CN111864124B - Preparation method of quantum dot light-emitting device and quantum dot light-emitting device - Google Patents
Preparation method of quantum dot light-emitting device and quantum dot light-emitting device Download PDFInfo
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Abstract
The application provides a preparation method of a quantum dot light-emitting device and the quantum dot light-emitting device, wherein the preparation method comprises the following steps: sequentially forming an anode layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer and a cathode aluminum metal layer on a substrate; and applying current to the cathode aluminum metal layer by using current output equipment so as to form a rough aluminum oxide barrier layer on the surface of the cathode aluminum metal layer, thereby obtaining the quantum dot light-emitting device. The method applies current treatment to the metallic aluminum at a certain temperature by utilizing the chemical property of easy oxidation of the metallic aluminum, so that the metallic aluminum of the cathode is oxidized to improve the stability of the quantum dot light-emitting device.
Description
Technical Field
The application relates to the technical field of LEDs (light emitting diodes), in particular to a quantum dot light emitting device and a preparation method thereof.
Background
A quantum dot LED is a device that emits light using quantum dots, which are semiconductor nanocrystals that can produce pure monochromatic red, green, and blue light.
The cathode of the quantum dot LED is generally made of a metal material, the metal work function directly influences the luminous efficiency and the service life of the quantum dot LED, the lower the metal work function is, the easier the electron injection is, the higher the luminous efficiency is, while the lower the metal work function is, the less Joule heat is generated during the operation of the device, the service life of the device is greatly prolonged, and the cathode of the quantum dot LED is generally made of a metal with a low work function, such as aluminum. However, water and oxygen (especially water) in the air tend to have a large influence on the metallic aluminum during the use of the device, which affects the device stability of the quantum dot LED. At present, the adopted solution is to package the outer layer of the device by using packaging glue through a packaging process, so as to ensure that water and oxygen in the air can be isolated after the packaging is finished. However, it is difficult to avoid that a small amount of water and oxygen in the air permeates into the device through the packaging adhesive, and the permeated water and oxygen still have an influence on the aluminum metal.
Disclosure of Invention
An object of the embodiments of the present application is to provide a method for manufacturing a quantum dot light emitting device and a quantum dot light emitting device, so as to solve the above technical problems.
In a first aspect, an embodiment of the present application provides a method for manufacturing a quantum dot light emitting device, including: sequentially forming an anode layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer and a cathode aluminum metal layer on a substrate; and applying current to the cathode aluminum metal layer by using current output equipment to form a rough aluminum oxide barrier layer on the surface of the cathode aluminum metal layer so as to obtain the quantum dot light-emitting device.
This application utilizes the easy oxidized chemical property of metallic aluminum, applys the electric current to metallic aluminum and handles, makes the metallic aluminum of negative pole take place the oxidation, forms the aluminium oxide barrier layer to the outside water of separation and oxygen and aluminium contact and take place chemical reaction, and then improve quantum dot luminescent device's stability.
In an alternative embodiment, the applying current to the cathodic aluminum metal layer with a current output device includes: and applying current to the cathode aluminum metal layer by using current output equipment in an environment of nitrogen-oxygen mixed gas with the oxygen content of 5-10% under the temperature condition of 25-150 ℃.
In an alternative embodiment, the applying current to the cathodic aluminum metal layer with a current output device includes: and applying current to the cathode aluminum metal layer by using a current output device in an air environment under the temperature condition of 25-150 ℃.
In an alternative embodiment, the applying current to the cathodic aluminum metal layer with a current output device includes: encapsulating an anode layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer and a cathode aluminum metal layer formed on a substrate to obtain an encapsulated device; and applying current to the cathode aluminum metal layer on the packaging device by using current output equipment until a rough aluminum oxide barrier layer is formed on the surface of the cathode aluminum metal layer to obtain the quantum dot light-emitting device.
