CN113130786A - Light emitting diode and preparation method thereof - Google Patents
Light emitting diode and preparation method thereof Download PDFInfo
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- CN113130786A CN113130786A CN201911415399.9A CN201911415399A CN113130786A CN 113130786 A CN113130786 A CN 113130786A CN 201911415399 A CN201911415399 A CN 201911415399A CN 113130786 A CN113130786 A CN 113130786A
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- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
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Abstract
The invention belongs to the technical field of display, and particularly relates to a light-emitting diode and a preparation method thereof. The preparation method provided by the invention comprises the following steps: depositing a metal compound precursor on a substrate to form a metal compound precursor film; and irradiating the metal compound precursor film by adopting infrared laser, and annealing to form the electron transport layer. The problem that the annealing process of the conventional electron transport layer easily causes damage to the inside of a device is solved.
Description
Technical Field
The invention belongs to the technical field of display, and particularly relates to a light-emitting diode and a preparation method thereof.
Background
In recent years, metal compound materials such as zinc oxide (ZnO) have been widely used in the preparation of solar cells, thin film transistors, light emitting diodes, and the like, due to their excellent electrical properties and good visible light transmittance, and have a wide development prospect. The method for preparing the zinc oxide (ZnO) and other metal compound materials by adopting the sol-gel method can meet most research and development requirements and is widely used due to the advantages of short manufacturing period, controllable components, simple process, low cost and the like.
Quantum Dot Light Emitting Diodes (QLEDs) are mainly composed of functional film layers such as a hole injection layer, a hole transport layer, a Light Emitting layer, an electron transport layer, and an electron injection layer to form a p-i-n junction-like structure. The balance of electrons and holes is an important factor influencing the performance of the device, so how to optimize the transmission efficiency of the electrons and the holes directly influences the service life and the performance improvement of the QLED device. In the existing process for preparing the electron transport layer, a metal compound material such as zinc oxide (ZnO) is often used as an electron transport layer material to be coated on the luminescent layer, and then annealing treatment is performed. And during annealing, connecting the device deposited with the ZnO precursor film with a heating plate, annealing at 80 ℃ in an inert gas environment, and connecting one side of the device close to the anode with the heating plate. However, the annealing process requires a long time, and the long-time heat treatment is liable to damage the internal structure of the device, resulting in fluorescence quenching.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a light-emitting diode, and aims to solve the problem that the annealing process of the conventional electron transport layer is easy to cause damage to the inside of a device.
Another object of the present invention is to provide a light emitting diode prepared by the above preparation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a light emitting diode comprises the following steps of preparing an electron transport layer:
providing a substrate and a metal compound precursor, and depositing the metal compound precursor on the substrate to form a metal compound precursor film;
and irradiating the metal compound precursor film by adopting infrared laser, and annealing to form the electron transport layer.
According to the preparation method of the light-emitting diode, infrared laser is adopted to irradiate the metal compound precursor film, so that the temperature of the surface of the material is instantly increased to generate a heat effect, and an electron transport layer is formed, thereby achieving the purpose of annealing, being short and effective, greatly reducing the annealing time, reducing the risk of contact between a device and water and oxygen, and being beneficial to prolonging the service life of the device; meanwhile, the roughness of the film is reduced by the short-time and effective laser annealing, and the crystallinity of the film is improved, so that the resistivity is improved; in addition, the infrared laser directly radiates the metal compound precursor film, so that high temperature generated by the infrared laser mainly acts on the metal compound precursor film, the damage of the high temperature to the internal structure of the device is avoided, and the luminous performance of the device is integrally improved. Therefore, the invention adopts the infrared laser annealing method when preparing the electron transmission layer, realizes effective annealing, simultaneously considers the influence of annealing on the internal structure of the device, greatly shortens the annealing time, improves the performance of the film layer, improves the electron transmission efficiency, and integrally improves the performance and the service life of the device.
Correspondingly, the light-emitting diode is prepared by the preparation method.
