CN108346752A - A kind of preparation method and application of light emitting diode with quantum dots - Google Patents
A kind of preparation method and application of light emitting diode with quantum dots Download PDFInfo
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- CN108346752A CN108346752A CN201810046972.2A CN201810046972A CN108346752A CN 108346752 A CN108346752 A CN 108346752A CN 201810046972 A CN201810046972 A CN 201810046972A CN 108346752 A CN108346752 A CN 108346752A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
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Abstract
The present invention provides a kind of preparation methods of light emitting diode with quantum dots, including：Substrate is provided, first electrode is prepared in the substrate surface；Light emitting functional layer is prepared in the first electrode surface, the light emitting functional layer includes at least quantum dot light emitting layer；Second electrode is prepared in the light emitting functional layer, obtains initial quantum point luminescent diode；The initial quantum point luminescent diode is integrally made annealing treatment, light emitting diode with quantum dots is obtained.The preparation method is simple for process, can be used for industrialized production, and light emitting diode with quantum dots obtained has very high luminous efficiency and outstanding luminescent properties.The present invention also provides the applications of light emitting diode with quantum dots.
Description
Technical field
The invention belongs to technical field of semiconductor luminescence more particularly to a kind of preparation sides of light emitting diode with quantum dots
Method and application.
Background technology
Quantum dot (Quantum Dot, QD) is typically a kind of nano particle being made of II-VI group or iii-v element,
Fluorescence can be emitted after being excited, luminescent spectrum can be controlled by changing the size of quantum dot, and its fluorescence intensity
It is all fine with stability, it is a kind of good electroluminescent material.Quantum dot is inexpensive by it, energy expenditure is low, raw material
The advantages such as utilization rate is high, environmental pollution is small, are answered extensively in fields such as light emitting diode, solar cell and biological fluorescent labellings
With.It is hair with quantum dot compared to existing Organic Light Emitting Diode (Organic Light-Emitting Diode, OLED)
The light emitting diode with quantum dots (Quantum Dot Light-Emitting Diode, QLED) of photosphere has the excitation purity that shines
Height, color tunable control, stability is good, can whole soln processing the advantages that, therefore QLED is the next-generation display technology of great potential
With solid-state lighting light source.In addition, the great advantage of QLED is luminance purity higher, therefore the display screen based on QLED will have more
Wide display colour gamut can preferably show the realistic colour of nature, and truer abundant vision body is brought for the mankind
It tests.
Currently, the preparation process of QLED achieves significant progress, and tentatively have commercialized primary condition,
But there are still problems are urgently to be resolved hurrily before QLED achievees the effect that the full-color display of high-resolution dynamic.Existing QLED
In carrier transport inadequate balance, QLED stablizes not enough, luminous efficiency and light emission luminance be not high, especially blue light
The luminous efficiency of QLED is very low.
Therefore, it is necessary to study go out a kind of simple, efficient preparation process for promoting QLED luminescent properties.
Invention content
In view of this, the present invention provides a kind of preparation method and application of light emitting diode with quantum dots, the quantum dot
The preparation method of light emitting diode is simple for process, can be used for industrialized production, and light emitting diode with quantum dots obtained has very high
Luminous efficiency, outstanding luminescent properties.
In a first aspect, the present invention provides a kind of preparation methods of light emitting diode with quantum dots, including：
Substrate is provided, first electrode is prepared in the substrate surface；
Light emitting functional layer is prepared in the first electrode surface, the light emitting functional layer includes at least quantum dot light emitting
Layer；
Second electrode is prepared in the light emitting functional layer, obtains initial quantum point luminescent diode；
The initial quantum point luminescent diode is integrally made annealing treatment, light emitting diode with quantum dots is obtained.
Optionally, the temperature of the annealing is 50-300 DEG C, annealing time 0.1-30min.Optionally, described to move back
The temperature of fire processing is 200-300 DEG C.Further, it is preferable to ground, the temperature of the annealing is 255-300 DEG C.Optionally,
The annealing time is 5-25 minutes.Further, it is preferable to ground, the annealing time is 20-30 minutes.Due to the knot of quantum dot
Structure, material composi and of different sizes, annealing temperature that the light emitting diode with quantum dots handles the after annealing and
The requirement of annealing time is different；The annealing temperature of the after annealing can be according to quantum dot light emitting layer difference with annealing time
And it accordingly adjusts.
Wherein, the operation of annealing of the present invention can carry out in air, vacuum or atmosphere of inert gases.It is described
Air atmosphere includes laboratory place or common external environment；The vacuum refers to that gas pressure intensity is less than 5 × 10-4Pa's is close
Closed chamber body；The atmosphere of inert gases includes the airtight cavity full of nitrogen, argon gas, helium, neon or other inert gases.
Optionally, the light emitting functional layer be included in the first electrode surface stack gradually preparation hole injection layer,
Hole transmission layer, quantum dot light emitting layer, electron transfer layer and electron injecting layer；Or the light emitting functional layer is included in described first
Electrode surface stacks gradually electron injecting layer, electron transfer layer, quantum dot light emitting layer, hole transmission layer and the hole injection of preparation
Layer.
