CN110416423A - QLED device and preparation method thereof - Google Patents
QLED device and preparation method thereof Download PDFInfo
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- 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 relates to a kind of QLED devices and preparation method thereof, wherein QLED device includes luminescent layer, includes quanta point material and organic nano line in the luminescent layer, and the organic nano line is uniformly distributed in the quanta point material.The QLED device can be improved cavity transmission ability, reduce electronic current by the Uniform Doped organic nano line in luminescent layer, so that the injection and transmission of equilbrium carrier, promote device performance.
Description
Technical field
The present invention relates to Light-Emitting Diode technical fields, more particularly to a kind of QLED device and preparation method thereof.
Background technique
Light emitting diode with quantum dots (Quantum dot light-emitting diode, QLED) is due to full with color
With the advantages that degree is high, luminescent color is adjustable, photoluminescence efficiency is high and solution processable (spin coating, inkjet printing), in big face
Product display aspect has wealthy application prospect and gets more and more people's extensive concerning.
In the synthesis process, surface can make its photostability there are many dangling bonds and surface defect state to quanta point material
Difference.Therefore, the quanta point material applied in luminescent device generally by the outer layer growing broad-band gap in quantum dot core nothing
Machine semiconductor shell, or be passivated in organic ligands such as quantum dot surface addition surfactants, improve its quantum dot
Efficiency and photostability.
Currently, the semiconductor-quantum-point of the II-VI group based on Cd is in luminous efficiency, excitation purity and luminescent spectrum adjustability etc.
The performance of aspect is the most prominent, the relevant electroluminescent device research of the materials such as such as CdSe/ZnS, CdSe/CdS/ZnS
Also at most.But the electroluminescent efficiency of these devices and the practical also biggish distance of device lifetime distance, therefore,
The device of the semiconductor-quantum-point of II-VI group based on Cd has yet to be improved and developed.
Summary of the invention
Based on this, it is necessary to provide a kind of QLED device, can be improved hole current, to improve the performance of QLED device.
Present invention applicant's discovery, in current QLED device, electronics majority is carrier, and the performance of device depends on
The injection in hole and transmission situation, due to HOMO highest occupied molecular orbital (HOMO) energy level of quanta point material it is mostly deep (up to 6eV~
7eV), excessive hole injection barrier causes the injection of device inside carrier and transmission uneven, therefore, improves hole current
It is the effective ways for promoting device performance.
A kind of QLED device, which is characterized in that include quanta point material including luminescent layer, in the luminescent layer and organic receive
Rice noodles, the organic nano line are distributed in the quanta point material.
In one of the embodiments, in the luminescent layer, the concentration of the organic nano line is 1wt%~7wt%.
It is appreciated that the concentration of organic nano line is that 1wt%~7wt% refers to that the quality of organic nano line accounts for luminescent layer gross mass
1%~7%.
The material of the organic nano line is the nano wire that benzothiophene derivative is formed in one of the embodiments,.
Further, the material of the benzothiophene derivative is selected from formula (1), formula (2), formula (3), formula (4) and formula (5) institute
Show at least one of the compound of structure:
Wherein, R1And R2For-n-C12H25, R3、R4And R5It is independently selected from-n-C5H11Group and-n-C12H25Group
One of.
In one of the embodiments, the luminescent layer with a thickness of 20nm~40nm, the partial size of the organic nano line
Less than 10nm.It is appreciated that the partial size of organic nano line refers to the trans D of organic nano line.
The QLED device includes the substrate set gradually, anode, hole injection layer, institute in one of the embodiments,
State luminescent layer, electron transfer layer and cathode.
LUMO (lowest unoccupied molecular orbital) energy level of organic nano line and institute in the luminescent layer in one of the embodiments,
The lumo energy difference for stating electron transfer layer is more than or equal to 1.5eV.