In the above scheme, since the current is applied to the cathode aluminum metal layer after encapsulation, at this time, the cathode aluminum metal layer has been encapsulated, even if a small amount of water and oxygen in the air penetrate into the device through the encapsulating material, they are consumed by oxidation reaction with aluminum under the action of the current, and finally a rough aluminum oxide barrier layer is formed on the surface of the cathode aluminum metal layer, thereby stabilizing the cathode of the device. Because a small amount of water and oxygen in the packaging layer are consumed by oxidation reaction, and the external water and oxygen are blocked by the aluminum oxide barrier layer and the packaging layer and cannot be in contact with the aluminum substrate, the influence of the water and the oxygen on the quantum dot light-emitting device is reduced. Furthermore, the quantum dot light-emitting device after current treatment has the advantages of reduced starting voltage, improved maximum brightness and obviously prolonged service life.
In an alternative embodiment, the applying current to the cathodic aluminum metal layer with a current output device includes: applying current to the cathode aluminum metal layer by using current output equipment until a rough aluminum oxide barrier layer is formed on the surface of the cathode aluminum metal layer to obtain a device to be packaged; and packaging the device to be packaged to obtain the quantum dot light-emitting device.
In the scheme, before packaging, current is applied to the cathode aluminum metal layer, and the aluminum oxide barrier layer with high roughness is formed on the surface of the metal aluminum, so that the bonding force between the metal aluminum layer and a packaging material during next packaging is improved, the point discharge effect is obvious, the turn-on voltage of the quantum dot light-emitting device is reduced, the service life is prolonged, and the maximum brightness is improved obviously.
In an alternative embodiment, the sequentially forming an anode layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, and a cathode aluminum metal layer on a substrate includes: an anode layer, a hole injection layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, an electron injection layer and a cathode aluminum metal layer are sequentially deposited on a substrate base plate.
In an alternative embodiment, the cathode aluminum metal layer has a reflectivity of not less than 98% to visible light.
In an alternative embodiment, the current applied by the current output device comprises: pulsed current, direct current, or alternating current.
In a second aspect, an embodiment of the present application provides a quantum dot light emitting device, which is prepared by the preparation method according to any one of the optional embodiments of the first aspect and the first aspect, and includes: a substrate base plate; an anode layer on the substrate; a hole transport layer on the anode layer; the quantum dot light-emitting layer is positioned on the hole transport layer; the electron transmission layer is positioned on the quantum dot light-emitting layer; a cathode aluminum metal layer on the electron transport layer; and the aluminum oxide barrier layer with the rough surface is positioned on the cathode aluminum metal layer.
In an alternative embodiment, the alumina barrier layer comprises: the cathode structure comprises a compact alumina film barrier layer and an alumina uneven layer with a rough surface, wherein the alumina film barrier layer is positioned on the cathode aluminum metal layer, and the alumina uneven layer is positioned on the surface of the alumina film barrier layer.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and that those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
Fig. 1 is a flowchart of a method for manufacturing a quantum dot light-emitting device according to an embodiment of the present disclosure;
fig. 2 is a schematic diagram illustrating a change of the surface of the cathode aluminum metal layer in step S160;
FIG. 3 is a flow chart of one embodiment of a method of fabricating a quantum dot light emitting device;
FIG. 4 is a graph showing the relationship between the current density at a certain point on the cathode aluminum metal layer and the time after the current output device applies the DC superimposed pulse wave;
FIG. 5 is a flow chart of another embodiment of a method of fabricating a quantum dot light emitting device;
fig. 6 is a schematic view of a quantum dot light-emitting device provided in an embodiment of the present application;
fig. 7 is a specific schematic diagram of a quantum dot light-emitting device provided in an embodiment of the present application.
An icon: a 200-alumina barrier layer; a 210-aluminum matrix; a 220-alumina thin film barrier layer; 230-alumina unevenness; 310-an anode layer; 320-a hole transport layer; 330-a quantum dot light emitting layer; 340-an electron transport layer; 350-cathode aluminum metal layer; a 360-alumina barrier layer; 361-alumina thin film barrier layer; 362-alumina unevenness.