Optionally, the material of the first electrode includes indium tin oxide (indium tin oxide, ITO), indium zinc oxygen
One kind in compound (indium zinc oxide, IZO) and Al-Doped ZnO (Aluminum doped Zinc Oxid, AZO)
Or it is a variety of；The material of the second electrode includes one kind or more in aluminium (Al), silver (Ag), gold (Au), copper (Cu) and magnesium (Mg)
Kind.Such as the material of the second electrode is aluminium, or be silver, or be gold, or be copper magnesium alloy, or be albronze, or be gold
Copper alloy, or be copper magnesium alloy, or be copper magnalium silver alloy.Optionally, the thickness of the second electrode is 70-300nm.Into
Optionally, the thickness of shown second electrode is 200-300nm to one step.
Optionally, the material of the quantum dot light emitting layer includes red light quantum point material, green light quantum point material and blue light
It is one or more in quanta point material.
Optionally, the thickness of the quantum dot light emitting layer is 10-30nm.
Optionally, the material of the quantum dot light emitting layer includes the cadmium system quantum dot for having nucleocapsid or alloy structure.
Cadmium system quantum dot includes CdZnSeS/ZnS.A diameter of 5-20nm of cadmium system quantum dot.The alloy structure refers to packet
It is alloy material to cover quantum dot nuclear structure outer layer or shell.
Optionally, the specific preparation process of the quantum dot light emitting layer includes：By the quantum dot light emitting containing surface ligand
Layer material, which is dissolved in organic solvent, obtains mixed slurry, and the mixed slurry is carried out with the spin coating rotating speed of 2000-3000r/min
Spin coating then toasts 4-8min in 80-120 DEG C.The organic solvent includes one kind or more in normal octane, n-hexane and chlorobenzene
Kind.The surface ligand includes one or more in oleic acid (Oleic acid) and mercaptan (Thioalcohol).
Optionally, the hole injection layer and the hole transmission layer, the hole injection are prepared by the way of spin coating
The material of layer includes poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid (PEDOT:PSS), molybdenum oxide (MoOx), vanadium oxide
(VOx), tungsten oxide (WOx) and nickel oxide (NiOx) in it is one or more, the material of the hole transmission layer includes PVK, TFB
With it is one or more in Poly-TPD.Wherein, the PVK is organic polymer polyvinylcarbazole, and the TFB is organic polymer
Object is poly-, and ((9,9- dioctyl fluorene -2,7- diyl)-is total (4,4'- (N- (4- sec-butyls phenyl) diphenylamines)), the Poly-TPD
It is poly- (bis- bis- (phenyl) benzidine of (4- butyl phenyls)-N, N'- of N, N'-) for organic polymer.
Optionally, the specific preparation process of the hole injection layer includes：The sky of the first solvent will be dissolved in using spin-coating method
Cave injects layer material and carries out spin coating, is toasted after spin coating, and spin coating rotating speed is 2000-3000r/min, baking temperature 130-
150 DEG C, time 10-20min.First solvent includes one kind or more in water, chlorobenzene, o-dichlorohenzene, toluene, dichloromethane
Kind.The thickness of the hole injection layer is 15-50nm.
Optionally, the specific preparation process of the hole transmission layer includes：The sky of the second solvent will be dissolved in using spin-coating method
Cave transmits layer material and carries out spin coating, is toasted after spin coating, and spin coating rotating speed is 4000-5000r/min, baking temperature 100-
120 DEG C, baking time 10-30min.Second solvent includes one or more in chlorobenzene, toluene and dichloromethane.It is described
The thickness of hole transmission layer is 10-50nm.
Optionally, the electron injecting layer or the electron transfer layer, the electron injection are prepared by the way of spin coating
The material of layer or the electron transfer layer includes zinc oxide (ZnO) nano particle, doping zinc oxide nanometer particle and titanium dioxide
(TiO2) one or more in nano particle.The doping zinc oxide nanometer particle includes ZnxMg1-xO and ZnxGa1-xOne kind in O
Or it is a variety of.The thickness of the electron injecting layer is 30-100nm.The thickness of the electron transfer layer is 30-100nm.
Optionally, using electron injecting layer described in magnetron sputtering method or the electron transfer layer.
Optionally, the specific preparation process of the electron transfer layer or electron injecting layer includes：By the electron transfer layer
Material or the electron injecting layer material are dissolved in third solvent, and band carries out spin coating after mixing, is dried after the completion of spin coating
Roasting, the rotating speed of the spin coating is 2000-3000r/min, and the temperature of the baking is 80-120 DEG C, and the time of the baking is
10-20min.The third solvent is alcohol reagent.Specifically, the third solvent includes one kind or more in methanol and ethyl alcohol
Kind.
Optionally, the material of the substrate includes hard material or flexible material.Further, optionally, the substrate
Material include glass, polyethylene, polypropylene, polystyrene, polylactic acid, polyethylene terephthalate, polyimides and
It is one or more in polyurethane.
Optionally, it is described the initial quantum point luminescent diode is integrally made annealing treatment after further include：Using
Laser lift-off makes the first electrode be detached with the substrate.
