CN111864120A - QLED and manufacturing method thereof and method for improving light-emitting rate of QLED - Google Patents
QLED and manufacturing method thereof and method for improving light-emitting rate of QLED Download PDFInfo
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- H10K50/00—Organic light-emitting devices
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- 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
Abstract
A QLED and a method for manufacturing the same and improving the light-emitting rate of the QLED belong to the field of light-emitting diodes. The method for improving the light extraction rate of the QLED comprises the step of manufacturing a diffraction structure consisting of a nano-pillar array on the outer surface of a transparent substrate of the QLED. The light extraction rate of the device can be improved by forming the above diffraction structure in the QLED.
Description
Technical Field
The application relates to the field of light emitting diodes, in particular to a QLED and a method for manufacturing the same and improving the light extraction rate of the QLED.
Background
Due to the advantages of high light color purity degree centigrade, high luminous quantum efficiency, adjustable luminous color, long service life and the like, the quantum dot light emitting diode (QLED) has wide application prospect in the fields of illumination and flat panel display.
However, the conventional QLED device at present has a problem of low light extraction efficiency. Theoretically, the existing conventional QLED device has only about 25% of light energy exiting out of the QLED device, and the rest of light is confined in the device in a surface plasmon mode and a waveguide mode and cannot be guided out.
Therefore, how to improve the light extraction efficiency has become a problem to be solved urgently in the research and application field of the QLED.
Currently, the study on the light extraction efficiency of QLED devices can be divided into two directions:
one direction is to reasonably design the internal structure of the QLED device;
and the other direction is to design the external light-emitting surface of the QLED device.
The design of the external light emitting surface of the QLED device is to reduce total reflection at the light emitting surface and the air interface. At present, three schemes of directly roughening the light-emitting surface of the device, introducing a surface antireflection film and adding a surface micro thin film lens are mainly adopted for designing the external light-emitting surface of the QLED device.
However, practice shows that the three schemes have respective defects, such as high cost and difficulty in application to the manufacture of large-area QLED devices, although the light-emitting rate of the QLED devices is improved by a certain degree of celsius.
Therefore, a new way to replace the above three schemes is urgently needed in the market at present to improve the light-emitting rate of the QLED device.
Disclosure of Invention
Based on the above defects, the present application provides a QLED, a method for manufacturing the QLED and improving the light-emitting efficiency of the QLED, so as to improve the problem of low light-emitting efficiency of the QLED, and provide another alternative solution for relevant practitioners.
The application is realized as follows:
in a first aspect, examples of the present application provide a method of increasing the light extraction rate of a QLED. The QLED has a transparent substrate as an exit light window, and the method comprises: and manufacturing a diffraction structure on the outer surface of the transparent matrix, wherein the diffraction structure is formed by a nano-pillar array.
In a second aspect, examples of the present application provide a QLED having a transparent substrate as an exit light window. A diffraction structure composed of a nano-pillar array is formed on the outer surface of the transparent substrate.
According to some examples of the present application, the material of the nanopillar array is a solid oxide;
optionally, the oxide comprises zinc oxide, silicon dioxide or aluminum oxide.
According to some examples of the present application, the radius of the nanopillars is 100nm to 200nm, the high degree celsius is 200nm to 400nm, and the spacing between the respective nanopillars is 400nm to 800 nm.
According to some examples of the application, the pitch is a linear distance between axes of two adjacent nanopillars.
In a third aspect, examples of the present application provide a method of fabricating a QLED, comprising: providing a carrier material constituting a transparent matrix of the quantum dot light emitting diode; manufacturing a diffraction structure consisting of a nano-pillar array on the surface of the carrier; and manufacturing a functional layer of the quantum dot light-emitting diode on the surface of the carrier, which is far away from the diffraction structure.
According to some examples of the application, the diffractive structure is produced by a templating process.
According to some examples of the application, the template method includes:
providing a template having a plate for forming diffractive structures;
transferring the manufacturing material of the nano-column to the outer surface to form a covering layer covering the outer surface;
the pattern of the template is transferred to the cover layer.