Detailed Description
The technical solutions in the embodiments of the present application will be described below with reference to the drawings in the embodiments of the present application.
In the description of the present application, it should be noted that the terms "inside", "outside", "upper", "lower", and the like indicate orientations or positional relationships based on orientations or positional relationships shown in the drawings or orientations or positional relationships conventionally laid out when products of the application are used, and are only used for convenience in describing the present application and simplifying the description, but do not indicate or imply that the referred devices or elements must have specific orientations, be constructed in specific orientations, and be operated, and thus, should not be construed as limiting the present application.
It should also be noted that, unless expressly stated or limited otherwise, the terms "disposed" and "connected" are to be construed broadly, e.g., as meaning fixedly connected, detachably connected, or integrally connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.
The embodiment of the application provides a preparation method of a quantum dot light-emitting device, wherein the quantum dot light-emitting device selects metal aluminum (Al) as a cathode material for the following reasons: (1) The metallic aluminum belongs to low work function metal and is suitable for being used as a cathode material; (2) Although aluminum is a very active metal, aluminum is different from general metals, and the surface oxidation of pure aluminum can generate a layer of dense aluminum oxide (Al) 2 O 3 ) The film can protect the aluminum from further oxidation; and (3) the price is relatively low. The application utilizes the chemical property that metallic aluminum is easy to oxidize to a certain extentAnd applying current treatment to the metallic aluminum under the temperature condition to oxidize the metallic aluminum of the cathode so as to improve the stability of the quantum dot light-emitting device.
As shown in fig. 1, the method for manufacturing a quantum dot light emitting device provided in this embodiment includes:
step S110: an anode layer is deposited on a substrate.
Step S120: a hole transport layer is deposited over the anode layer.
Step S130: a quantum dot light emitting layer is deposited on the hole transport layer.
Step S140: and depositing an electron transport layer on the quantum dot light emitting layer.
Step S150: and depositing a cathode aluminum metal layer on the electron transport layer.
In the above steps S110 to S150, an anode layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, and a cathode aluminum layer are sequentially formed on the substrate.
In other embodiments, the method of making further comprises: depositing a hole injection layer on the anode layer, so step S120 includes: depositing a hole transport layer on the hole injection layer; the preparation method also comprises the following steps: an electron injection layer is deposited on the electron transport layer, so step S150 includes: and depositing a cathode aluminum metal layer on the electron injection layer. Electrons are injected into the quantum dot light-emitting layer through the cathode aluminum metal layer, the electron injection layer and the electron transport layer, holes are injected into the quantum dot light-emitting layer through the anode layer, the hole injection layer and the hole transport layer, and the electrons and the holes are compounded in the quantum dot light-emitting layer to emit light.
Step S160: and applying current to the cathode aluminum metal layer by using a current output device so as to form a rough aluminum oxide barrier layer on the surface of the cathode aluminum metal layer.
Fig. 2 (a) - (B) show the change of the cathode aluminum metal layer surface in step S160, the change includes two stages, wherein fig. 2 (a) shows a stage a, and fig. 2 (B) shows a stage B. The high purity aluminum metal has a strong affinity for oxygen, and a dense, non-porous alumina thin film barrier 220 (stage a) is rapidly formed on the aluminum matrix 210 of the cathode aluminum metal layer at the instant of energization. With the extension of the power-on time, the alumina thin film barrier layer 220 grows to a certain thickness, which protects the aluminum substrate 210 and improves the stability of the device. Along with the thickening of the alumina thin film barrier layer 220, the alumina thin film barrier layer 220 expands due to the fact that the generated alumina is larger than the atomic volume of aluminum, an alumina uneven layer 230 is formed, the microscopic surface becomes uneven (section B), current is unevenly distributed, the resistance of a concave part is small, the current is large, the resistance of a convex part is large, the current is small, the phenomenon of point discharge is formed, the starting voltage of the quantum dot light-emitting device is reduced, and the maximum brightness is improved.