Annealing of the present invention is all to complete that initial quantum is prepared in each functional layer of light emitting diode with quantum dots
After point luminescent diode, the whole full device of the initial quantum point luminescent diode is subjected to after annealing processing.The after annealing
Processing operation can be effectively improved the contact interface between electrode (first electrode or second electrode) light emitting functional layer adjacent thereto,
And the contact interface of the electron injecting layer/electron transfer layer and quantum dot light emitting layer in light emitting functional layer structure；On the one hand have
Effect reduces contact resistance, on the other hand inhibits the nonradiative transition of exciton, to achieve the effect that promote device performance,
Such as the luminescent properties of device.Further, electrode hair adjacent thereto can be effectively facilitated after after annealing processing of the present invention
Contact between light functional layer is even closer, is conducive to the injection of carrier；Simultaneously as the hole transmission layer and the sky
Cave implanted layer has lower lumo energy, effectively electronics can be inhibited to reveal, and injected electrons is effectively blocked in described
Quantum dot light emitting layer.
Optionally, described by the way of chemical vapor deposition, physical vapour deposition (PVD), magnetron sputtering, vapor deposition or coating
Lighting function layer surface prepares the second electrode.Second electrode of the present invention has excellent electric conductivity, and can be
Light emitting functional layer that can be adjacent thereto after the after annealing processing is in close contact.
The preparation method for the light emitting diode with quantum dots that the first aspect of the present invention provides, simple process and low cost is honest and clean, can
For industrialized production；Have stable luminescent property, luminous efficiency high by light emitting diode with quantum dots prepared by the preparation method
The strong feature with light emission luminance has stronger luminescent properties compared to existing light emitting diode with quantum dots.
Second aspect, the present invention provides a kind of quantum dot hairs prepared by the preparation method by described in first aspect present invention
Optical diode, the light emitting diode with quantum dots include red quantum point luminescent diode, green quantum point luminescent diode and
It is one or more in blue light quantum point light emitting diode；It is in close contact between each functional layer of light emitting diode with quantum dots,
With stabilization, efficient luminescent properties.The light emitting diode with quantum dots can be used for showing equipment, which can be aobvious
Show device, mobile phone, computer or smartwatch.
Advantages of the present invention will be illustrated partly in the following description, and a part is apparent according to specification
, or can be through the embodiment of the present invention implementation and know.
Description of the drawings
Fig. 1 is the process flow chart for the QLED preparation methods that one embodiment of the invention provides；
Fig. 2 is the QLED structural schematic diagrams that one embodiment of the invention provides；
Fig. 3 is the voltage-current density curve for the QLED that one embodiment of the invention provides；
Fig. 4 is the voltage-brightness curve for the QLED that one embodiment of the invention provides；
Fig. 5 is the current density-current efficiency curve for the QLED that one embodiment of the invention provides；
Fig. 6 is the current density-external quantum efficiency curve for the QLED that one embodiment of the invention provides；
Fig. 7 is the current density-energy efficient curves for the QLED that one embodiment of the invention provides.
Specific implementation mode
As described below is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Unless otherwise noted, raw material used by the embodiment of the present invention and other chemical reagent are all commercial goods.
The present invention provides a kind of preparation methods of light emitting diode with quantum dots, as shown in Figure 1, including：
S10, substrate is provided, first electrode is prepared in the substrate surface；
S20, light emitting functional layer is prepared in the first electrode surface, the light emitting functional layer is sent out including at least quantum dot
Photosphere；
S30, second electrode is prepared in the light emitting functional layer, obtains initial quantum point luminescent diode；
S40, the initial quantum point luminescent diode is integrally made annealing treatment, obtains light emitting diode with quantum dots.
In embodiment of the present invention, in S10, the material of the substrate include glass, polyethylene, polypropylene, polystyrene,
It is one or more in polylactic acid, polyethylene terephthalate, polyimides and polyurethane.The substrate can have compared with
High laser transmittance, in order to being smoothed out for post laser stripping process.Certainly, in order to make substrate with it is subsequent first electricity
Pole combines more preferably, can be surface-treated substrate, improve the surface energy of the substrate.Using chemical vapor deposition, physics
Vapor deposition, magnetron sputtering, vapor deposition or coating method prepare first electrode in the substrate surface.The first electrode includes
It is one or more in indium tin oxide, indium-zinc oxide and Al-Doped ZnO.
In embodiment of the present invention, in S20, the light emitting functional layer can also be included in the first electrode surface successively
Hole injection layer, hole transmission layer, quantum dot light emitting layer, electron transfer layer and the electron injecting layer prepared is laminated；Or the hair
Light functional layer is included in the electron injecting layer, electron transfer layer, quantum dot light emitting that the first electrode surface stacks gradually preparation
Layer, hole transmission layer and hole injection layer.The hole injection layer and the hole transmission layer can be respectively individual structure；
Or the hole injection layer and the hole transmission layer can have be integral, the cavitation layer of a single layer structure.The electronics passes
Defeated layer and the electron injecting layer can be respectively individual structure；Or the electron transfer layer and the electron injecting layer can be with
Have be integral, the cavitation layer of a single layer structure.The quantum dot light emitting layer can be blue light quantum point luminescent layer, red quantum
It is one or more in point luminescent layer and green light quantum point luminescent layer.
In embodiment of the present invention, in S30, using chemical vapor deposition, physical vapour deposition (PVD), magnetron sputtering, vapor deposition or
The mode of coating prepares the second electrode in the lighting function layer surface.The material of the second electrode include Al, Ag,
It is one or more in Cu, Au and Mg.It is described effectively to provide driving voltage to intermediate quantum dot light emitting layer.It is optional
The thickness on ground, the second electrode is 70-300nm.Further, optionally, the thickness of the second electrode is 80-200nm.
