CN106409995B - The preparation method of QLED - Google Patents
The preparation method of QLED Download PDFInfo
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- CN106409995B CN106409995B CN201610971260.2A CN201610971260A CN106409995B CN 106409995 B CN106409995 B CN 106409995B CN 201610971260 A CN201610971260 A CN 201610971260A CN 106409995 B CN106409995 B CN 106409995B
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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
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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
Abstract
The present invention provides the preparation methods of QLED a kind of, on the electron transport layer before depositing light emitting layer, the electron transfer layer is surface-treated, the following steps are included: the electron transfer layer is carried out oxygen gas plasma pretreatment or ozone treatment and ultraviolet lamp radiation treatment, wherein, the photon energy of the ultraviolet lamp radiation treatment is greater than effective band gap of electron transport material.The preparation method of QLED of the present invention, concentration, the removal organic residue impurity of electron transport layer materials surface defect can be effectively reduced, exciton is quenched to reduce electron transfer layer surface defect, and then effectively improves the luminous efficiency and service life of QLED device.
Description
Technical field
The invention belongs to field of display technology more particularly to a kind of preparation methods of QLED.
Background technique
The quantum dot light emitting material of inorganic nano-crystal has the advantages that emergent light color saturation, Wavelength tunable, and photic, electric
Photoluminescence quantum yield is high, is suitble to prepare Performance Monitor part.In addition, in terms of preparation process angle, quantum dot light emitting material
The solution processing methods such as spin coating, printing, printing device preparation film forming can be used under non-vacuum condition.So with quantum dot
The light emitting diode with quantum dots (QLED) of film preparation becomes the contenders of next-generation display technology.
Common, QLED device includes anode, hole injection, transport layer, luminescent layer, electron-transport, implanted layer and cathode.
According to the relative position of electrode 1 and electrode 2, i.e. back electrode and top electrode, the structure of QLED can be divided into tradition and transoid device
Two kinds.Wherein, hole injection, transport layer are used to provide transportable hole from dispatch from foreign news agency road direction luminescent layer, and electron transfer layer is for mentioning
For transportable electronics.Electron-hole forms exciton in quantum dot, and exciton is shone by radiation recombination output photon.
Nano zine oxide is the electron-transport generallyd use in QLED device, injection material, and conduction level is conducive to electricity
Injection of the son from cathode to quantum dot, and its deeper valence-band level can play the role of effectively stopping hole.But how
The photoelectric characteristic of nano zine oxide is further increased, so that the device efficiency for improving QLED is also the emphasis studied at present.
The preparation of zinc oxide nanocrystalline (quantum dot) generally uses the sol-gel process of low temperature.Due to the specific surface of quantum dot superelevation
Product, quantum dot can equally have a large amount of surface defect state.On the one hand these defects can pass through the side of optics and elemental analysis
Method is characterized, and another aspect surface defect is effective excitonic luminescence quenching mechanism.In addition, remaining organic in synthesis process
Object has been electrically coupled negative effect between interface.Electron-transport, implanted layer boundary defect will directly affect QLED device
Luminescent properties and its stability.
Summary of the invention
The purpose of the present invention is to provide the preparation methods of QLED a kind of, and the QLED prepared in the method, it is intended to
Solving the problem of existing QLED, there are luminescent properties and its stability that electron transfer layer boundary defect influences QLED device.
The invention is realized in this way a kind of preparation method of QLED, right on the electron transport layer before depositing light emitting layer
The electron transfer layer is surface-treated, comprising the following steps: locates electron transfer layer progress oxygen gas plasma in advance
Reason or ozone treatment and ultraviolet lamp radiation treatment, wherein the photon energy of the ultraviolet lamp radiation treatment is greater than electron-transport
Effective band gap of material.
And a kind of QLED, including substrate, hearth electrode, electron transfer layer, the luminescent layer, hole biography being cascading
Defeated layer, hole injection layer and top electrode, the electron transfer layer are the electron transfer layer that the above method is surface-treated.