The inventive concept total as one, another object of the present invention are a kind of preparation method of QLED device, including with
Lower step:
Form luminescent layer;
The step of forming the luminescent layer includes: depositing light emitting layer solution, and drying and forming-film is to get arriving the luminescent layer;
It include quanta point material and organic material in the luminescent layer solution, the organic material is in the luminescent layer solution
Organic nano line is self-assembly of during drying and forming-film, the organic nano line is distributed in the quanta point material.
In one of the embodiments, further include the preparation step of the luminescent layer solution:
The organic material is dissolved in organic solvent, mixed solution is obtained, the organic material is selected from benzothiophene
Derivative;
The quanta point material is dissolved in organic solvent, quantum dot ink is obtained;
The mixed solution is blended with the quantum dot ink, obtains the luminescent layer solution.
In one of the embodiments, when the depositing light emitting layer solution, the temperature of the luminescent layer solution is 40 DEG C ± 2
℃。
Beneficial effects of the present invention:
1, above-mentioned QLED device can be improved cavity transmission ability, reduce by adulterating organic nano wire in luminescent layer
Electronic current, so that the injection and transmission of equilbrium carrier, promote device performance.
2, select forming material of the benzothiophene derivative as organic nano line, and control doping concentration 1wt%~
7wt%, deposition when luminescent layer solution temperature be 40 DEG C ± 2 DEG C, using solvent volatilize induction benzothiophene derivative molecule from
Assembling and growth form nano wire, and a step is realized the self-organizing growth of organic nano line and is uniformly distributed.
3, formula (1)~formula (5) compound is the benzothiophene derivative that height replaces, and contains multiple S (sulphur) atom,
Aspectant accumulation is easily occurred by the pi-conjugated interaction of π-, self assembly generates nano wire, makes luminescent layer sky with higher
Cave transmittability, while it can also be effectively reduced electronic current, achieve the effect that promote device performance.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of an embodiment of the present invention QLED device;
Fig. 2 is the level structure schematic diagram of one embodiment of the invention QLED device.
Specific embodiment
To facilitate the understanding of the present invention, below will to invention is more fully described, and give it is of the invention compared with
Good embodiment.But the invention can be realized in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
As shown in Figure 1, the QLED device 10 of an embodiment of the present invention, successively includes substrate 110, anode from bottom to top
120, hole injection layer 130, luminescent layer 140, electron transfer layer 150 and cathode 160;It include quanta point material in luminescent layer 140
With organic nano line, organic nano line is uniformly distributed in quanta point material.
Cavity transmission ability, drop can be improved in Uniform Doped organic nano line in the luminescent layer 140 of above-mentioned QLED device 10
Low electronic current, so that the injection and transmission of equilbrium carrier, promote device performance.
Into one, organic nano line is hole-transporting type organic nano line.
In one embodiment, the concentration of organic nano line is 1wt%~7wt%.So, on the one hand, organic nano line can
To be uniformly distributed in organic luminous layer 140 by self-assembled growth, on the other hand can guarantee to be distributed in luminescent layer 140
The size of organic nano line is suitable for being not exposed to the surface of luminous layer film, avoids being formed around organic nano line and not send out
The blackspot of light influences the performance of device.
In one embodiment, organic nano line is the nano wire that benzothiophene derivative is formed.
Further, benzothiophene derivative is selected from least one in the compound of the structure as shown in following formula (1)~formula (5)
Kind:
Wherein, R1And R2For-n-C12H25, R3、R4And R5It is independently selected from-n-C5H11Group and-n-C12H25Group
One of.
It is appreciated that π-π interaction is the most important intermolecular non-covalent bond active force of self assembly between organic molecule, it is main
Occur between aromatic rings, energy is about 0-50Kj/mol.Contain multiple S atoms in the molecule of above compound, it is easily logical
It crosses π-π to interact to form one-dimensional nanostructure, is self-assembled into nano wire, cavity transmission ability with higher;Simultaneously also
Electronic current can be effectively reduced.
In one embodiment, luminescent layer 140 with a thickness of 20nm~40nm, the partial size of organic nano line is less than 10nm.