Such as the thickness of the second electrode is 90nm, or be 160nm, or be 180nm, or be 200nm, or be 250nm.This embodiment party
In formula, the second electrode is conducive to provide the driving voltage stablized enough for intermediate quantum dot light emitting layer.
In embodiment of the present invention, in S40, the temperature of the annealing is 50-300 DEG C, annealing time 0.1-30
Minute.Optionally, the temperature of the annealing is 200-300 DEG C.Optionally, the annealing time is 5-25 minutes.Into one
Step ground, it is preferable that the annealing time is 20-30 minutes.Such as the temperature of the annealing can be invariable or described
The temperature of annealing is arranged for change of program.Such as the temperature of the annealing rises to 250 DEG C from 205 DEG C, heating rate
To heat up 15 DEG C every 30s.The operation of the annealing can carry out in air, vacuum or atmosphere of inert gases.
In embodiment of the present invention, it can only pass through the full device annealing operation of a step, the technique letter of the preparation method
It is single efficient.It can also be passed in the hole injection layer, hole transmission layer, quantum dot light emitting layer, electronics in embodiment of the present invention
Annealing operation is carried out in one or more layers preparation process in defeated layer and electron injecting layer.Such as the hole injection layer,
It anneals in the preparation process of every layer of structure of hole transmission layer, quantum dot light emitting layer, electron transfer layer and electron injecting layer
Processing, and finally carry out full device annealing；Or the system in the hole injection layer, hole transmission layer, quantum dot light emitting layer
It anneals during standby, and finally carries out full device annealing.
Present embodiment is additionally providing a kind of light emitting diode with quantum dots prepared by above-mentioned preparation method, sees Fig. 2 institutes
State, including be cascading substrate 101, first electrode 102, hole injection layer 103, hole transmission layer 104, quantum dot hair
Photosphere 105, electron transfer layer 106 and second electrode 107, the hole injection layer 103, hole transmission layer 104, quantum dot light emitting
Layer 105 and electron transfer layer 106 constitute light emitting functional layer.
The specific material of hole injection layer 103 described in present embodiment is not particularly limited, it is in the art it is any
The hole generation type semi-conducting material known, those skilled in the art can select according to actual conditions.Preferably, described
The material of hole injection layer 103 is PEDOT:PSS、MoOX、VOX、WOXAnd NiOXIn it is one or more.Using above-mentioned material
The hole injection layer 103 have good transparency, have and the matched work function of adjacent layer, be conducive to hole to quantum dot hair
The injection of photosphere, and can realize prepared by solwution method.
Present embodiment exists, and the specific material of the hole transmission layer 104 is not particularly limited, and in the art is any
Known hole-transporting type material, as long as the hole transmission layer 104 has good hole injection transmittability and has
The blocking electronic capability of effect.Preferably, the material of the hole transmission layer includes one kind in PVK, TFB and Poly-TPD
Or it is a variety of.The hole transmission layer of currently preferred material preparation has good hole-conductive ability, and translucency is preferable,
Also there is more matched work function with quantum dot light emitting layer.
In present embodiment, the specific material of the electron transfer layer 106 is not particularly limited, it is in the art it is any
The electron-transporting type metal oxide semiconductor known or the defeated type semiconducting organic materials of electrical transmission, those skilled in the art
It can be selected according to actual conditions.Preferably, the material of the electron transfer layer 106 includes ZnO nano particle, doping ZnO
Nano particle and TiO2It is one or more in nano particle.Using the electron-transport 106 of above-mentioned material, have good saturating
Bright property, with high electron transport ability and with quantum dot light emitting layer with more matched work function.The electron transfer layer 106
The function of electron-transport and electron injection can also be provided simultaneously with.
In present embodiment, one layer can also be stacked between the electron transfer layer 106 and the second electrode 107
Electron injecting layer, the electron injecting layer can effectively improve carrier injectability, improve the light emitting diode with quantum dots
Luminous efficiency.The material of the electron injecting layer includes ZnO nano particle, doping zinc oxide nanometer particle and TiO2Nano particle
In it is one or more.
In present embodiment, the material concentration of the hole injection layer, the material concentration of the hole transmission layer, the amount
Material concentration, the material concentration of the electron transfer layer or the material concentration of the electron injecting layer of son point luminescent layer are 10-
40mg/mL.It is more superior in the concentration range to be that material preparation comes out functional layer structure performance, and distribution is more balanced.
In present embodiment, the material of the quantum dot light emitting layer 105 includes red light quantum point material, green light quantum point material
It is one or more in material and blue light quantum point material.
Embodiment 1
Blue light QLED devices are used to prepare in the present embodiment, wherein quantum dot light emitting layer includes blue quanta point material, this
Place is known as blue light quantum point luminescent layer.Specifically, the structure of the blue light QLED devices stacks gradually from bottom to top is equipped with：Glass
Substrate, ito thin film (first electrode), hole injection layer, hole transmission layer, blue light quantum point luminescent layer, electron transfer layer and gold
Belong to electrode layer (second electrode).Specifically preparation process includes：
(1) take ito glass substrate, electrode pattern produced using photoetching technique, then substrate is successively respectively placed in washing lotion,
It is cleaned by ultrasonic in deionized water, three times, each ultrasonic time is 30min to ultrasound, waits after the completion of being cleaned by ultrasonic, substrate is put
It is placed in cleaning oven and is dried for standby.