The preparation method of QLED provided by the invention, by carrying out oxygen-enriched atmosphere to electron-transport layer surface and combining ultraviolet
The surface treatment of light radiation, effectively remove part defect state in electron transport material such as Zinc oxide nanoparticle (as reduce colour center,
Such as oxygen vacancy concentration), conditional electronic transport layer boundary defect state is reduced, organic residue impurity is removed, to reduce reduction table
The excitonic luminescence quenching effect that planar defect generates improves the luminous efficiency of especially red, the green QLED device of QLED device and makes
Use the service life.By QLED prepared by the method for the present invention, there is preferable luminous efficiency, device stability, longer service life.
Detailed description of the invention
Fig. 1 is to show in the preparation method of QLED provided in an embodiment of the present invention what electron transfer layer was surface-treated
It is intended to；
Fig. 2 is QLED structural schematic diagram provided in an embodiment of the present invention.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
In conjunction with Fig. 1, the embodiment of the invention provides the preparation method of QLED a kind of, the depositing light-emitting on electron transfer layer 3
Before layer, the electron transfer layer 3 is surface-treated, comprising the following steps: the electron transfer layer 3 is subjected to oxygen etc.
Gas ions pretreatment or ozone treatment and ultraviolet lamp radiation treatment, wherein the photon energy of the ultraviolet lamp radiation treatment is big
In effective band gap of electron transport material.
In view of in traditional QLED, there are segmental defect states for electron transport material, and then in electron transfer layer 3 and luminescent layer
Between form boundary defect, directly affect the luminescent properties and its stability of QLED device.In view of this, the embodiment of the present invention is logical
The surface treatment that oxygen-enriched atmosphere is carried out to 3 surface of electron transfer layer and combines ultraviolet radiation is crossed, electron-transport material is effectively removed
Material such as part defect state (as reduced colour center, such as oxygen vacancy concentration) in Zinc oxide nanoparticle, reduces conditional electronic transmitting layer 3
Boundary defect state (defect density for reducing the luminous bed boundary electron transfer layer 3-), removes organic residue impurity, subtracts to reduce
The excitonic luminescence quenching effect that few surface defect generates, and then improve luminous efficiency and the service life of QLED device.
Specifically, oxygen gas plasma pretreatment or ozone treatment, in conjunction with ultraviolet lamp radiation treatment, can not only subtract
The concentration of few surface defect, and ultraviolet radiant light can largely excite free electron, and these free electrons can fill band gap
The defects of energy state make its inactivation, reduce quenching effect.In addition, the electron transport material of sol-gal process synthesis is for example nano oxidized
Organic substance residues are usually contained in zinc colloid, organic substance residues usually contain higher contain in 3 upper surface of electron transfer layer after film forming
Amount.3 surface of electron transfer layer can be effectively removed by oxygen gas plasma pretreatment or ozone treatment and ultraviolet radiation
Organic substance residues improve being electrically coupled between electron transfer layer 3 and luminescent layer.
It will be appreciated that the photon energy of ultraviolet lamp radiation treatment described in the embodiment of the present invention is greater than electron-transport
Effective band gap of material, just can guarantee the realization of said effect, and specific photon energy is different because of electron transport material.It is preferred that
, wavelength≤300nm of the ultraviolet lamp radiation treatment.
In the embodiment of the present invention, the surface treatment can be accomplished in several ways.Wherein, when using oxygen plasma
Body pretreatment, it is desirable to provide vacuum environment improves the purity of oxygen gas plasma, and then reaches preferable plasma and locate in advance
Manage effect.