The light-emitting diode provided by the invention is prepared by the preparation method, and has good light-emitting performance and long service life.
Drawings
Fig. 1 is a flowchart of a method for manufacturing a light emitting diode according to an embodiment of the present invention;
fig. 2 is a schematic diagram of a light emitting diode according to an embodiment of the present invention;
FIG. 3 is a schematic view of annealing treatment using an infrared laser in example 1;
fig. 4 is a schematic view of the annealing treatment in comparative example 1.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A method for manufacturing a light emitting diode, as shown in fig. 1, includes the following steps:
s01, providing a substrate and a metal compound precursor, and depositing the metal compound precursor on the substrate to form a metal compound precursor film;
and S02, irradiating the metal compound precursor film by adopting infrared laser, and carrying out annealing treatment to form the electron transport layer.
According to the preparation method of the light-emitting diode provided by the embodiment of the invention, the infrared laser is adopted to irradiate the metal compound precursor film, so that the temperature on the surface of the material is instantly increased to generate a heat effect, and an electron transport layer is formed, thereby achieving the purpose of annealing, being short and effective, greatly reducing the annealing time, reducing the risk of contact between the device and water and oxygen, and being beneficial to prolonging the service life of the device; meanwhile, the roughness of the film is reduced by the short-time and effective laser annealing, and the crystallinity of the film is improved, so that the resistivity is improved; in addition, the infrared laser directly radiates the metal compound precursor film, so that high temperature generated by the infrared laser mainly acts on the metal compound precursor film, the damage of the high temperature to the internal structure of the device is avoided, and the luminous performance of the device is integrally improved. Therefore, the invention adopts the infrared laser annealing method when preparing the electron transmission layer, realizes effective annealing, simultaneously considers the influence of annealing on the internal structure of the device, greatly shortens the annealing time, improves the performance of the film layer, improves the electron transmission efficiency, and integrally improves the performance and the service life of the device.
Specifically, in step S01, the metal compound precursor is deposited on the substrate to obtain a metal compound precursor thin film.
The substrate is used as a carrier for depositing the metal compound precursor, the specific structure can refer to the conventional technology in the field, and the metal compound precursor film can be formed on the substrate.
As an embodiment, the substrate has formed thereon: a light emitting layer;
the step of depositing the metal compound precursor on the substrate comprises: depositing the metal compound precursor on the light emitting layer.
And depositing a metal compound precursor on the light emitting layer to form a metal compound thin film on the light emitting layer. Because the embodiment of the invention uses the infrared laser annealing method, the annealing time is greatly shortened, the performance of the film layer is improved, the influence of annealing on luminescent layer materials such as quantum dots and the like is considered, and the performance and the service life of the device are integrally improved. By preparing the electron transport layer on the luminescent layer, when the electron transport layer is made of zinc oxide, the annealing time can be greatly shortened, the performance of the film layer can be improved, and the current zinc oxide annealing process can be simplified.
In some embodiments, the matrix comprises: an anode on which the light emitting layer is formed.
The material of the anode can refer to the conventional anode in the art, and in some embodiments, the material of the anode is selected from at least one of indium tin oxide, indium antimony oxide and arsenic trioxide.
The material of the light emitting layer can be inorganic semiconductor nanoparticles, including blue quantum dots, red quantum dots, green quantum dots, or the like. In some embodiments, the material of the light emitting layer is a blue quantum dot, including CdZnS/ZnS, CdZnSe/ZnS, CuXIn1-XS/ZnS and ZnXCd1-XAt least one of Te/ZnS. The embodiment of the invention adopts the infrared laser annealing method, avoids the transmission of high temperature to the light-emitting layer, can reduce the influence of the annealing process on the blue quantum dots to a certain extent, prevents the device from fluorescence quenching, and is beneficial to improving the performance of the blue quantum dot light-emitting device. In a further embodiment, the surface of the quantum dot is also combined with a ligand, wherein the ligand is one or more of acid ligand, thiol ligand, amine ligand, phosphine oxide ligand, phospholipid, lecithin, polyvinyl pyridine and the like.
