CN106409995A - Preparation method of QLED - Google Patents
Preparation method of QLED Download PDFInfo
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- CN106409995A CN106409995A CN201610971260.2A CN201610971260A CN106409995A CN 106409995 A CN106409995 A CN 106409995A CN 201610971260 A CN201610971260 A CN 201610971260A CN 106409995 A CN106409995 A CN 106409995A
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- qled
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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 invention provides a preparation method of a QLED. The surface of an electron transmission layer is treated before a light emitting layer is deposited on the electron transmission layer. The method comprises the following steps that oxygen plasma pretreatment or ozone treatment and ultraviolet lamp radiation treatment is carried out on the electron transmission layer, and the photo energy of the ultraviolet lamp radiation treatment is greater than the effective band gap of an electron transmission material. The preparation method of the QLED can be used to reduce the concentration of surface defects of the electron transmission layer material and remove organic residual impurities, further reduce exciton quenching caused by surface defects of the electron transmission layer, and improve the light emitting efficiency and service life of a QLED device effectively.
Description
Technical field
The invention belongs to display technology field, more particularly, to a kind of preparation method of QLED.
Background technology
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 suitable for preparing Performance Monitor part.Additionally, in terms of preparation technology angle, quantum dot light emitting material
The solution processing mode such as spin coating, printing, printing device preparation film forming can be adopted under non-vacuum condition.So, with quantum dot
The light emitting diode with quantum dots (QLED) of film preparation becomes the contenders of Display Technique of future generation.
Common, QLED device includes anode, hole injection, transport layer, luminescent layer, electric transmission, implanted layer and negative electrode.
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 for providing transportable hole from dispatch from foreign news agency road direction luminescent layer, and electron transfer layer is used for carrying
For transportable electronics.Electron-hole forms exciton in quantum dot, and exciton passes through radiation recombination output photon, and then luminous.
Nano zine oxide is commonly used electric transmission in QLED device, injection material, and its conduction level is conducive to electricity
Injection from negative electrode to quantum dot for the son, and its deeper valence-band level can play effective effect stopping hole.But how
Improve the photoelectric characteristic of nano zine oxide further, thus the device efficiency improving QLED is also an emphasis of current research.
The preparation of zinc oxide nanocrystalline (quantum dot) typically adopts the sol-gel process of low temperature.Specific surface due to quantum dot superelevation
Long-pending, equally can there is substantial amounts of surface defect state in quantum dot.These defect one side can be by the side of optics and elementary analysis
Method is characterized, and another aspect surface defect is effective excitonic luminescence quenching mechanism.Additionally, remain in building-up process is organic
Thing is coupled with negative effect to the electricity between interface.Electric transmission, the boundary defect of implanted layer will directly affect QLED device
Luminescent properties and its stability.
Content of the invention
It is an object of the invention to provide a kind of preparation method of QLED, and the QLED for preparing in the method it is intended to
Solve existing QLED and there is electron transfer layer boundary defect, the impact luminescent properties of QLED device and its problem of stability.
The present invention is achieved in that a kind of preparation method of QLED, on the electron transport layer before depositing light emitting layer, right
Described electron transfer layer is surface-treated, and comprises the following steps:Described electron transfer layer is carried out oxygen gas plasma locate in advance
Reason or ozone are processed and uviol lamp radiation treatment, and wherein, the photon energy of described uviol lamp radiation treatment is more than electric transmission
Effective band gap of material.
And, a kind of QLED, pass including the substrate being cascading, hearth electrode, electron transfer layer, luminescent layer, hole
Defeated layer, hole injection layer and top electrode, the electron transfer layer that described electron transfer layer is surface-treated for said method.
The preparation method of the QLED that the present invention provides, by carrying out oxygen-enriched atmosphere to electric transmission 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 reduced colour center,
Such as oxygen vacancy concentration), reducing conditional electronic transport layer boundary defect state, removing organic residue impurity, thus reducing minimizing table
The excitonic luminescence quenching effect that planar defect produces, improves the luminous efficiency of particularly red, the green QLED device of QLED device and makes
Use the life-span.By the QLED of the inventive method preparation, there is preferable luminous efficiency, device stability, longer service life.