As a preferred embodiment, it is described surface treatment be vacuum condition under oxygen gas plasma pretreatment and it is ultraviolet
Lamp radiation treatment, and oxygen gas plasma pretreatment and ultraviolet lamp radiation treatment carry out simultaneously, handle time 30-300s,
Wherein, the pretreated sputtering power of the oxygen gas plasma is 25-250mw/cm2, oxygen flow 5-1000sccm；It is described
Power density >=100mw/cm of ultraviolet lamp radiation treatment2。
In the embodiment of the present invention, plasma is carried out on 3 surface of electron transfer layer, the oxygen gas plasma is located in advance
The sputtering power of reason is unsuitable too high or too low, if sputtering power is too low, plasma cannot be effectively realized, if sputtering power mistake
Height is then easy etching electron transport material, so that its performance is changed, cause the damage of electron transport material.In above-mentioned sputtering
Under the premise of power, likewise, the oxygen flow is not easy too high or too low, the cation of plasma if oxygen flow is too low
Concentration is too low, and surface treatment effect is limited；If oxygen flow is excessively high, oxygen cannot get sufficient plasma, due to it is equal from
Sonization directly occurs on 3 surface of electron transfer layer, and therefore, the part oxygen of non-plasma still can exist in the form of oxygen molecule
3 surface of electron transfer layer, and then influence surface treatment effect.When the ultraviolet lamp radiation treatment, as power density >=100mw/
cm2When, the electron transfer layer 3 could absorb enough uv energies, and then excite a large amount of free electron to fill band gap
The defects of energy state, and make its inactivation.
It is further preferred that the surface treatment carries out in the prerinse equipment for being provided with magnetron.The equipment helps
It is carried out while oxygen gas plasma pretreatment and ultraviolet lamp radiation treatment, improves surface processing efficiency.
As a preferred embodiment, it is described surface treatment be vacuum condition under oxygen gas plasma pretreatment and it is ultraviolet
Lamp radiation treatment, wherein the oxygen gas plasma pretreatment is set in the surface treatment for being provided with independent oxonium ion generating device
Standby middle progress, the hot-wire coil power of the independent oxonium ion generating device are 10-200W, sputtering power 25-250mw/
cm2, oxygen flow 5-200sccm, processing time 15-150s；Power density >=100mw/ of the ultraviolet lamp radiation treatment
cm2。
In the embodiment of the present invention, oxygen etc. is carried out by will first be transported to again 3 surface of electron transfer layer after oxygen plasma
Gas ions pretreatment, wherein the hot-wire coil of the independent oxonium ion generating device is used for oxygen plasma, the live wire
The power of circle is 10-200W, not only can guarantee good plasma effect, but also can effectively reduce energy consumption.Institute of the embodiment of the present invention
The sputtering power of above-described embodiment can be lower than by stating the pretreated sputtering power of oxygen gas plasma, and obtain preferable plasma
Effect.Under the premise of above-mentioned sputtering power, the oxygen flow is not easy too high or too low, the plasma if oxygen flow is too low
Cation concn it is too low, surface treatment effect is limited；If oxygen flow is excessively high, even if carrying out the stroke phase of plasma processing
To longer, but oxygen, it is possible to cannot get sufficient plasma, part oxygen still can be transferred to electricity in the form of oxygen molecule
Sub- transmitting layer 3 surface, and then influence surface treatment effect.When the ultraviolet lamp radiation treatment, as power density >=100mw/cm2
When, the electron transfer layer 3 could absorb enough uv energies, and then excite a large amount of free electron to fill in band gap
Defect states, and make its inactivation.
It as another preferred embodiment, is or else able to satisfy under conditions of vacuum, the surface treatment is at ozone
Reason and ultraviolet lamp radiation treatment.Further, the surface treatment carries out in UV-ozone generating device.Preferably, described
Power >=100W of UV-ozone generating device, the electron transfer layer 3 could absorb enough uv energies as a result, in turn
A large amount of free electron is excited to fill the defects of band gap energy state, and makes its inactivation.