According to some examples of the present application, the nano-pillars are made of an oxide colloid and transferred to the outer surface by means of coating;
the method of transferring a plate of a template to an overlay layer comprises: imprinting a template on the covering layer, heating to enable the oxide colloid to form a nano-pillar array, and removing the template.
According to some examples of the application, the method of transferring a plate of a template to an overlay layer further comprises: after removing the template, the nanopillar array is heat treated.
In the implementation process, the embodiment of the present application provides a method for manufacturing a diffraction structure on an outer surface (light exit surface) of a transparent substrate of a quantum dot light emitting diode, so as to improve the light exit rate of the quantum dot light emitting diode. The diffraction structure can effectively inhibit the total reflection between the air of the light and the light-emitting surface, so that the light can be emitted more.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments or the prior art of the present application, the drawings used in the description of the embodiments or the prior art will be briefly described below.
Fig. 1 is a schematic structural diagram of a QLED in an example of the present application;
fig. 2 shows a schematic process flow diagram for making the QLED of fig. 1.
Icon: 101-an aluminum layer; 102-an electron injection layer; 103-a light emitting layer; 104-a hole injection layer; 105-a hole transport layer; 106-indium-selenium oxide layer; 107-glass substrate; 108-diffractive structure.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of the QLED and the method for manufacturing the QLED and improving the light extraction rate of the QLED according to the embodiment of the present application:
the QLED is a light source device with various excellent performances, but its light-emitting rate is not high, which is a difficult problem to be solved urgently.
In view of the above, in the present example, the inventor proposes a new QLED device structure, and the structure thereof refers to fig. 1.
Among them, a glass substrate 107, an indium-selenium oxide layer 106 (as an anode), a hole transport layer 105, a hole injection layer 104, a light emitting layer 103, an electron injection layer 102, and an aluminum layer 101 (as a metal electrode-cathode) are laminated in this order on the non-light emitting side. A rod-shaped body formed on the outer surface of the glass substrate on the light-emitting side. And a plurality of rods form a periodic array. In the present example, the rods form a diffractive structure 108 made of an array of nanorods.
It should be noted that, in order to illustrate the diffractive structure 108, the presence of the diffractive structure 108 is shown in the figures. However, the relative sizes and proportions of the diffractive structure 108 and the other layer structures in the structure shown in fig. 1 do not constitute structural limitations for the QLED device of the present application. For example, the diffractive structure is significantly smaller relative to the other layers.
The material for forming the diffraction structure 108 may be selected from metal oxides or non-metal oxides. Illustratively, the metal oxide is, for example, zinc oxide (ZnO), aluminum oxide (Al)2O3) (ii) a Non-metal oxides, for example, being silicon dioxide (SiO)2). In principle, it would be beneficial to have a material for the diffractive structure 108 that is transparent at high degrees celsius, environmentally stable, and inexpensive.
In order to implement the diffractive structure 108, it can be fabricated by photolithography in a semiconductor process. In the present example, the diffractive structure 108 is chosen to be fabricated by a templating method. The method has the advantages of low requirements on process conditions, low implementation difficulty and capability of meeting the size requirements of a large area.
In general, the method essentially comprises the steps of: providing a carrier material (e.g., transparent lift-off) that forms the transparent matrix of the quantum dot light emitting diode; then manufacturing a diffraction structure consisting of a nano-pillar array on the surface of the carrier; and manufacturing a functional layer of the quantum dot light-emitting diode on the surface of the carrier deviating from the diffraction structure. The functional layers mainly comprise quantum dot light-emitting layers and other electron blocking layers, hole blocking layers, electron transport layers, electron injection layers, hole transport layers or hole injection layers and the like which are selected and constructed according to requirements.
This scheme is described in detail below with reference to fig. 2.
First, a template is produced.