Brief description
Fig. 1 is in the preparation method of QLED provided in an embodiment of the present invention, and what electron transfer layer was surface-treated shows
It is intended to;
Fig. 2 is QLED structural representation provided in an embodiment of the present invention.
Specific embodiment
In order that the technical problem to be solved in the present invention, technical scheme and beneficial effect become more apparent, 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 in order to explain
The present invention, is not intended to limit the present invention.
In conjunction with Fig. 1, embodiments provide a kind of preparation method of QLED, depositing light-emitting on electron transfer layer 3
Before layer, described electron transfer layer 3 is surface-treated, comprises the following steps:Described electron transfer layer 3 is carried out oxygen etc.
Gas ions pretreatment or ozone are processed and uviol lamp radiation treatment, and wherein, the photon energy of described uviol lamp radiation treatment is big
Effective band gap in electron transport material.
In view of in traditional QLED, electron transport material has segmental defect state, and then in electron transfer layer 3 and luminescent layer
Between formed boundary defect, directly affect luminescent properties and its stability of QLED device.In view of this, the embodiment of the present invention is led to
Cross surface treatment electron transfer layer 3 surface being carried out with oxygen-enriched atmosphere and combining ultraviolet radiation, effectively remove electric transmission material
In material such as Zinc oxide nanoparticle, part defect state (as reduced colour center, such as oxygen vacancy concentration), reduces conditional electronic transmitting layer 3
Boundary defect state (reduces the defect density of the luminous bed boundary of electron transfer layer 3-), removes organic residue impurity, thus reduce subtracting
The excitonic luminescence quenching effect that few surface defect produces, and then improve luminous efficiency and the life-span of QLED device.
Specifically, described oxygen gas plasma pretreatment or ozone process, combine uviol lamp radiation treatment, not only can subtract
The concentration of few surface defect, and ultraviolet radiant light can excite free electron in a large number, and these free electrons can fill band gap
In defect states so that it is inactivated, reduce quenching effect.Additionally, the electron transport material of sol-gal process synthesis is for example nano oxidized
Organic substance residues are usually contained, after film forming, organic substance residues generally contain higher containing in electron transfer layer 3 upper surface in zinc colloid
Amount.Pre-processed by oxygen gas plasma or ozone processes and can effectively remove electron transfer layer 3 surface with ultraviolet radiation
Organic substance residues, improve the electricity coupling between electron transfer layer 3 and luminescent layer.
It will be appreciated that the photon energy of uviol lamp radiation treatment described in the embodiment of the present invention is more than electric transmission
Effective band gap of material, the realization of guarantee the effect above, concrete photon energy is different because of electron transport material.Preferably
, the wavelength≤300nm of described uviol lamp radiation treatment.
In the embodiment of the present invention, described surface treatment can be accomplished in several ways.Wherein, when adopting oxygen plasma
Body pre-processes, it is desirable to provide vacuum environment is improving the purity of oxygen gas plasma, and then reaches preferable plasma and locate in advance
Reason effect.
As a preferred embodiment, described surface treatment is oxygen gas plasma pretreatment and ultraviolet under vacuum condition
Lamp radiation treatment, and described oxygen gas plasma pre-processes and uviol lamp radiation treatment is carried out simultaneously, process time 30-300s,
Wherein, the sputtering power of described oxygen gas plasma pretreatment is 25-250mw/cm2, oxygen flow is 5-1000sccm;Described
Power density >=the 100mw/cm of uviol lamp radiation treatment2.