As shown in fig. 2, in step S160, the alumina barrier layer 200 on the surface of the cathode aluminum metal layer includes an alumina thin film barrier layer 220 and an alumina uneven layer 230.
In one embodiment, as shown in fig. 3, step S160 includes:
step S161: and applying current to the cathode aluminum metal layer by using current output equipment until a rough aluminum oxide barrier layer is formed on the surface of the cathode aluminum metal layer to obtain a device to be packaged.
Connecting the anode of the current output device with the anode layer of the device, connecting the cathode of the current output device with the cathode aluminum metal layer of the device, and applying current to the cathode aluminum metal layer by using the current output device, wherein the type of applied current may include: pulsed current, direct current, or alternating current. The oxidation reaction of the surface of the cathode aluminum metal layer can be accelerated by applying current to the cathode aluminum metal layer, so that the surface of the cathode aluminum metal layer can quickly form an aluminum oxide barrier layer to prevent external water and oxygen from contacting the aluminum matrix.
In one embodiment, the current output of the current output equipment is started in the environment of nitrogen-oxygen mixed gas with the oxygen content of 5% -10% under the temperature condition of 25-150 ℃, so that the current passes through the surface of the cathode aluminum metal layer. The oxygen content in the nitrogen-oxygen mixed gas is not suitable to be too high so as to prevent other organic functional layers (a hole injection layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer and an electron injection layer) from being oxidized.
In one embodiment, the current output device is used to apply current to the cathode aluminum metal layer in an air environment at a temperature of 25-150 ℃.
Step S162: and packaging the device to be packaged to obtain the quantum dot light-emitting device.
After step S161, the surface of the device to be packaged has a rough alumina barrier layer, which can effectively improve the bonding force with the packaging material, so that the packaging result of step S162 is better.
In one embodiment, in step S162, encapsulation is performed using UV resin.
In a specific embodiment, in an environment of a nitrogen-oxygen mixed gas with a temperature of 25 ℃ and an oxygen content of 5%, a direct current superimposed pulse wave is applied to a cathode aluminum metal layer of the device for 30min, so as to obtain detailed technical parameters as shown in the following table, and the detailed technical parameters are compared with the technical parameters obtained without current treatment:
watch 1
The lifetime listed in Table I means that the luminance of the red quantum dot LED is from 100cd/cm 2 Time corresponding to 50% of the initial brightness. The parameters of the dc superimposed pulse wave applied by the current output device are shown in fig. 4, which shows the relationship between the current density and the time at a certain point on the cathode aluminum metal layer.
In the above embodiment, before the encapsulation step S162, a current is applied to the cathode aluminum metal layer, and an aluminum oxide barrier layer with large roughness is formed on the surface of the aluminum substrate, so that on one hand, the bonding force with the encapsulation material during the next encapsulation is improved, and on the other hand, the point discharge effect is significant, and the turn-on voltage of the quantum dot light emitting device is reduced, the service life is prolonged, and the maximum brightness is improved significantly.
In another embodiment, as shown in fig. 5, step S160 includes:
step S163: and encapsulating the anode layer, the hole transmission layer, the quantum dot light-emitting layer, the electron transmission layer and the cathode aluminum metal layer formed on the substrate to obtain an encapsulated device.
And forming an anode layer, a hole transmission layer, a quantum dot light emitting layer, an electron transmission layer and a cathode aluminum metal layer on the substrate, and then packaging the anode layer, the hole transmission layer, the quantum dot light emitting layer, the electron transmission layer and the cathode aluminum metal layer by using a packaging material to obtain a packaging device. In one embodiment, in step S163, encapsulation is performed using UV resin.
Step S164: and applying current to the cathode aluminum metal layer on the packaging device by using current output equipment until a rough aluminum oxide barrier layer is formed on the surface of the cathode aluminum metal layer to obtain the quantum dot light-emitting device.