Illustratively, a silicon material is taken as a substrate, and a silicon nano-pillar array is manufactured on the surface of the substrate. The specifications are, for example, 100 to 200nm in radius, 200 to 400nm in nanopillar height, and 400 to 800nm in nanopillar distance (distance between centers of two nanopillars). Thereby obtaining a silicon substrate with nanopatterning.
The nano-patterned silicon substrate described above is then used to fabricate a template. In the present example, the template to be manufactured is a Polydimethylsiloxane (PDMS, which is an organosilicon) template. Spin coating PDMS on the nano-patterned silicon substrate; the parameters during spin coating can be selected as follows: spin coating at the speed of 1500-. The PDMS was cured (by heating at 60 to 80 ℃) and then peeled off from the silicon substrate, thereby obtaining a template.
The template is made in the above manner in the present application example, but obviously, the method for making the template does not constitute a limitation to the present application. The template can be fabricated in a variety of ways, with the limitation that an effective periodic nanorod array can be obtained.
Next, a diffraction structure is fabricated
Illustratively, an oxide (ZnO, SiO) is prepared2Or Al2O3) The precursor of (1). Oxide colloid is prepared by a sol-gel method, and the prepared colloid is transferred to an ITO glass substrate by a spin coating or spray coating mode to obtain a precursor (sol). The spin coating process may be, for example: spin-coating at 500-1000r/min for 10-20s, and then spin-coating at 4000-6000r/min for 20-40 s.
The precursor composed of the oxide colloid is covered with a template, and pressure is applied to form a columnar structure of the precursor, and simultaneously heating (for example, aging is performed for 2 to 4 hours in a vacuum drying oven at 100 to 120 degrees celsius) is performed to mold (gel) the oxide nanopillars.
The template is then removed to obtain the nano-pillars of the gel material of the oxide that have been cured, and then a periodic array of nano-pillars in the form of a stable oxide is obtained by further heating (e.g., at a temperature of 300-. The oxide constituting the nano-pillars can be crystallized by further heat treatment of the solidified nano-pillars, thereby obtaining a more stable oxide, and further, achieving an effect of improving the lifetime of the device (e.g., QLED).
The present application is described in further detail with reference to examples below.
Example 1
(1) Cleaning a silicon substrate, and preparing silicon nano-pillars on the silicon substrate by using a mask etching process, wherein the radius of each nano-pillar is 100nm, the height of each nano-pillar is 400nm, and the distance between the nano-pillars (the distance between the centers of the two nano-pillars) is 600 nm.
(2) Transferring the prepared silicon substrate to a spin coater to be horizontal, dripping uncured PDMS on the surface of the silicon substrate, spin-coating at 1500r/min for 20s, heating and curing on a heating plate at 60 ℃, and taking the PDMS off the substrate for later use.
(3) Preparation of SiO Using the Sol-gel Process2And filtering the sol to remove larger particles. Cleaning and drying the ITO glass light-emitting surface, and then, cleaning and drying SiO2The sol is coated on the light-emitting surface in a spin mode. During the spin coating, 500r/min is firstly used for spin coating for 10s, and then 4000r/min is used for spin coating for 20 s. Then covering the prepared PDMS template in the step (2) on SiO2Putting the sol film on a sol film, and aging the sol film in a vacuum drying oven at 100 ℃ for 2 hours to form solid SiO2The gel of (4).
(4) Stripping off the PDMS template, heating the ITO glass in a high-temperature furnace at 300 ℃ for 1 hour to enable SiO in the step (3)2Periodic nano-pillars are formed.
(5) And finally, cleaning the ITO surface of the ITO glass again, preparing a 100nm thick PEDOT serving as a hole transport layer, an 80nm thick TFB serving as a hole injection layer, a 50nm thick CdSe/ZnS serving as a quantum dot light emitting layer and a 120nm thick ZnO serving as an electron injection layer in a spin coating mode, and preparing a 100nm thick Al metal electrode in an evaporation plating mode.