In the embodiment of the present invention, carry out plasma on described electron transfer layer 3 surface, described 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, effectively can not realize plasma, if sputtering power mistake
Height, then easily etching electron transport material, so as to performance changes, causes the damage of electron transport material.In above-mentioned sputtering
Under the premise of power, likewise, described oxygen flow be difficult too high or too low, if oxygen flow is too low, the cation of plasma
Concentration is too low, and surface treatment effect is limited;If oxygen flow is too high, oxygen cannot sufficient plasma, due to wait from
Sonization directly occurs on electron transfer layer 3 surface, and therefore, the part oxygen of non-plasma still can be presented in oxygen molecule
Electron transfer layer 3 surface, and then affect surface treatment effect.During described uviol lamp radiation treatment, as power density >=100mw/
cm2When, described electron transfer layer 3 could absorb enough uv energies, and then excites substantial amounts of free electron to fill band gap
In defect states, and so that it is inactivated.
It is further preferred that described surface treatment is carried out in the prerinse equipment be provided with magnetron.This equipment helps
Carry out while the pretreatment of described oxygen gas plasma and uviol lamp radiation treatment, improve surface processing efficiency.
As a preferred embodiment, described surface treatment is oxygen gas plasma pretreatment and ultraviolet under vacuum condition
Lamp radiation treatment, wherein, described oxygen gas plasma pretreatment sets in the surface treatment being provided with independent oxonium ion generating means
Carry out in standby, the hot-wire coil power of described independent oxonium ion generating means is 10-200W, and sputtering power is 25-250mw/
cm2, oxygen flow is 5-200sccm, process time 15-150s;Power density >=the 100mw/ of described uviol lamp radiation treatment
cm2.
In the embodiment of the present invention, it is transported to electron transfer layer 3 surface again after first by oxygen plasma and carries out oxygen etc.
Gas ions pre-process, and wherein, the hot-wire coil of described independent oxonium ion generating means is used for oxygen plasma, described live wire
The power of circle is 10-200W, both can guarantee that good plasma effect, and can effectively reduce energy consumption again.Embodiment of the present invention institute
The sputtering power stating oxygen gas plasma pretreatment can be less than the sputtering power of above-described embodiment, and obtains preferable plasma
Effect.Under the premise of above-mentioned sputtering power, described oxygen flow be difficult too high or too low, if oxygen flow is too low, plasma
Cation concn too low, surface treatment effect is limited;If oxygen flow is too high, even if carrying out the stroke phase of plasma process
To longer, but oxygen it is possible to cannot sufficient plasma, part oxygen still can be transferred to electricity in the form of oxygen molecule
Sub- transmitting layer 3 surface, and then affect surface treatment effect.During described uviol lamp radiation treatment, as power density >=100mw/cm2
When, described electron transfer layer 3 could absorb enough uv energies, and then excites substantial amounts of free electron to fill in band gap
Defect states, and so that it is inactivated.
As another preferred embodiment, under conditions of or else meeting vacuum, described it is surface-treated at for ozone
Reason and uviol lamp radiation treatment.Further, described surface treatment is carried out in UV-ozone generating means.Preferably, described
Power >=the 100W of UV-ozone generating means, thus, described electron transfer layer 3 could absorb enough uv energies, and then
Excite substantial amounts of free electron to fill the defect states in band gap, and so that it is inactivated.
As a specific embodiment, taking the UV ozone generating means of 100W and zinc oxide electron transfer layer 3 as a example,
15min UV-ozone process can substantially remove the thick Nano zinc oxide film medium wavelength center of 30nm in 520nm about, half
Defect luminescence generated by light in peak width 50nm (proves that the defect density of nano zine oxide can be processed by significantly by UV-ozone
Reduce), thus improving the conversion 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, described transition group oxide includes zinc oxide, titanium dioxide, tantalum pentoxide, and wherein, described zinc oxide includes zinc oxide
Nanocrystalline (including ball shaped nano crystalline substance (i.e. quantum dot), nanometer rods), undoped zinc oxide, undoped zinc oxide-organic nano are multiple
Compound;Described titanate includes bismuth titanates, barium titanate.
Described in the embodiment of the present invention, the preparation method of electron transfer layer 3 includes solution spin coating, printing;Magnetic under vacuum condition
Cosputtering etc..Other Rotating fields of the embodiment of the present invention (include substrate 1, hearth electrode 2, luminescent layer, hole transmission layer, hole injection
Layer and top electrode) preparation, be referred to this area conventional method and realize.