After the encapsulation is finished, under the temperature condition of 25-150 ℃, the current output of the current output equipment is started in the environment of nitrogen-oxygen mixed gas with the oxygen content of 5% -10% or air environment, so that the current passes through the surface of the cathode aluminum metal layer.
Optionally, the current output device in the present application may select a DMD01-100/50 type multifunctional pulse power supply device.
In a specific embodiment, in an air environment with a temperature of 25 to 150 ℃, the positive electrode and the negative electrode of a DMD01-100/50 type multifunctional pulse power supply device are respectively connected to the anode layer and the cathode aluminum metal layer of the packaging device, and a direct current superimposed pulse wave is applied to the cathode aluminum metal layer of the packaging device for 30min to obtain detailed technical parameters as the following table two, and the detailed technical parameters are compared with the technical parameters obtained without current treatment:
watch two
The lifetime listed in Table II means that the luminance of the red quantum dot LED is from 100cd/cm 2 Time corresponding to 50% of the initial brightness.
In the above embodiment, since the current is applied to the cathode aluminum metal layer after step S163, at this time, the cathode aluminum metal layer has been completely encapsulated, a small amount of water and oxygen in the air are consumed by oxidation reaction with the aluminum matrix under the current even if the encapsulating adhesive penetrates into the device, and finally a rough aluminum oxide barrier layer is formed on the surface of the cathode aluminum metal layer, thereby stabilizing the cathode of the device. Because a small amount of water and oxygen in the packaging layer are consumed by oxidation reaction, and the external water and oxygen are blocked by the aluminum oxide barrier layer and the packaging layer and cannot be in contact with the aluminum substrate, the influence of the water and the oxygen on the quantum dot light-emitting device is reduced. Furthermore, according to the technical parameters actually measured in the second table, the quantum dot light-emitting device after current processing has the advantages of reduced starting voltage, improved maximum brightness and obviously prolonged service life.
Optionally, the quantum dot light emitting device in this embodiment is a front bottom emission structure, and the reflectivity of the cathode aluminum metal layer to visible light is not lower than 98%. It will be appreciated that if the reflectivity is too low, light may be transmitted through the cathode aluminum metal layer, and in the case of high reflectivity, light is reflected at the cathode aluminum metal layer and exits the anode layer side of the front side of the device.
Further, the embodiment of the application provides a quantum dot light-emitting device, and the quantum dot light-emitting device is prepared by the preparation method provided by the embodiment. Fig. 6 shows a schematic structural view of the quantum dot light emitting device, which includes: anode layer 310, hole transport layer 320, quantum dot light emitting layer 330, electron transport layer 340, cathode aluminum metal layer 350, and alumina barrier layer 360. Wherein the anode layer 310 is located on the substrate base plate; a hole transport layer 320 on the anode layer 310; a quantum dot light emitting layer 330 on the hole transport layer 320; an electron transport layer 340 on the quantum dot light emitting layer 330; a cathode aluminum metal layer 350 on the electron transport layer 340; and an alumina barrier layer 360 on the cathode aluminum metal layer 350, wherein the surface of the alumina barrier layer 360 is rough.
Optionally, the quantum dot light emitting device further includes: the anode comprises a hole injection layer and an electron injection layer, wherein the hole injection layer is positioned between an anode layer and a hole transport layer, the hole injection layer is deposited on the anode layer, the hole transport layer is deposited on the hole injection layer, the electron injection layer is positioned between a cathode aluminum metal layer and the electron transport layer, the electron injection layer is deposited on the electron transport layer, and a cathode aluminum metal layer is deposited on the electron injection layer.
Optionally, the quantum dot light emitting device includes: and the aluminum oxide barrier layer is positioned in the packaging layer.