In one embodiment, the lumo energy of organic nano line and the lumo energy of electron transfer layer are poor in luminescent layer 140
More than or equal to 1.5eV.
An embodiment of the present invention provides a kind of preparation method of QLED device, comprising the following steps:
It is stacked gradually on substrate 110 and prepares anode 120, hole injection layer 130, luminescent layer 140, electron transfer layer 150
With cathode 160;
Wherein, the preparation step of luminescent layer 140 includes: that luminescent layer solution is deposited on hole injection layer 130, is dried to
Film obtains luminescent layer 140;
It include quanta point material and organic material, mistake of the organic material in luminescent layer solution drying and forming-film in luminescent layer solution
Journey kind is self-assembly of organic nano line, and after drying and forming-film, organic nano line is uniformly distributed in quanta point material.
Specifically, the above-mentioned deposition method of the present invention can be, but not limited to spin-coating method, knife coating, print process, spray coating method, strip
One of rubbing method is a variety of.
In one embodiment, the preparation step of luminescent layer solution includes:
Organic material is dissolved in organic solvent, mixed solution is obtained, organic material is selected from benzothiophene derivative;
Quanta point material is dissolved in organic solvent, quantum dot ink is obtained;
Mixed solution is blended with quantum dot ink, obtains luminescent layer solution.
In one embodiment, quanta point material can be selected from but not limited to the semiconductor-quantum-point of the II-VI group of Cd, such as
CdSe/ZnS and CdSe/CdS/ZnS.It is appreciated that the quanta point material is soluble in toluene, dimethylbenzene, chlorobenzene, chloroform equal solvent
In.
In one embodiment, benzothiophene derivative is selected from least one in the compound of previously described formula (1)~formula (5)
Kind.It is appreciated that formula (1)~formula (5) compound be soluble in heat organic solvent, such as toluene, dimethylbenzene, chlorobenzene, chloroform, four
Hydrogen furans etc., and nano wire is easily self-assembly of by π-π interaction.
In one embodiment, the doping concentration of benzothiophene derivative is 1wt%~7wt% in luminescent layer solution.It can be with
Understand, in luminescent layer is molten, the quality of benzothiophene derivative accounts for the 1% of benzothiophene derivative and quanta point material gross mass
~7%.In this way, the doping concentration of benzothiophene derivative maintains 1wt%~7wt%, on the one hand, benzothiophene derivative can
It to form nano wire by self-assembled growth, and is uniformly distributed in quanta point material, on the other hand can guarantee the amount of being distributed in
The size of organic nano line in son point material is suitable for being not exposed to the surface of 140 film of luminescent layer, avoiding in organic nano
Non-luminous blackspot is formed around line, influences the performance of device.
Inventor in experiments it is found that, when the doping ratio of benzothiophene derivative be lower than 1wt% when, it is intermolecular be difficult from
Assembling forms organic nano wire;And when doping ratio is higher than 7wt%, organic nano that benzothiophene derivative is self-assembly of
Line partial size is larger, is easy to be exposed to the surface of luminous layer film, and in device work, these are exposed to the organic of film surface and receive
It will form non-luminous blackspot around rice noodles, to influence device performance.
In one embodiment, when depositing light emitting layer solution, the temperature of luminescent layer solution is 40 DEG C ± 2 DEG C.In this way, can protect
The organic nano line that benzothiophene derivative molecular self-assembling generates is demonstrate,proved, and is uniformly distributed in quanta point material.
Specifically, by taking spin-coating method as an example, the step of preparing luminescent layer, is as follows:
In organic solvent by quanta point material dissolution, the quantum dot ink that concentration is 15mg/mL~25mg/mL is prepared
Water;
Benzothiophene derivative is dissolved in 40 DEG C ± 2 DEG C of organic solvent, obtaining concentration is 10mg/mL~20mg/
The benzothiophene derivative solution of mL;
It is 1wt%~7wt% according to doping concentration, a certain amount of benzothiophene derivative solution and quantum dot ink is mixed
It is even, obtain luminescent layer solution;
Then luminescent layer solution is spin-coated on hole injection layer 130, then heat drying forms a film, as luminescent layer 140;
It needs to keep luminescent layer solution temperature at 40 DEG C or so in spin coating process.