In addition to the anode and the light-emitting layer, other functional film layers may be formed on the substrate. In some embodiments, the anode further has formed thereon: the hole injection layer is arranged between the anode and the light-emitting layer, and the hole transport layer is arranged between the hole injection layer and the light-emitting layer so as to improve the hole transport efficiency of the device and improve the light-emitting performance of the device. In some embodiments, the material of the hole injection layer is selected from at least one of poly-PEDOT: PSS (Chinese name: 3, 4-ethylenedioxythiophene: poly (styrenesulfonic acid)), 2,3,5, 6-tetrafluoro-7, 7',8,8' -tetracyanoquinodimethane, and 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-hexaazabenzophenanthrene. In some embodiments, the material of the hole transport layer is selected from at least one of poly (3-alkylthiophene) (P3AT), 1,2,4, 5-tetrakis (trifluoromethyl) benzene, polysilanes, triphenylmethanes, and triarylamines.
Specifically, in step S01, a metal compound precursor is used as a precursor material for preparing the electron transport layer.
As an embodiment, the material of the metal compound precursor includes: at least one of a zinc oxide precursor, a gallium nitride precursor, a titanium dioxide precursor, and a tin dioxide precursor, and the material of the metal compound thin film thus obtained includes: at least one of zinc oxide, gallium nitride, titanium dioxide, and tin dioxide. In some embodiments, the material of the metal compound thin film is zinc oxide. In some embodiments, the metal compound precursor is a zinc oxide precursor solution prepared by a sol-gel method, the annealing temperature required by the formed zinc oxide precursor film is always less than or equal to 100 ℃, and by adopting the infrared laser annealing method provided by the embodiments of the present invention, the damage of high temperature annealing to the light emitting layer can be avoided while the effective annealing is realized, the annealing time is greatly shortened, the roughness of the film surface can be reduced, and the electron transfer efficiency can be improved.
Specifically, in step S01, the metal compound precursor is deposited on the substrate to form a metal compound precursor thin film.
The step of depositing the metal compound precursor on the substrate may refer to the conventional operation in the art, and the deposition may be performed by spin coating, inkjet printing, magnetron sputtering, or the like. In some embodiments, the metal compound precursor is spin-coated on the light-emitting layer using a spin coating method, thereby forming a metal compound precursor thin film.
Specifically, in step S02, the metal compound precursor film is irradiated with infrared laser light and annealed to form a metal compound film.
The wavelength of the infrared laser is larger than that of visible light, such as more than 800 nanometers, and the infrared laser has the characteristics of high energy and high collimation, so that the energy can be instantaneously released at a radiation interface to generate an instantaneous thermal effect. According to the embodiment of the invention, the annealing treatment method is adopted by irradiating the metal compound precursor film with infrared laser, so that the temperature of the surface of the material is instantly increased to generate thermal effect laser evaporation, the rapid annealing of the metal compound precursor film can be realized, the time consumption is only within 10 seconds, and the annealing treatment method is short and effective. The infrared laser radiation in a short time can obviously reduce the roughness of the surface of the film and improve the crystallinity of the film, thereby reducing the resistivity of the film and further improving the luminous performance of the QLED device. Due to the fact that annealing time is greatly shortened, the risk that the device is invaded by water and oxygen before being packaged is reduced, and the service life of the device is prolonged. The short-time and effective infrared laser annealing can also reduce the damage degree of the film structure inside the device, such as avoiding the damage to the quantum dot structure caused by long-time high-temperature annealing, and effectively improving the electron mobility. Therefore, under the same current, the brightness of the device subjected to light treatment can be obviously improved, and the heat accumulation of the device can be reduced, thereby having a positive effect on the service life of the device.
The step of irradiating the metal compound precursor film with infrared laser refers to the step of conventional infrared laser irradiation in the field, so that infrared laser spots are directly irradiated on the metal compound precursor film.
