CN114695716A - Preparation method of quantum dot light-emitting diode - Google Patents
Preparation method of quantum dot light-emitting diode Download PDFInfo
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- 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
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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
- H01L33/14—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 carrier transport control structure, e.g. highly-doped semiconductor layer or current-blocking structure
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
Abstract
The application relates to the technical field of display, and provides a preparation method of a quantum dot light-emitting diode. The method comprises the following steps: providing a bottom electrode substrate, and preparing a first functional layer on the bottom electrode substrate; forming a quantum dot material with an organic ligand bonded on the surface on the first functional layer to prepare a quantum dot light-emitting layer, wherein the number of carbon atoms of the organic ligand is 4-12; and preparing a second functional layer on the quantum dot light-emitting layer, preparing a top electrode on the second functional layer to prepare a quantum dot light-emitting diode, and heating the device. The device containing the quantum dot light-emitting layer modified by the organic ligand with the carbon atom number of 4-12 is subjected to heating treatment, so that the flatness of the film layer can be increased, and the interface barrier between the quantum dot and the adjacent functional layer is optimized.
Description
Technical Field
The application belongs to the technical field of display, and particularly relates to a preparation method of a quantum dot light-emitting diode.
Background
Quantum Dot Light Emitting Diodes (QLEDs) have recently gained attention and research in the illumination and display fields due to their advantages of high brightness, low power consumption, wide color gamut, and easy processing. QLEDs are considered to be a trend of next generation display and illumination because they can realize self-luminescence, low power consumption, full color display, and solid state illumination. Through the rapid development of more than twenty years, the QLED has obtained better performance parameters.
The conventional QLED realizes normal operation of devices by stacking functional layers, and the high-quality film is favorable for injection and transmission of electrons and holes, so that the non-radiative recombination probability is reduced, and the efficiency and stability of the QLED are improved. Poor film-forming quality in the QLED can cause interface potential barrier, the temperature of the device can be increased by Joule heat generated in the working process of the device, the aging of the device is further accelerated, and meanwhile, the accumulated heat can influence the formation of excitons, so that the luminous efficiency and the service life of the device are influenced; in addition, the uneven interface between the film and the film is easy to cause contact separation, so that the device fails.
Disclosure of Invention
The application aims to provide a preparation method of a quantum dot light-emitting diode device, which aims to solve the problems of poor film forming smoothness and poor interface contact of the existing quantum dot light-emitting diode.
In order to achieve the purpose of the application, the technical scheme adopted by the application is as follows:
the application provides a preparation method of a quantum dot light-emitting diode, which comprises the following steps:
providing a bottom electrode substrate, and preparing a first functional layer on the bottom electrode substrate;
forming a quantum dot material with an organic ligand bonded on the surface on the first functional layer to prepare a quantum dot light-emitting layer, wherein the number of carbon atoms of the organic ligand is 4-12;
preparing a second functional layer on the quantum dot light-emitting layer, preparing a top electrode on the second functional layer to obtain a quantum dot light-emitting diode,
the device is subjected to a heat treatment,
the bottom electrode substrate is an anode substrate, the first functional layer is a hole functional layer, the second functional layer is an electron functional layer, and the top electrode is a cathode; or
The bottom electrode substrate is a cathode substrate, the first functional layer is an electronic functional layer, the second functional layer is a hole functional layer, and the top electrode is an anode.
According to the preparation method of the quantum dot light-emitting diode, the organic ligands on the surfaces of the stacked quantum dots and the adjacent functional layers are fused at the interface through heating treatment, the distances between the quantum dots and the quantum dots in the quantum dot light-emitting layers and between the light-emitting layers and the adjacent functional layers can be shortened, the transmission efficiency of current carriers in the light-emitting layers and the interface is effectively increased, the equivalent resistance in the device is reduced, and the stability and the reliability of the device in the working state are improved. In addition, a buffer layer is formed at the interface of the quantum dot light-emitting layer and the functional layers at two adjacent sides, so that the interface potential barrier between the light-emitting layer and the functional layers at two adjacent sides can be flattened, the carrier injection efficiency can be improved, and the photoelectric performance of the device can be improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
Fig. 1 is a flow chart of a process for manufacturing a quantum dot light emitting diode according to an embodiment of the present disclosure;
FIG. 2 is a schematic view of a quantum dot stack of a luminescent layer before heat treatment provided in application example 1;
fig. 3 is a schematic view of the interface fusion between the heated light-emitting layer and the adjacent transport layer provided in embodiment 1.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
In quantum dot light emitting diodes, the length of the surface ligands affects the spacing between the quantum dots in the quantum dot light emitting layer.