Example 2
(1) Cleaning a silicon substrate, and preparing silicon nano-pillars on the silicon substrate by using a mask etching process, wherein the radius of each nano-pillar is 100nm, the height of each nano-pillar is 400nm, and the distance between the nano-pillars (the distance between the centers of the two nano-pillars) is 600 nm.
(2) Transferring the prepared silicon substrate to a spin coater to be horizontal, dripping uncured PDMS on the surface of the silicon substrate, performing spin coating at 1750r/min for 26s, heating and curing on a heating plate at 64 ℃, and taking the PDMS off the substrate for later use.
(3) ZnO sol is prepared by a sol-gel method, and the sol is filtered to remove larger particles. And cleaning and drying the ITO glass light-emitting surface, and spin-coating ZnO sol on the light-emitting surface. During the spin coating, the spin coating is performed for 12s at 630r/min, and then the spin coating is performed for 25s at 4400 r/min. And (3) covering the PDMS template prepared in the step (2) on the ZnO sol film, and aging the PDMS template in a vacuum drying oven at 104 ℃ for 3 hours to form solid ZnO gel.
(4) And (3) stripping and removing the PDMS template, and heating the ITO glass in a high-temperature furnace at 335 ℃ for 1 hour to form the ZnO in the step (3) into periodic nano-columns.
(5) And finally, cleaning the ITO surface of the ITO glass again, preparing a 100nm thick PEDOT serving as a hole transport layer, an 80nm thick TFB serving as a hole injection layer, a 50nm thick CdSe/ZnS serving as a quantum dot light emitting layer and a 120nm thick ZnO serving as an electron injection layer in a spin coating mode, and preparing a 100nm thick Al metal electrode in an evaporation plating mode.
Example 3
(1) Cleaning a silicon substrate, and preparing silicon nano-pillars on the silicon substrate by using a mask etching process, wherein the radius of each nano-pillar is 200nm, the height of each nano-pillar is 400nm, and the distance between the nano-pillars (the distance between the centers of the two nano-pillars) is 800 nm.
(2) Transferring the prepared silicon substrate to a spin coater to be horizontal, dripping uncured PDMS on the surface of the silicon substrate, spin-coating at 2000r/min for 20s, heating and curing on a heating plate at 76 ℃, and taking the PDMS off the substrate for later use.
(3) Preparation of SiO Using the Sol-gel Process2Sol andand filtering the sol to remove larger particles. Cleaning and drying the ITO glass light-emitting surface, and then, cleaning and drying SiO2The sol is coated on the light-emitting surface in a spin mode. During the spin coating, 760r/min is firstly used for 18s, and then 5000r/min is used for 36 s. Then covering the prepared PDMS template in the step (2) on SiO2Putting the sol film on a sol film, and aging the sol film in a vacuum drying oven for 3 hours at 110 ℃ to form solid SiO2The gel of (4).
(4) Stripping off the PDMS template, heating the ITO glass in a high temperature furnace at 370 ℃ for 2 hours to obtain SiO in the step (3)2Periodic nano-pillars are formed.
(5) And finally, cleaning the ITO surface of the ITO glass again, preparing a 100nm thick PEDOT serving as a hole transport layer, an 80nm thick TFB serving as a hole injection layer, a 50nm thick CdSe/ZnS serving as a quantum dot light emitting layer and a 120nm thick ZnO serving as an electron injection layer in a spin coating mode, and preparing a 100nm thick Al metal electrode in an evaporation plating mode.
Example 4
(1) Cleaning a silicon substrate, and preparing silicon nano-pillars on the silicon substrate by using a mask etching process, wherein the radius of each nano-pillar is 200nm, the height of each nano-pillar is 400nm, and the distance between the nano-pillars (the distance between the centers of the two nano-pillars) is 800 nm.
(2) Transferring the prepared silicon substrate to a spin coater to be horizontal, dripping uncured PDMS on the surface of the silicon substrate, spin-coating for 40s at 2500r/min, heating and curing on a heating plate at 80 ℃, and taking the PDMS off the substrate for later use.