As a specific embodiment, by taking the UV ozone generating device of 100W and zinc oxide electron transfer layer 3 as an example,
The processing of 15min UV-ozone can remove the Nano zinc oxide film medium wavelength center of 30nm thickness in 520nm or so, half substantially
Defect luminescence generated by light on peak width 50nm (proves that the defect density of nano zine oxide can be handled by UV-ozone by significantly
Reduce), to improve the transfer efficiency of photovoltaic device.
Electron transport material described in the embodiment of the present invention includes but is not limited to transition group oxide, II-VI group semiconductor, titanium
Hydrochlorate, the transition group oxide include zinc oxide, titanium dioxide, tantalum pentoxide, wherein the zinc oxide includes zinc oxide
Nanocrystalline (including ball shaped nano brilliant (i.e. quantum dot), nanometer rods), undoped zinc oxide, undoped zinc oxide-organic nano are multiple
Close object；The titanate includes bismuth titanates, barium titanate.
The preparation method of electron transfer layer 3 described in the embodiment of the present invention includes solution spin coating, printing；Magnetic under vacuum condition
Cosputtering etc..Other layer of structure of the embodiment of the present invention (including substrate 1, hearth electrode 2, luminescent layer, hole transmission layer, hole injection
Layer and top electrode) preparation, be referred to conventional method in that art realization.
And in conjunction with Fig. 2, the embodiment of the invention also provides a kind of QLED, including be cascading substrate 1, bottom
Electrode 2, electron transfer layer 3, luminescent layer 4, hole transmission layer 5, hole injection layer 6 and top electrode 7, the electron transfer layer 7 are
The electron transfer layer that the above method is surface-treated.
The preparation method of QLED provided in an embodiment of the present invention, by carrying out oxygen-enriched atmosphere to electron-transport layer surface and tying
The surface treatment for closing ultraviolet radiation effectively removes part defect state in electron transport material such as Zinc oxide nanoparticle (as dropped
Low colour center, such as oxygen vacancy concentration), conditional electronic transport layer boundary defect state is reduced, organic residue impurity is removed, to reduce
The excitonic luminescence quenching effect that surface defect generates is reduced, the luminous efficiency of especially red, the green QLED device of QLED device is improved
And service life.By QLED prepared by present invention method, there is preferable luminous efficiency, device stability, it is longer
Service life.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of preparation method of QLED, which is characterized in that on the electron transport layer before depositing light emitting layer, passed to the electronics
Defeated layer is surface-treated, comprising the following steps: carries out the electron transfer layer at oxygen gas plasma pretreatment or ozone
Continue to keep oxygen-enriched atmosphere after reason, carries out ultraviolet lamp radiation treatment, wherein the photon energy of the ultraviolet lamp radiation treatment is greater than
Effective band gap of electron transport material.
2. the preparation method of QLED as described in claim 1, which is characterized in that the surface treatment is the oxygen under vacuum condition
The pretreatment of gas plasma and ultraviolet lamp radiation treatment, and oxygen gas plasma pretreatment and ultraviolet lamp radiation treatment are simultaneously
It carries out, handles time 30-300s, wherein
The pretreated sputtering power of oxygen gas plasma is 25-250mw/cm2, oxygen flow 5-1000sccm；
Power density >=100mw/cm of the ultraviolet lamp radiation treatment2。
3. the preparation method of QLED as claimed in claim 2, which is characterized in that the surface treatment is being provided with magnetron
It is carried out in prerinse equipment.
4. the preparation method of QLED as described in claim 1, which is characterized in that the surface treatment is the oxygen under vacuum condition
The pretreatment of gas plasma and ultraviolet lamp radiation treatment, wherein
The oxygen gas plasma pretreatment carries out in the surface processing equipment for being provided with independent oxonium ion generating device, described
The hot-wire coil power of independent oxonium ion generating device is 10-200W, sputtering power 25-250mw/cm2, oxygen flow 5-
200sccm handles time 15-150s；
Power density >=100mw/cm of the ultraviolet lamp radiation treatment2。
5. the preparation method of QLED as described in claim 1, which is characterized in that the surface treatment is ozone treatment and ultraviolet
Lamp radiation treatment.