In this way, in spin coating process, as the volatilization of organic solvent reduces the cooling with solution, benzothiophene derivative
The accumulation on generating surface opposite is uniformly distributed in be self-assembled into nano wire under π-π interaction force between molecule and molecule
In luminescent layer.
The following are specific embodiments
Embodiment 1:
(1) base-plate cleaning: the glass substrate with 150nm ITO (tin indium oxide) is passed through into deionized water, acetone, is washed
Liquid, deionized water and the ultrasonic cleaning of five step of isopropanol, each 10~15 minutes of every step.It is placed in vacuum drying oven and dries after cleaning up
It does spare.
(2) substrate P lasma is handled: the ITO of drying is carried out oxygen Plasma processing, time 4min.
(3) prepared by hole injection layer: within Plasma treated half an hour, in one layer of about 40nm of the surface ITO spin coating
Thick PEDOT:PSS (poly- (3,4-ethylene dioxythiophene)-polystyrolsulfon acid), then under the conditions of 120 DEG C, in air plus
It is heat-treated 20min.
(4) prepared by luminescent layer:
Using toluene as organic solvent, compound concentration is the quantum dot ink and formula (1) compound solution of 15mg/mL respectively,
Then it is 2wt% according to doping concentration, the two is blended, CdSe/ZnS is obtained: the luminescent layer solution of formula (1) compound;
The luminescent layer CdSe/ZnS of one layer of 25nm thickness of face spin coating on the hole transport layer: formula (1) compound (luminescent layer
CdSe/ZnS: formula (1) compound refers to that the material of luminescent layer is made of CdSe/ZnS and formula (1) compound), in 80 DEG C of conditions
Under in N2Middle heating 10min.
(5) prepared by electron transfer layer: spin coating forms the ZnO film of one layer of about 30nm thickness on the light-emitting layer, in 100 DEG C of conditions
Under, in N2Middle heating 10min.
(6) prepared by electrode: the Al of one layer of 12 0nm thickness is finally deposited as electrode, wherein evaporation rate control is
Vacuum degree is 2 × 10-4Pa。
As shown in Fig. 2, the level structure schematic diagram of the QLED device for embodiment 1, according to luminescent layer and organic nano
From the point of view of energy level, due to the presence of organic nano line, the lumo energy of ZnO film layer (electron transfer layer) and organic nano line
Lumo energy difference is 2eV, and the electronic current reached in quantum dot light emitting layer can be effectively reduced in the presence of this potential barrier, thus flat
Weighing apparatus part internal electron and hole current are conducive to the raising of device performance.
Embodiment 2:
(1) base-plate cleaning: deionized water, acetone, washing lotion, deionized water will be passed through with the glass substrate of 150nm ITO
It is cleaned by ultrasonic with five step of isopropanol, each 10~15 minutes of every step.It is placed in vacuum drying oven and is dried for standby after cleaning up.
(2) substrate P lasma is handled: the ITO of drying is carried out oxygen Plasma processing, time 4min.
(3) prepared by hole injection layer: within Plasma treated half an hour, in one layer of about 40nm of the surface ITO spin coating
Thick PEDOT:PSS heats 20min then in 120 DEG C in air;
(4) prepared by luminescent layer: using toluene as organic solvent, compound concentration is the quantum dot ink and formula of 15mg/mL respectively
(2) then compound solution is 2wt% according to doping concentration, the two is blended, CdSe/ZnS is obtained: the hair of formula (2) compound
Photosphere solution;
The luminescent layer CdSe/ZnS of one layer of 25nm thickness of face spin coating on the hole transport layer: formula (2) compound, in 80 DEG C of conditions
Under in N2Middle heating 10min.