In the present embodiment, the alumina barrier layer 360 of the quantum dot light emitting device is obtained by applying a current to the cathode aluminum metal layer 350 for a certain time using a current output apparatus, as shown in fig. 7, the alumina barrier layer 360 includes a dense alumina thin film barrier layer 361 and an alumina uneven layer 362 having a rough surface. In the process of applying a current to the cathode aluminum metal layer 350, a dense and nonporous alumina thin film barrier layer 361 is rapidly formed on the aluminum substrate of the cathode aluminum metal layer 350 at the moment of energization, and as the energization time is prolonged, the surface of the alumina thin film barrier layer 361 expands, thereby forming an alumina uneven layer 362 above the alumina thin film barrier layer 361. An alumina thin film barrier layer 361 is positioned above the cathode aluminum metal layer 350, and an alumina uneven layer 362 is positioned above the alumina thin film barrier layer 361.
The above description is only an example of the present application and is not intended to limit the scope of 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 (7)
1. A method for manufacturing a quantum dot light-emitting device, comprising:
sequentially forming an anode layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer and a cathode aluminum metal layer on a substrate;
applying current to the cathode aluminum metal layer by using current output equipment to form a rough aluminum oxide barrier layer on the surface of the cathode aluminum metal layer to obtain a quantum dot light-emitting device;
wherein the applying current to the cathodic aluminum metal layer with a current output device comprises:
applying current to the cathode aluminum metal layer by using current output equipment in an environment of nitrogen-oxygen mixed gas with the oxygen content of 5-10% under the temperature condition of 25-150 ℃;
or applying current to the cathode aluminum metal layer by using current output equipment in an air environment under the temperature condition of 25-150 ℃.
2. The method of claim 1, wherein the applying current to the cathodic aluminum metal layer with a current output device comprises:
applying current to the cathode aluminum metal layer by using current output equipment until a rough aluminum oxide barrier layer is formed on the surface of the cathode aluminum metal layer to obtain a device to be packaged;
and packaging the device to be packaged to obtain the quantum dot light-emitting device.
3. The method of claim 1, wherein sequentially forming an anode layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, and a cathode aluminum metal layer on a substrate comprises: and sequentially depositing an anode layer, a hole injection layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, an electron injection layer and a cathode aluminum metal layer on the substrate.
4. The method of claim 1, wherein the cathode aluminum metal layer has a reflectivity of no less than 98% of visible light.
5. The method of claim 1, wherein the current applied by the current output device comprises: pulsed current, direct current, or alternating current.
6. A quantum dot light-emitting device produced by the production method according to any one of claims 1 to 5, comprising:
a substrate base plate;
an anode layer on the substrate;
a hole transport layer on the anode layer;
the quantum dot light-emitting layer is positioned on the hole transport layer;
the electron transmission layer is positioned on the quantum dot light-emitting layer;
a cathode aluminum metal layer on the electron transport layer;
and the aluminum oxide barrier layer with the rough surface is positioned on the cathode aluminum metal layer.
7. The quantum dot light emitting device of claim 6, wherein the alumina barrier layer comprises: the cathode structure comprises a compact alumina film barrier layer and an alumina uneven layer with a rough surface, wherein the alumina film barrier layer is positioned on the cathode aluminum metal layer, and the alumina uneven layer is positioned on the surface of the alumina film barrier layer.
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| CN103165816A (en) * | 2011-12-14 | 2013-06-19 | 海洋王照明科技股份有限公司 | Inverted top emission organic light emission diode and manufacture method thereof |
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| JP2010153365A (en) * | 2008-11-19 | 2010-07-08 | Semiconductor Energy Lab Co Ltd | Light-emitting element, light-emitting device, electronic equipment, and illumination device |
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| JPH05331696A (en) * | 1992-06-01 | 1993-12-14 | Kobe Steel Ltd | Iron-based electroplating method |
| JPH11329753A (en) * | 1998-05-06 | 1999-11-30 | Toyota Motor Corp | Organic el element |
| CN103165816A (en) * | 2011-12-14 | 2013-06-19 | 海洋王照明科技股份有限公司 | Inverted top emission organic light emission diode and manufacture method thereof |
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