(2) substrate of glass of the surface with ito thin film is handled 15 minutes using UV ozone, is then made on the surface thereof
Make light emitting functional layer.Specifically, hole injection layer, hole transmission layer, blue light quantum point hair are prepared on ito thin film surface successively
Photosphere, electron transfer layer, metal electrode layer, concrete operations include：
Water-soluble polyelectrolyte polystyrolsulfon acid (PSS) will be used to make the 3,4- ethylene adulterated using spin-coating method
The polymer P EDOT of dioxythiophene monomers (EDOT)：PSS water-soluble liquids are toasted after being spin-coated to the ito thin film surface,
Spin coating rotating speed is 2000r/min, and baking temperature is 150 DEG C, and baking time 15min obtains hole injection layer；
It is toasted after the PVK mixed liquors for being dissolved in chlorobenzene are spin-coated to the hole injection layer surface using spin-coating method, PVK
A concentration of 15mg/mL, spin coating rotating speed are 4000r/min, and 100 DEG C of baking temperature, baking time 10min obtains hole transmission layer；
By CdZnSeS/ZnS nucleocapsids alloy quantum dot, (core CdZnSeS, wherein main component are Cd, surface package
Alloying component, shell ZnS) it is dissolved in normal octane solution, a concentration of 15mg/mL, the quantum dot surface contains oleic acid ligand,
Blue light quantum point luminescent layer is prepared in the hole transport layer surface using rotary process；Rotary speed is 2000r/min, baking temperature
Degree is 80 DEG C, time 5min, a diameter of 10nm of CdZnSeS/ZnS quantum dots；
The Zn of ethyl alcohol will be dissolved in using spin-coating methodxMg1-xO nano particle mixed liquors are spin-coated to the blue light quantum point and shine
It is toasted after layer surface, ZnxMg1-xA concentration of 20mg/mL of O nano particles, spin-coating time rotating speed are 2000r/min, baking
120 DEG C of temperature, time 10min obtain electron transfer layer.
(3) material of electrode is aluminum metal, deposits 150nm's on the electron transport layer using the method for vacuum evaporation
Aluminium film obtains original blue light quantum dot diode.
(4) under inert gas conditions, the original blue light quantum dot diode that step (3) obtains is placed on hot plate whole
It anneals, annealing temperature is 260 DEG C, and annealing time 5min obtains blue light QLED.
Comparative example 1
Blue light QLED devices are used to prepare in this comparative example 1, wherein quantum dot light emitting layer includes blue quanta point material, this
Place is known as blue light quantum point luminescent layer.Specifically, the structure of the blue light QLED devices stacks gradually from bottom to top is equipped with：Glass
Substrate, ito thin film (first electrode), hole injection layer, hole transmission layer, blue light quantum point luminescent layer, electron transfer layer and gold
Belong to electrode layer (second electrode).Specifically preparation process includes：
(1) take ito glass substrate, electrode pattern produced using photoetching technique, then substrate is successively respectively placed in washing lotion,
It is cleaned by ultrasonic in deionized water, three times, each ultrasonic time is 30min to ultrasound, waits after the completion of being cleaned by ultrasonic, substrate is put
It is placed in cleaning oven and is dried for standby.
(2) substrate of glass of the surface with ito thin film is handled 15 minutes using UV ozone, is then made on the surface thereof
Make light emitting functional layer.Specifically, hole injection layer, hole transmission layer, blue light quantum point hair are prepared on ito thin film surface successively
Photosphere, electron transfer layer, metal electrode layer, concrete operations include：
The 3,4- ethylene dioxies that will make to adulterate using water-soluble polyelectrolyte polystyrolsulfon acid using spin-coating method
The polymer P EDOT of thiophene monomer：PSS water-soluble liquids are toasted after being spin-coated to the ito thin film surface, and spin coating rotating speed is
2000r/min, baking temperature are 150 DEG C, and baking time 15min obtains hole injection layer；
It is toasted after the PVK mixed liquors for being dissolved in chlorobenzene are spin-coated to the hole injection layer surface using spin-coating method, PVK
A concentration of 15mg/mL, spin coating rotating speed are 4000r/min, and 100 DEG C of baking temperature, baking time 10min obtains hole transmission layer；
CdZnSeS/ZnS nucleocapsid alloy quantum dots are dissolved in normal octane solution, a concentration of 15mg/mL, are used
Rotary process prepares blue light quantum point luminescent layer in the hole transport layer surface；Rotary speed is 2000r/min, and baking temperature is
80 DEG C, time 5min, a diameter of 10nm of CdZnSeS/ZnS quantum dots；
The ZnxMg1-xO nano particle mixed liquors for being dissolved in ethyl alcohol the blue light quantum point is spin-coated to using spin-coating method to shine
It is toasted after layer surface, a concentration of 20mg/mL of ZnxMg1-xO nano particles, spin-coating time rotating speed is 2000r/min, is dried
Roasting 120 DEG C of temperature, time 10min obtain electron transfer layer.
(3) material of electrode is aluminum metal, deposits 150nm's on the electron transport layer using the method for vacuum evaporation
Aluminium film obtains the blue light quantum point diode of non-integrally annealed.