And, in conjunction with Fig. 2, the embodiment of the present invention additionally provides a kind of QLED, including the substrate 1 being cascading, bottom
Electrode 2, electron transfer layer 3, luminescent layer 4, hole transmission layer 5, hole injection layer 6 and top electrode 7, described electron transfer layer 7 is
The electron transfer layer that said method is surface-treated.
The preparation method of QLED provided in an embodiment of the present invention, by carrying out oxygen-enriched atmosphere to electric transmission layer surface and tying
Close the surface treatment of ultraviolet radiation, effectively remove part defect state in electron transport material such as Zinc oxide nanoparticle and (such as drop
Low colour center, such as oxygen vacancy concentration), reducing conditional electronic transport layer boundary defect state, removing organic residue impurity, thus reducing
Reduce the excitonic luminescence quenching effect that surface defect produces, improve the luminous efficiency of particularly red, the green QLED device of QLED device
And service life.By the QLED of present invention method preparation, there is preferable luminous efficiency, device stability, longer
Service life.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of QLED is it is characterised in that on the electron transport layer before depositing light emitting layer, pass to described electronics
Defeated layer is surface-treated, and comprises the following steps:Described electron transfer layer is carried out at oxygen gas plasma pretreatment or ozone
Reason and uviol lamp radiation treatment, wherein, the photon energy of described uviol lamp radiation treatment is more than the effective of electron transport material
Band gap.
2. the preparation method of QLED as claimed in claim 1 is it is characterised in that described surface treatment is the oxygen under vacuum condition
The pretreatment of gas plasma and uviol lamp radiation treatment, and the pretreatment of described oxygen gas plasma and uviol lamp radiation treatment are simultaneously
Carry out, process time 30-300s, wherein,
The sputtering power of described oxygen gas plasma pretreatment is 25-250mw/cm2, oxygen flow is 5-1000sccm;
Power density >=the 100mw/cm of described uviol lamp radiation treatment2.
3. the preparation method of QLED as claimed in claim 2 is it is characterised in that described surface treatment is being provided with magnetron
Carry out in prerinse equipment.
4. the preparation method of QLED as claimed in claim 1 is it is characterised in that described surface treatment is the oxygen under vacuum condition
The pretreatment of gas plasma and uviol lamp radiation treatment, wherein,
Described oxygen gas plasma pretreatment is carried out in the surface processing equipment being provided with independent oxonium ion generating means, described
Individually the hot-wire coil power of oxonium ion generating means is 10-200W, and sputtering power is 25-250mw/cm2, oxygen flow is 5-
200sccm, process time 15-150s;
Power density >=the 100mw/cm of described uviol lamp radiation treatment2.
5. the preparation method of QLED as claimed in claim 1 is it is characterised in that described surface treatment is processed and ultraviolet for ozone
Lamp radiation treatment.
6. the preparation method of QLED as claimed in claim 5 is it is characterised in that described surface treatment occurs in UV-ozone
Carry out in device.
7. the preparation method of QLED as claimed in claim 6 is it is characterised in that the power of described UV-ozone generating means
≥100W.
8. the preparation method of described QLED as arbitrary in claim 1-7 was it is characterised in that described electron transport material included
Cross race's oxide, II-VI group semiconductor, titanate.
9. QLED as claimed in claim 8 preparation method it is characterised in that described transition group oxide include zinc oxide,
Titanium dioxide, tantalum pentoxide, wherein, described zinc oxide includes zinc oxide nanocrystalline, undoped zinc oxide, undoped oxidation
Zinc-organic nano compound;Described II-VI group semiconductor includes zinc sulphide, zinc selenide, zinc telluridse, cadmium sulfide;Described titanate
Including bismuth titanates, barium titanate.
10. a kind of QLED, including the substrate being cascading, hearth electrode, electron transfer layer, luminescent layer, hole transmission layer, sky
Cave implanted layer and top electrode are it is characterised in that what described electron transfer layer was surface-treated for claim 1-9 either method
Electron transfer layer.
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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 |
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