(3) Preparation of Al using sol-gel method2O3And filtering the sol to remove larger particles. Cleaning and drying the ITO glass light emitting surface, and then adding Al2O3The sol is coated on the light-emitting surface in a spin mode. In the spin coating, 1000r/min is first used for 20s, and then 6000r/min is used for 40 s. Then covering the prepared PDMS template in the step (2) on Al2O3Putting the sol film on a sol film, and aging the sol film for 4 hours at 120 ℃ in a vacuum drying oven to form solid Al2O3The gel of (4).
(4) Stripping off the PDMS templateRemoving and heating the ITO glass in a high-temperature furnace at 400 ℃ for 2 hours to ensure that Al in the (3)2O3Periodic nano-pillars are formed.
(5) And finally, cleaning the ITO surface of the ITO glass again, preparing a 100nm thick PEDOT serving as a hole transport layer, an 80nm thick TFB serving as a hole injection layer, a 50nm thick CdSe/ZnS serving as a quantum dot light emitting layer and a 120nm thick ZnO serving as an electron injection layer in a spin coating mode, and preparing a 100nm thick Al metal electrode in an evaporation plating mode.
Comparative example 1
After the ITO glass is cleaned, a 100nm thick PEDOT layer is prepared through a spin coating mode to serve as a hole transport layer, an 80nm thick TFB layer serves as a hole injection layer, a 50nm thick CdSe/ZnS layer serves as a quantum dot light emitting layer, a 120nm thick ZnO layer serves as an electron injection layer, and an Al metal electrode with the thickness of 100nm can be prepared through an evaporation mode.
The devices prepared in examples 1 to 4 and comparative example 1 were subjected to photoelectric property tests. The External Quantum Efficiency (EQE) of the device is tested by using an integrating sphere system at normal temperature and normal pressure, the EQE value of the same device is higher when the light-emitting rate of the same device is higher, and the EQE test value is shown in the following table 1.
TABLE 1
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A method of increasing the light extraction from a QLED having a transparent substrate as an extraction window, the method comprising: and manufacturing a diffraction structure on the outer surface of the transparent matrix, wherein the diffraction structure is composed of a nano-pillar array.
2. A QLED having a transparent substrate as an exit light window, characterized in that a diffraction structure composed of a nanopillar array is formed on an outer surface of the transparent substrate.
3. A QLED of claim 2, wherein the material of the nanopillar array is a solid oxide;
optionally, the oxide comprises zinc oxide, silicon dioxide or aluminum oxide.
4. A QLED according to claim 2 or 3, wherein the nanopillars have a radius of 100nm to 200nm, a height of 200nm to 400nm and a spacing between individual nanopillars of 400nm to 800 nm.
5. A QLED according to claim 4 wherein the pitch is the linear distance between the axes of two adjacent nanopillars.
6. A method of fabricating a QLED as claimed in any of claims 2 to 5, the method comprising:
providing a carrier material constituting a transparent matrix of the quantum dot light emitting diode;
manufacturing a diffraction structure consisting of a nano-pillar array on the surface of the carrier;
and manufacturing a functional layer of the quantum dot light-emitting diode on the surface of the carrier, which is far away from the diffraction structure.
7. A method of fabricating a QLED as claimed in claim 6, wherein the diffractive structure is fabricated by a stencil method.
8. A method of fabricating a QLED as recited in claim 7, wherein the stencil method comprises:
providing a template having a plate for forming the diffractive structure;
transferring the manufacturing material of the nano-pillars to the outer surface to form a covering layer covering the outer surface;
transferring the pattern of the template to the cover layer.
9. A method of fabricating a QLED as recited in claim 8, wherein the nanopillar is fabricated from an oxide gel and is transferred to the outer surface by coating;
the method of transferring the plate of the template to the cover layer comprises: and imprinting the template on the covering layer, heating to enable the oxide colloid to form a nano-pillar array, and removing the template.
10. A method of fabricating a QLED as recited in claim 9, wherein the step of transferring the template plate to the cover layer further comprises: after removing the template, thermally treating the nanopillar array.
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