It will be proceeded through under identical test environment by embodiment 1 and QLED made from preparation method described in comparative example 1
Experiments of Electricity are tested, as a result as follows：
Fig. 3 is the QLED voltage-current density curve graphs of embodiment 1 and comparative example 1, apparent can be obtained from figure
When voltage is more than 6V, the current density of QLED (embodiment 1) is better than the current density of QLED (comparative example 1)；When voltage is equal to
When 8V, the current density of QLED (embodiment 1) is 3 times or so of the current density of QLED (comparative example 1).From the figure 3, it may be seen that by
The QLED (embodiment 1) of integrally annealed processing is more advantageous to load compared to the QLED (comparative example 1) handled without integrally annealed
The injection of son is flowed, current density is promoted.
Fig. 4 is the voltage-brightness curve graph of embodiment 1 and the QLED of comparative example 1, can obtain from figure and be more than in voltage
When 6V, the brightness for the QLED (comparative example 1) that the brightness of QLED (embodiment 1) is better than；When voltage is equal to 12V, QLED (comparative examples
1) brightness is 1.9 × 104cd/m2, the brightness of QLED (embodiment 1) is 2.8 × 104cd/m2, i.e., in the identical voltage,
The brightness of QLED (embodiment 1) is 1.47 times of QLED (comparative example 1) brightness.As shown in Figure 4, by integrally annealed processing
QLED (embodiment 1) is compared to the luminous efficiency higher of the QLED (comparative example 1) handled without integrally annealed, and luminous intensity is more
It is outstanding.
Fig. 5 is current density-current efficiency curve graph of the QLED of embodiment 1 and comparative example 1, can be obtained from figure with
The increase of current density, the current efficiency of QLED (embodiment 1) is higher than QLED (comparative example 1), when current density is
100mA/cm2, the current efficiency of QLED (comparative example 1) is 4.2cd/A, and the current efficiency of QLED (embodiment 1) is 7.8cd/
A, i.e., in the same current density, the current efficiency of QLED (embodiment 1) is the 1.86 of QLED (comparative example 1) current efficiency
Times.
Fig. 6 is current density-external quantum efficiency curve graph of embodiment 1 and the QLED of comparative example 1, can be obtained from figure
With the increase of current density, the external quantum efficiency of QLED (embodiment 1) is higher than QLED (comparative example 1), when current density is
100mA/cm2, the external quantum efficiency of QLED (embodiment 1) is 9.7%, and the external quantum efficiency of QLED (comparative example 1) is
5.1%, the external quantum efficiency of QLED (embodiment 1) at this time is 1.9 times of the external quantum efficiency of QLED (comparative example 1), explanation
QLED (embodiment 1) shining compared to the QLED (comparative example 1) handled without integrally annealed by integrally annealed processing
Performance is stronger.
Fig. 7 is current density-energy efficient curves figure of the QLED of embodiment 1 and comparative example 1, can be obtained from figure with
The increase of current density, the energy efficiency (or luminous efficiency) of QLED (embodiment 1) is higher than QLED (comparative example 1), when
Current density is 100mA/cm2, the energy efficiency of QLED (comparative example 1) is 1.6Im/W, and the energy dose-effect of QLED (embodiment 1)
Rate is 3.2Im/W, i.e., in the same current density, QLED (embodiment 1) energy efficiency is QLED (comparative example 1) energy efficiency
2 times.
To sum up, due to by integrally annealed processing QLED compared to the QLED that non-integrally annealed is handled electrode (including
First electrode and second electrode) contact resistance of functional layer adjacent thereto reduces, i.e. connecing between electrode functional layer adjacent thereto
It is tactile even closer, be conducive to the injection of carrier；Simultaneously as hole transmission layer and hole injection layer have lower LUMO energy
Grade, effectively can inhibit electronics to reveal, injected electrons is effectively blocked in quantum dot light emitting layer.Whole after annealing operation has
Conducive to the Exciton quenching center of electron injection/transport layer and quantum dot interface is reduced, to be conducive to inhibit the non-radiative of exciton
Transition improves the luminous efficiency of quantum dot.It is identical be under the conditions of, the current density, bright of the QLED by integrally annealed processing
The QLED of degree, current efficiency, external quantum efficiency and energy efficiency parameter than non-integrally annealed processing is outstanding (see Fig. 3-Fig. 7
Electrical testing experimental result shown in).
Embodiment 2
Green light QLED devices are used to prepare in the present embodiment, wherein quantum dot light emitting layer includes green light quantum point material, this
Place is known as green light quantum point luminescent layer.Specifically, the structure of the green light QLED devices stacks gradually from bottom to top is equipped with：Glass
Substrate, ito thin film (first electrode), hole injection layer, hole transmission layer, green light quantum point luminescent layer, electron transfer layer and gold
Belong to electrode layer (second electrode).Specifically preparation process includes：
(1) take ito glass substrate, electrode pattern produced using photoetching technique, then substrate is successively respectively placed in washing lotion,
It is cleaned by ultrasonic in deionized water, ultrasound is secondary, and each ultrasonic time is 40min, waits after the completion of being cleaned by ultrasonic, substrate is put
It is placed in cleaning oven and is dried for standby.