(5) prepared by electron transfer layer: spin coating forms the ZnO film of one layer of about 30nm thickness on the light-emitting layer, in 100 DEG C of conditions
Under in N2Middle heating 10min.
(6) prepared by electrode: the Al of one layer of 120nm thickness is finally deposited as electrode, wherein evaporation rate control isVery
Reciprocal of duty cycle is 2 × 10-4Pa。
Embodiment 3:
(1) base-plate cleaning: deionized water, acetone, washing lotion, deionized water will be passed through with the glass substrate of 150nm ITO
It is cleaned by ultrasonic with five step of isopropanol, each 10~15 minutes of every step.It is placed in vacuum drying oven and is dried for standby after cleaning up;
(2) substrate P lasma is handled: the ITO of drying is carried out oxygen Plasma processing, time 4min;
(3) prepared by hole injection layer: within Plasma treated half an hour, in one layer of about 40nm of the surface ITO spin coating
Then thick PEDOT:PSS heats 120 DEG C of processing 20min in air;
(4) prepared by luminescent layer: using toluene as organic solvent, compound concentration is the quantum dot ink and formula of 15mg/mL respectively
(4) then compound solution is 1.5wt% according to doping concentration, the two is blended, CdSe/ZnS is obtained: formula (4) compound
Luminescent layer solution;
The luminescent layer CdSe/ZnS: 4 compound of formula of one layer of 25nm thickness of face spin coating on the hole transport layer, under the conditions of 80 DEG C
In N2Middle heating 10min.
(5) prepared by electron transfer layer: spin coating forms the ZnO film of one layer of about 30nm thickness on the light-emitting layer, in 100 DEG C of conditions
Under, in N2Middle heating 10min.
(6) prepared by electrode: the Al of one layer of 120nm thickness is finally deposited as electrode, wherein evaporation rate control isVery
Reciprocal of duty cycle is 2 × 10-4Pa。
Embodiment 4:
(1) base-plate cleaning: deionized water, acetone, washing lotion, deionized water will be passed through with the glass substrate of 150nm ITO
It is cleaned by ultrasonic with five step of isopropanol, each 10~15 minutes of every step.It is placed in vacuum drying oven and is dried for standby after cleaning up;
(2) substrate P lasma is handled: the ITO of drying is carried out oxygen Plasma processing, time 4min;
(3) prepared by hole injection layer: within Plasma treated half an hour, in one layer of about 40nm of the surface ITO spin coating
Then thick PEDOT:PSS heats 120 DEG C of processing 20min in air;
(4) prepared by luminescent layer: using toluene as organic solvent, compound concentration is the quantum dot ink and formula of 15mg/mL respectively
(3) then compound solution is 2wt% according to doping concentration, the two is blended, CdSe/ZnS is obtained: the hair of formula (3) compound
Photosphere solution;
The luminescent layer CdSe/ZnS of one layer of 25nm thickness of face spin coating on the hole transport layer: formula (3) compound, in 80 DEG C of conditions
Under in N2Middle heating 10min.
(5) prepared by electron transfer layer: spin coating forms the ZnO film of one layer of about 30nm thickness on the light-emitting layer, in 100 DEG C of conditions
Under, in N2Middle heating 10min.
(6) prepared by electrode: the Al of one layer of 120nm thickness is finally deposited as electrode, wherein evaporation rate control isVery
Reciprocal of duty cycle is 2 × 10-4Pa。
Embodiment 5:
(1) base-plate cleaning: deionized water, acetone, washing lotion, deionized water will be passed through with the glass substrate of 150nm ITO
It is cleaned by ultrasonic with five step of isopropanol, each 10~15 minutes of every step.It is placed in vacuum drying oven and is dried for standby after cleaning up;
(2) substrate P lasma is handled: the ITO of drying is carried out oxygen Plasma processing, time 4min;
(3) prepared by hole injection layer: within Plasma treated half an hour, in one layer of about 40nm of the surface ITO spin coating
Then thick PEDOT:PSS heats 120 DEG C of processing 20min in air;
(4) prepared by luminescent layer: using toluene as organic solvent, compound concentration is the quantum dot ink and formula of 15mg/mL respectively
(5) then compound solution is 2.5wt% according to doping concentration, the two is blended, CdSe/ZnS is obtained: formula (5) compound
Luminescent layer solution;
The luminescent layer CdSe/ZnS of one layer of 25nm thickness of face spin coating on the hole transport layer: formula (5) compound, in 80 DEG C of conditions
Under in N2Middle heating 10min.