As one embodiment, the wavelength of the infrared laser is 950-1050 nanometers. When the material of the light-emitting layer is the blue quantum dot, the wavelength of the infrared laser is larger than the excitation wavelength of the blue quantum dot, and the method of annealing by irradiating the metal compound precursor film with the infrared laser has very little influence on the blue quantum dot, so that the light-emitting layer is effectively protected, and the device has good light-emitting performance.
In one embodiment, the annealing step is performed by irradiating the metal compound precursor thin film with infrared laser for 0.1 to 0.2 μ sec.
As an implementation mode, the pulse width of the infrared laser is 115-125fs, the frequency is 0.8-1.2kHz, and the beam quality factor is 1-1.2. The infrared laser beam is adopted to anneal the film, and three-dimensional localized annealing is carried out on an electron transmission layer of the device with high focusing and high collimation through a physical heat effect, so that the influence on other film layers of the QLED device is reduced to the greatest extent. Meanwhile, the laser annealing period is short, generally 0.1-0.2 microseconds, and uncontrollable impurity pollution cannot be introduced, so that the performance of the device is improved.
In one embodiment, the electron transport layer has a thickness of 50 to 60 nanometers. The electron transport layer with the thickness has the best influence on the overall electrical performance of the device, and particularly in the preparation process of the top emission device, the electron transport layer with the thickness not only has relatively good electron mobility, but also has excellent optical performance.
In the method for manufacturing a light emitting diode provided by the embodiment of the present invention, after the step of manufacturing the electron transport layer, the method further includes: depositing a cathode on the electron transport layer. The step of depositing the cathode on the electron transport layer can be performed by means of a conventional technique in the art, such as spin coating, ink jet printing, magnetron sputtering, and the like. The cathode material can be referred to the cathode conventional in the art.
In summary, compared with the conventional method of annealing for a long time at a high temperature, the embodiment of the invention uses the infrared laser annealing method to achieve the annealing purpose transiently and effectively, improve the film performance and the service life of the device, and improve the performance and the service life of the device as a whole.
Based on the technical scheme, the embodiment of the invention also provides the light-emitting diode.
Correspondingly, the light-emitting diode is prepared by the preparation method.
The light-emitting diode provided by the invention is prepared by the preparation method, and has good light-emitting performance and long service life.
As an embodiment, as shown in fig. 2, the light emitting diode sequentially includes: an anode L01, a hole injection layer L02, a hole transport layer L03, a light emitting layer L04, an electron transport layer L05, and a cathode L06. In some embodiments, the electron transport layer has a thickness of 50-60 nanometers. In some embodiments, the light emitting layer has a thickness of 20-60 nm. In some embodiments, the cathode has a thickness of 15-30 nm.
In order that the above details of the practice and operation of the present invention will be clearly understood by those skilled in the art, and the advanced nature of the light emitting diode and the method of making the same according to the embodiments of the present invention will be apparent, the practice of the present invention will be illustrated by the following examples.
Example 1
The embodiment prepares the light emitting diode, and specifically comprises the following steps:
(1) on an ITO glass substrate, PEDOT: PSS, the spin coating time is 30 seconds, the spin coating is carried out, then the heating is carried out for 15 minutes, the temperature is 150 ℃, and a hole injection layer is formed.
(2) On the hole injection layer, TFB of 8mg/ml was spin-coated at 3000rpm for 30 seconds, and then heated at 150 ℃ for 30 minutes to form a hole transport layer.
(3) And spin-coating CdZnS/ZnS blue quantum dots with the concentration of 20mg/mL on the hole transport layer at the rotating speed of 2000rpm for 30 seconds to form a quantum dot light-emitting layer.
(4) Spin-coating a ZnO precursor solution on the quantum dot light-emitting layer at the rotating speed of 3000rpm for 30 seconds to form a ZnO precursor film;
(5) as shown in fig. 3, the ZnO precursor film is irradiated by infrared laser for 0.2 microseconds to form an electron transport layer; wherein, the light-emitting diameter of the infrared laser is 3mm, the wavelength is 1053nm, the pulse width is 120fs, the repetition frequency is 1kHz, and the beam quality factor is 1.2.