(2) substrate of glass of the surface with ito thin film is handled 15 minutes using UV ozone, is then made on the surface thereof
Make light emitting functional layer.Specifically, hole injection layer, hole transmission layer, green light quantum point hair are prepared on ito thin film surface successively
Photosphere, electron transfer layer, metal electrode layer, concrete operations include：
The MoO of chlorobenzene will be dissolved in using spin-coating methodxMixed serum is toasted after being spin-coated to the ito thin film surface, rotation
Painting rotating speed is 3000r/min, and baking temperature is 140 DEG C, and baking time 20min obtains hole injection layer；
It is toasted after the PVK mixed serums for being dissolved in chlorobenzene are spin-coated to the hole injection layer surface using spin-coating method,
A concentration of 10mg/mL of PVK, spin coating rotating speed are 5000r/min, and 130 DEG C of baking temperature, baking time 10min obtains hole transport
Layer；
CdZnSeS/ZnS nucleocapsid alloy quantum dots are dissolved in hexane solution, the quantum dot it is a concentration of
10mg/mL, the quantum dot surface contain oleic acid ligand, and green quantum is prepared in the hole transport layer surface using rotary process
Point luminescent layer；Rotary speed is 3000r/min, and baking temperature is 100 DEG C, time 6min, the diameter of CdZnSeS/ZnS quantum dots
For 11nm；
The Zn of ethyl alcohol will be dissolved in using spin-coating methodxMg1-xO nano particle mixed liquors are spin-coated to the green light quantum point and shine
It is toasted after layer surface, ZnxMg1-xA concentration of 30mg/mL of O nano particles, spin-coating time rotating speed are 2500r/min, baking
100 DEG C of temperature, time 10min obtain electron transfer layer.
(3) material of electrode is electrum, and 150nm is deposited on the electron transport layer using the method for vacuum evaporation
Electrum film, obtain initial green light quantum point diode.
(4) under vacuum, the initial green light quantum point diode that step (3) obtains is placed on hot plate and is integrally carried out
Annealing, annealing temperature are 200 DEG C, and annealing time 5min obtains green light QLED.
Embodiment 3
Feux rouges QLED devices are used to prepare in the present embodiment, wherein quantum dot light emitting layer includes green red light quantum point material,
Referred to herein as red light quantum point luminescent layer.Specifically, the structure of the feux rouges QLED devices stacks gradually from bottom to top is equipped with：Glass
Glass substrate, ito thin film (first electrode), hole injection layer, hole transmission layer, red light quantum point luminescent layer, electron transfer layer and
Metal electrode layer (second electrode).Specifically preparation process includes：
(1) take ito glass substrate, electrode pattern produced using photoetching technique, then substrate is successively respectively placed in washing lotion,
It is cleaned by ultrasonic in deionized water, three times, each ultrasonic time is 25min to ultrasound, waits after the completion of being cleaned by ultrasonic, substrate is put
It is placed in cleaning oven and is dried for standby.
(2) substrate of glass of the surface with ito thin film is handled 15 minutes using UV ozone, is then made on the surface thereof
Make light emitting functional layer.Specifically, hole injection layer, hole transmission layer, red light quantum point hair are prepared on ito thin film surface successively
Photosphere, electron transfer layer, metal electrode layer, concrete operations include：Water-soluble polyelectrolyte will be used using spin-coating method
Polystyrolsulfon acid makees the polymer P EDOT of the 3,4- ethene dioxythiophene monomers adulterated：PSS water-soluble liquids are spin-coated to described
Ito thin film is toasted behind surface, spin coating rotating speed is 2500r/min, and baking temperature is 140 DEG C, and baking time 15min is obtained
Hole injection layer；
It is toasted after the PVK mixed serums for being dissolved in chlorobenzene are spin-coated to the hole injection layer surface using spin-coating method,
A concentration of 10mg/mL of PVK, spin coating rotating speed are 4500r/min, and 150 DEG C of baking temperature, baking time 20min obtains hole transport
Layer；
CdZnSeS/ZnS nucleocapsid alloy quantum dots are dissolved in normal octane solution, the quantum dot it is a concentration of
15mg/mL, the quantum dot surface contain mercaptan ligand, and red quantum is prepared in the hole transport layer surface using rotary process
Point luminescent layer；Rotary speed is 2500r/min, and baking temperature is 100 DEG C, time 8min, the diameter of CdZnSeS/ZnS quantum dots
For 12nm；
The Zn of acetone will be dissolved in using spin-coating methodxGa1-xO nano particle mixed serums are spin-coated to the red light quantum point hair
Photosphere is toasted behind surface, ZnxMg1-xA concentration of 25mg/mL of O nano particles, spin-coating time rotating speed are 3000r/min, are dried
Roasting 100 DEG C of temperature, time 15min obtain electron transfer layer.
(3) material of electrode is silver metal, deposits the silver of 300nm on the electron transport layer using magnetron sputtering method
Film obtains initial red light quantum point diode.
(4) under air conditions, the initial green light quantum point diode that step (3) obtains is placed on hot plate and is integrally carried out
Annealing, annealing temperature are 180 DEG C, and annealing time 30min obtains feux rouges QLED.