6. the preparation method of QLED as claimed in claim 5, which is characterized in that the surface treatment occurs in UV-ozone
It is carried out in device.
7. the preparation method of QLED as claimed in claim 6, which is characterized in that the power of the UV-ozone generating device
≥100W。
8. the preparation method of QLED as claimed in claim 1, which is characterized in that the electron transport material included
Cross race's oxide, II-VI group semiconductor, titanate.
9. the preparation method of QLED as claimed in claim 8, which is characterized in that the transition group oxide include zinc oxide,
Titanium dioxide, tantalum pentoxide, wherein the zinc oxide includes zinc oxide nanocrystalline, undoped zinc oxide, undoped oxidation
Zinc-organic nano compound；The II-VI group semiconductor includes zinc sulphide, zinc selenide, zinc telluridse, cadmium sulfide；The titanate
Including bismuth titanates, barium titanate.
10. a kind of QLED, including substrate, hearth electrode, electron transfer layer, luminescent layer, hole transmission layer, the sky being cascading
Cave implanted layer and top electrode, which is characterized in that the electron transfer layer is what claim 1-9 either method was surface-treated
Electron transfer layer.
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| CN109994622B (en) * | 2017-12-29 | 2020-06-23 | Tcl科技集团股份有限公司 | QLED device |
| CN110739404B (en) * | 2018-07-18 | 2021-04-02 | Tcl科技集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
| CN108987258A (en) * | 2018-07-19 | 2018-12-11 | 京东方科技集团股份有限公司 | The preparation method and device of oxide semiconductor layer |
| CN111384304B (en) * | 2018-12-29 | 2021-06-29 | Tcl科技集团股份有限公司 | Post-processing method of quantum dot light-emitting diode |
| CN111384308B (en) * | 2018-12-29 | 2021-05-28 | Tcl科技集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| CN110277498B (en) * | 2019-06-10 | 2022-08-02 | 储天新能源科技（长春）有限公司 | Preparation method of perovskite battery |
| US20230157049A1 (en) * | 2019-11-14 | 2023-05-18 | Beijing Boe Technology Development Co., Ltd. | Quantum dots light emitting diode, display apparatus, and method of fabricating quantum dots light emitting diode |
| CN112331784B (en) * | 2019-12-17 | 2023-01-31 | 广东聚华印刷显示技术有限公司 | Film and use thereof |
| CN111725440B (en) * | 2020-07-01 | 2022-12-09 | 合肥福纳科技有限公司 | Metal oxide nanoparticle, processing method thereof and QLED device |
| US11968852B2 (en) * | 2020-09-21 | 2024-04-23 | Boe Technology Group Co., Ltd. | Light-emitting device and method of manufacturing the same, light-emitting substrate and method of manufacturing the same, and light-emitting apparatus |
| CN112349856B (en) * | 2020-11-30 | 2022-05-20 | 河南工程学院 | Quantum dot light-emitting diode based on corona discharge interface modification and preparation method thereof |
| CN114695816A (en) * | 2020-12-30 | 2022-07-01 | Tcl科技集团股份有限公司 | Quantum dot light-emitting diode device and preparation method thereof |
| CN112802974A (en) * | 2020-12-30 | 2021-05-14 | 广东聚华印刷显示技术有限公司 | Electronic device structure, preparation method thereof, light emitting diode and display device |
| CN114695708A (en) * | 2020-12-31 | 2022-07-01 | Tcl科技集团股份有限公司 | Light emitting device and method of manufacturing the same |
| CN116193939A (en) * | 2021-11-26 | 2023-05-30 | Tcl科技集团股份有限公司 | Film treatment method |
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