(5) prepared by electron transfer layer: spin coating forms the ZnO film of one layer of about 30nm thickness on the light-emitting layer, in 100 DEG C of conditions
Under, in N2Middle heating 10min.
(6) prepared by electrode: the Al of one layer of 120nm thickness is finally deposited as electrode, wherein evaporation rate control isVery
Reciprocal of duty cycle 2 × 10-4Pa。
Comparative example 1
Comparative example 1 is substantially the same manner as Example 1, the difference is that, there is no the compound of formula (1) in luminescent layer solution,
Non-impurity-doped nano wire in the luminescent layer of gained QLED device.
Comparative example 2
Comparative example 2 is substantially the same manner as Example 1, the difference is that, the doping concentration of nano wire raw material is different, specifically
Doping concentration for the compound of luminescent layer solution Chinese style (1) is 0.5wt%.
Comparative example 3
Comparative example 3 is substantially the same manner as Example 1, the difference is that, the doping concentration of nano wire raw material is different, specifically
Compound doped concentration for luminescent layer solution Chinese style (1) is 9wt%.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of QLED device, which is characterized in that include quanta point material and organic nano in the luminescent layer including luminescent layer
Line, the organic nano line are distributed in the quanta point material.
2. QLED device according to claim 1, which is characterized in that in the luminescent layer, the organic nano line
Concentration is 1wt%~7wt%.
3. QLED device according to claim 1, which is characterized in that the organic nano line is benzothiophene derivative shape
At nano wire.
4. QLED device according to claim 3, which is characterized in that the benzothiophene derivative is selected from formula (1), formula
(2), at least one of the compound of structure shown in formula (3), formula (4) and formula (5):
Wherein, R1And R2For n-C12H25, R3、R4And R5It is independently selected from-n-C5H11Group and n-C12H25One in group
Kind.
5. QLED device according to claim 4, which is characterized in that the luminescent layer with a thickness of 20nm~40nm, institute
The partial size for stating organic nano line is less than 10nm.
6. any QLED device according to claim 1~5, which is characterized in that the QLED device includes setting gradually
Substrate, anode, hole injection layer, the luminescent layer, electron transfer layer and cathode.
7. QLED device according to claim 6, which is characterized in that the lumo energy of organic nano line in the luminescent layer
It is more than or equal to 1.5eV with the lumo energy difference of the electron transfer layer.
8. a kind of preparation method of QLED device, which comprises the following steps:
Form luminescent layer;
The step of forming the luminescent layer includes: depositing light emitting layer solution, and drying and forming-film is to get arriving the luminescent layer;
It include quanta point material and organic material in the luminescent layer solution, the organic material is dry in the luminescent layer solution
Organic nano line is self-assembly of during film forming, the organic nano line is distributed in the quanta point material.
9. the preparation method of QLED device according to claim 8, which is characterized in that further include the luminescent layer solution
Preparation step:
The organic material is dissolved in organic solvent, mixed solution is obtained, the organic material is derivative selected from benzothiophene
Object;
The quanta point material is dissolved in organic solvent, quantum dot ink is obtained;
The mixed solution is blended with the quantum dot ink, obtains the luminescent layer solution.
10. the preparation method of QLED device according to claim 8 or claim 9, which is characterized in that the depositing light emitting layer solution
When, the temperature of the luminescent layer solution is 40 DEG C ± 2 DEG C.
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