Embodiment 4
QLED devices are used to prepare in the present embodiment, wherein quantum dot light emitting layer includes blue quanta point material, amount of green color
Specifically, the structure of the QLED devices stacks gradually from bottom to top to be equipped with for son point material and red quantum dot material：Glass base
Bottom, ito thin film (first electrode), hole injection layer, hole transmission layer, quantum dot light emitting layer, electron transfer layer and metal electrode
Layer (second electrode).Specifically preparation process includes：
(1) take ito glass substrate, electrode pattern produced using photoetching technique, then substrate is successively respectively placed in washing lotion,
It is cleaned by ultrasonic in deionized water, three times, each ultrasonic time is 30min to ultrasound, waits after the completion of being cleaned by ultrasonic, substrate is put
It is placed in cleaning oven and is dried for standby.
(2) substrate of glass of the surface with ito thin film is handled 20 minutes using UV ozone, is then made on the surface thereof
Make light emitting functional layer.Specifically, hole injection layer, hole transmission layer, quantum dot light emitting are prepared on ito thin film surface successively
Layer, electron transfer layer, metal electrode layer, concrete operations include：
The 3,4- ethylene dioxies that will make to adulterate using water-soluble polyelectrolyte polystyrolsulfon acid using spin-coating method
The polymer P EDOT of thiophene monomer：PSS water-soluble liquids are toasted after being spin-coated to the ito thin film surface, and spin coating rotating speed is
2000r/min, baking temperature are 150 DEG C, and baking time 15min obtains hole injection layer；
It is toasted after the PVK mixed liquors for being dissolved in chlorobenzene are spin-coated to the hole injection layer surface using spin-coating method, PVK
A concentration of 15mg/mL, spin coating rotating speed are 4000r/min, and 100 DEG C of baking temperature, baking time 10min obtains hole transmission layer；
CdZnSeS/ZnS nucleocapsid alloy quantum dots are dissolved in normal octane solution, a concentration of 20mg/mL, it is described
Quantum dot surface contains oleic acid ligand, using rotary process in the hole transport layer surface preparation amount point luminescent layer；Rotation speed
Degree is 2000r/min, and baking temperature is 80 DEG C, time 5min, a diameter of 10-12nm of CdZnSeS/ZnS quantum dots；
The Zn of ethyl alcohol will be dissolved in using spin-coating methodxMg1-xO nano particle mixed liquors are spin-coated to the quantum dot light emitting layer table
It is toasted behind face, ZnxMg1-xA concentration of 20mg/mL of O nano particles, spin-coating time rotating speed are 2000r/min, baking temperature
120 DEG C, time 10min obtains electron transfer layer.
(3) material of electrode is aluminum metal, deposits 150nm's on the electron transport layer using the method for vacuum evaporation
Aluminium film obtains original blue light quantum dot diode.
(4) under inert gas conditions, the initial quantum point diode that step (3) obtains is placed on hot plate and is integrally carried out
Annealing, annealing temperature are 300 DEG C, and annealing time 10min obtains QLED.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (10)
1. a kind of preparation method of light emitting diode with quantum dots, which is characterized in that including：
Substrate is provided, first electrode is prepared in the substrate surface；
Light emitting functional layer is prepared in the first electrode surface, the light emitting functional layer includes at least quantum dot light emitting layer；
Second electrode is prepared in the light emitting functional layer, obtains initial quantum point luminescent diode；
The initial quantum point luminescent diode is integrally made annealing treatment, light emitting diode with quantum dots is obtained.
2. preparation method as described in claim 1, which is characterized in that the temperature of the annealing is 50-300 DEG C, annealing
Time is 0.1-30min.
3. preparation method as claimed in claim 2, which is characterized in that the temperature of the annealing is 200-300 DEG C.
4. preparation method as described in claim 1, which is characterized in that the light emitting functional layer is included in the first electrode table
Face stacks gradually hole injection layer, hole transmission layer, quantum dot light emitting layer, electron transfer layer and the electron injecting layer of preparation；Or
The light emitting functional layer is included in the electron injecting layer, electron transfer layer, quantum that the first electrode surface stacks gradually preparation
Point luminescent layer, hole transmission layer and hole injection layer.
5. preparation method as described in claim 1, which is characterized in that the material of the first electrode include indium tin oxide,
It is one or more in indium-zinc oxide and Al-Doped ZnO；The material of the second electrode includes in aluminium, silver, gold, copper and magnesium
It is one or more.
6. preparation method as described in claim 1, which is characterized in that the material of the quantum dot light emitting layer includes red quantum
It is one or more in point material, green light quantum point material and blue light quantum point material.
7. preparation method as described in claim 1 or 6, which is characterized in that the specific preparation process of the quantum dot light emitting layer
Including：Quantum dot light emitting layer material containing surface ligand is dissolved in organic solvent and obtains mixed slurry, by the mixing slurry
Material carries out spin coating with the spin coating rotating speed of 2000-3000r/min, then toasts 4-8min in 80-120 DEG C.
8. preparation method as claimed in claim 4, which is characterized in that prepared by the way of spin coating the hole injection layer or
The material of the hole transmission layer, the hole injection layer includes PEDOT:PSS、MoOx, VOx, WOxAnd NiOxIn one kind or
A variety of, the material of the hole transmission layer includes one or more in PVK, TFB and Poly-TPD.
9. preparation method as claimed in claim 4, which is characterized in that prepared by the way of spin coating the electron injecting layer or
The material of the electron transfer layer, the electron injecting layer or the electron transfer layer include ZnO nano particle, doping ZnO receive
Rice grain and TiO2It is one or more in nano particle.
10. a kind of light emitting diode with quantum dots prepared by preparation method as described in any one of claims 1-9.
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