(6) And evaporating an Al electrode on the electron transport layer. The vacuum degree is not higher than 3 x 10 by adopting the metal thermal evaporation process to plate aluminum- 4Pa, speed of
The time was 800 seconds and the thickness was 80 nm.
Example 2
This example prepared a light emitting diode which differed from example 1 in that: the quantum dot light-emitting layer is made of CdZnSe/ZnS blue quantum dots; in the step of depositing an Al electrode on the electron transport layer, the deposition time was 150 seconds, and the thickness of the aluminum electrode was 12 nm.
The rest of the process is substantially the same as that of embodiment 1, and the description thereof is omitted here.
Comparative example 1
This comparative example prepared a light emitting diode which differed from example 1 in that: in the step of preparing the light-emitting diode, the original steps (5) to (6) are replaced by: and (3) placing the device prepared in the step (4) on a heating plate in an inert gas environment, connecting the ITO glass substrate with the heating plate, and then carrying out annealing treatment at 80 ℃, as shown in figure 4.
The rest of the process is substantially the same as that of embodiment 1, and the description thereof is omitted here.
The performance of the light emitting diodes prepared in example 1 and comparative example 1 was measured, and table 1 shows the results. In table 1, L is the luminous intensity per unit area, and is used to indicate the brightness intensity of the light emitting device; j is the current density, which represents the amount of electricity passing through a certain unit area in unit time; EOE is external quantum efficiency, and the overall luminous performance of the reaction device; eta a is the current efficiency of the device.
As shown in the results of table 1, L, J, EQE and η a of example 1 are both greater than those of comparative example 1, indicating that the light emitting performance of the device can be improved by the method provided by the example of the present invention.
TABLE 1
| L(cd/m2) | J(mA/cm2) | EQE(％) | ηA(Cd/A) | |
| Example 1 | 4571.5 | 47.3 | 7.6 | 9.7 |
| Comparative example 1 | 3066.4 | 38.3 | 6.3 | 8.0 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of a light-emitting diode is characterized by comprising the following steps of preparing an electron transport layer:
providing a substrate and a metal compound precursor, and depositing the metal compound precursor on the substrate to form a metal compound precursor film;
and irradiating the metal compound precursor film by adopting infrared laser, and annealing to form the electron transport layer.
2. The production method according to claim 1, wherein a light-emitting layer is formed on the substrate;
the step of depositing the metal compound precursor on the substrate comprises: depositing the metal compound precursor on the light emitting layer.
3. The production method according to claim 1, wherein the material of the metal compound precursor includes: at least one of a zinc oxide precursor, a gallium nitride precursor, a titanium dioxide precursor, and a tin dioxide precursor.
4. The production method according to claim 1, wherein the metal compound precursor is a zinc oxide precursor solution prepared by a sol-gel method.
5. The method as claimed in any one of claims 1 to 4, wherein the wavelength of the infrared laser is 950-1050 nm.
6. The production method according to any one of claims 1 to 4, wherein in the step of performing the annealing treatment, the metal compound precursor thin film is irradiated with infrared laser light for 0.1 to 0.2 microseconds.
7. The method as claimed in any one of claims 1 to 4, wherein the infrared laser has a pulse width of 115-125fs, a frequency of 0.8-1.2kHz, and a beam quality factor of 1-1.2.
8. The production method according to any one of claims 1 to 4, wherein the thickness of the electron transport layer is 50 to 60 nm.
9. The production method according to any one of claims 2 to 4, wherein a material of the light-emitting layer is a blue quantum dot; and/or
The material of the luminescent layer comprises CdZnS/ZnS, CdZnSe/ZnS and CuXIn1-XS/ZnS and ZnXCd1-XAt least one of Te/ZnS.
10. A light-emitting diode produced by the production method according to any one of claims 1 to 9.
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