In the preparation process of the quantum dot light-emitting diode device, the material selection of each functional layer and the property of the interface of the functional layer have great influence on the film forming and the electric conductivity of the device, for example, the existing film forming process, including spin coating, solution lifting, transfer printing, ink-jet printing, atomic layer deposition and other modes, has the problems of poor film forming smoothness, poor interface contact and the like. The quantum dot light-emitting layer is composed of inorganic nano-particles and surface organic ligands, and the structural composition of the quantum dots and the selection and content of surface organic matters have great influence on the properties of charge injection, exciton recombination and the like of the device. In addition, factors such as contact between quantum dot luminescent materials with different properties and an interface have a close relation with photoelectric properties and service life of the device. In view of this, it is preferable that,
as shown in fig. 1, the present application provides a method for preparing a quantum dot light emitting diode, comprising the following steps:
s01, providing a bottom electrode substrate, and preparing a first functional layer on the bottom electrode substrate;
s02, forming a quantum dot material with an organic ligand combined on the surface on the first functional layer, and preparing a quantum dot light-emitting layer, wherein the number of carbon atoms of the organic ligand is 4-12;
s03, preparing a second functional layer on the quantum dot light-emitting layer, preparing a top electrode on the second functional layer to prepare a quantum dot light-emitting diode,
and heating the device.
According to the preparation method of the quantum dot light-emitting diode provided by the embodiment of the application, the organic ligands on the surfaces of the stacked quantum dots and the adjacent functional layers are fused at the interface through heating treatment, so that the distances between the quantum dots and the quantum dots in the quantum dot light-emitting layers and between the light-emitting layers and the adjacent functional layers can be shortened, the transmission efficiency of carriers in the light-emitting layers and the transmission efficiency of the carrier at the interface can be effectively increased, the equivalent resistance in the device can be reduced, and the stability and the reliability of the device in the working state can be improved. In addition, a buffer layer is formed at the interface of the quantum dot light-emitting layer and the functional layers at two adjacent sides, so that the interface potential barrier between the light-emitting layer and the functional layers at two adjacent sides can be flattened, the carrier injection efficiency can be improved, and the photoelectric performance of the device can be improved.
In the embodiment of the present application, the bottom electrode substrate and the cathode are opposite electrodes, and are one of a cathode and an anode, and the same first functional layer and the same second functional layer are opposite functional layers, and are one of an electron functional layer and a hole functional layer. Wherein the electron function layer comprises at least one of an electron injection layer, an electron transport layer and a hole blocking layer; the hole function layer includes at least one of a hole injection layer, a hole transport layer, and an electron blocking layer.
In some embodiments, the anode is selected from one or more of indium tin oxide, fluorine doped tin oxide, indium zinc oxide, graphene, carbon nanotubes; in some embodiments, the material of the hole injection layer is PEDOT: one or more of PSS, nickel oxide, molybdenum oxide, tungsten oxide, vanadium oxide, molybdenum sulfide, tungsten sulfide and copper oxide; in some embodiments, the material of the hole transport layer is selected from one or more of the materials of the hole transport layer, PVK, Poly-TPD, CBP, TCTA, and TFB; in some embodiments, the material of the electron transport layer is n-type ZnO, TiO2、SnO、Ta2O3、AlZnO、ZnSnO、InSnO、Alq3、Ca、Ba、CsF、LiF、CsCO3One or more of (a); in some embodiments, the cathode is selected from one or more of Al, Ca, Ba, Ag. In a specific embodiment, the anode is selected from Indium Tin Oxide (ITO), and the hole injection layer is PEDOT: PSS, TFB as hole transport layer, ZnO as electron transport layer and Ag as cathode.
In some embodiments, the bottom electrode substrate is an anode substrate, the first functional layer is a hole functional layer, the second functional layer is an electron functional layer, and the top electrode is a cathode; in some embodiments, the bottom electrode substrate is a cathode substrate, the first functional layer is an electron functional layer, the second functional layer is a hole functional layer, and the top electrode is an anode.
Aiming at the problems in the prior art, in the preferable different quantum dot structures and surface ligand quantum dot light-emitting diode devices, by introducing a device heating treatment process, an interface fusion layer is formed between the light-emitting layer and the transmission layers at two adjacent sides, and the interface potential barrier between the light-emitting layer and the transmission layers at two adjacent sides is flattened, so that the carrier injection efficiency is improved, and the photoelectric performance of the device is improved.
