the method that water-soluble quantum dot LED built by luminescent layer with water soluble cadmium telluride quantum point, it is characterized in that: in step 6, and described Alq3 solution is take ethanol as solvent, and concentration is 200mL/g, and the solution after filtering; During spin coating, sol evenning machine rotating speed is 1000rpm/s, and spin-coating time is 40s; Annealing temperature 60 DEG C, time 30min.
6. according to claim 1 is the method that water-soluble quantum dot LED built by luminescent layer with water soluble cadmium telluride quantum point, it is characterized in that: in step 7, and the aluminum layer thickness of aluminizing is 200nm.
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Citations (4)
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|---|---|---|---|---|
| CN103247731A (en) * | 2013-04-16 | 2013-08-14 | 苏州瑞晟太阳能科技有限公司 | Novel light-operated light emitting diode based on nano material |
| CN103441220A (en) * | 2013-09-16 | 2013-12-11 | 东南大学 | White light quantum dot light emitting diode and preparation method thereof |
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| CN103840053A (en) * | 2014-03-14 | 2014-06-04 | 东南大学 | Surface-plasma-enhanced quantum dot light-emitting diode device and manufacturing method thereof |
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- 2015-07-24 CN CN201510443506.4A patent/CN105070796B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103247731A (en) * | 2013-04-16 | 2013-08-14 | 苏州瑞晟太阳能科技有限公司 | Novel light-operated light emitting diode based on nano material |
| CN103441220A (en) * | 2013-09-16 | 2013-12-11 | 东南大学 | White light quantum dot light emitting diode and preparation method thereof |
| CN103840048A (en) * | 2014-03-14 | 2014-06-04 | 东南大学 | Inverted type full inorganic nanometer oxide quantum dot light-emitting diode and manufacturing method thereof |
| CN103840053A (en) * | 2014-03-14 | 2014-06-04 | 东南大学 | Surface-plasma-enhanced quantum dot light-emitting diode device and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
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| 杜锦华等: "脱水硅酸凝胶状的水溶性CdTe量子点及LED应用", 《中国化学会第29届学术年会摘要集》 * |
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