In step S01, the first functional layer is formed on the bottom electrode substrate by a conventional method. In some embodiments, the first functional layer is prepared on the bottom electrode substrate by a solution process. Specifically, a solution of a first functional material is formed on the bottom electrode substrate, and the first functional layer is obtained through drying treatment. When the first functional layer includes a plurality of thin film layers, the thin film layers are sequentially prepared on the bottom electrode.
In some embodiments, the bottom electrode substrate is an anode substrate, the first functional layer is a hole functional layer, and the hole functional layer includes a hole injection layer and a hole transport layer. In this case, the first functional layer is prepared on the bottom electrode substrate, including: forming a hole injection material on the anode substrate to prepare a hole injection layer; and forming a hole transport material on the hole injection layer to prepare a hole transport layer.
In some embodiments, the bottom electrode substrate is a cathode substrate, the first functional layer is an electron functional layer, and the electron functional layer is an electron transport layer. In this case, the first functional layer is prepared on the bottom electrode substrate, including: an electron transport material was formed on the cathode substrate to prepare an electron transport layer.
In some embodiments, the bottom electrode substrate is a cathode substrate, the first functional layer is an electron functional layer, and the electron functional layer includes an electron injection layer and an electron transport layer. In this case, the first functional layer is prepared on the bottom electrode substrate, including: forming an electron injection material on the cathode substrate to prepare an electron injection layer; an electron transport material is formed on the electron injection layer to prepare an electron transport layer.
In the step S02, a quantum dot material is formed on the first functional layer to prepare the quantum dot light-emitting layer, which may refer to a conventional preparation method of a quantum dot light-emitting layer. In some embodiments, the quantum dot light emitting layer is prepared using a solution process. Specifically, a solution film of the quantum dot material is formed on the first functional layer, and the solvent is removed to obtain the quantum dot light-emitting layer.
In the embodiment of the application, the quantum dot material comprises an inorganic nanoparticle body and an organic ligand bonded on the surface of the inorganic nanoparticle body, wherein in the process of preparing the quantum dot solution, the organic ligand is beneficial to the dispersion of the quantum dot material in a solvent, and the appropriate organic ligand is beneficial to improving the dispersibility and stability of the quantum dot material. In the light-emitting layer solid-state film formed by the quantum dot material, quantum dots are isolated from quantum dots through the organic ligand, so that the loss of energy resonance transfer can be reduced, meanwhile, the organic ligand enables the quantum dots and adjacent functional layers to keep a certain distance, and the phenomenon that the adjacent transmission layer material quenches the light-emitting performance of the quantum dots is avoided.
In the embodiment of the application, the number of carbon atoms of the organic ligand is 4-12. When the number of carbon atoms of the organic ligand is less than 4, the dispersibility of the quantum dots in the solvent is sharply reduced, and the spacing between the quantum dots in the obtained quantum dot solid film is too small, so that the problems of energy resonance transfer, fluorescence quenching and the like are caused. Longer carbon chains and larger steric hindrance are beneficial to increasing the dispersibility of the quantum dots in an organic solvent, when the chain length of the selected ligand is larger than 12, the interface potential barrier after fusion is improved, but the quantum dot light-emitting layer and the adjacent functional layer have larger distance, still have insulation with certain strength, and are not beneficial to the injection and transmission of carriers. In addition, after the quantum dot solid-state film is formed, the distance between quantum dots can be increased, so that the distance between the quantum dots is larger than 2nm, the distance between luminescent bodies is increased, so that the equivalent resistance in the device is increased, and a part of energy is consumed and converted into joule heat, so that the photoelectric performance of the device is rapidly aged.
In some embodiments, the organic ligand is selected from the group consisting of carboxyl, amine, thiol, and phosphine-containing ligands, but the choice of reactive groups in the organic ligand is not limited thereto. In this case, active groups such as carboxyl, amino, sulfhydryl and phosphino on the surface organic ligand are connected with cations on the surface of the quantum dot in a coordination bond mode. In some embodiments, the organic ligand may be selected from the group consisting of, but not limited to, oleic acid, amines, n-octyl esters.
In some embodiments, the quantum dot surface ligand may be prepared by adding a coordinating solvent during the synthesis process to connect an organic ligand to the quantum dot surface, or by replacing the original ligand on the quantum dot surface with a selected organic ligand through ligand exchange.
In step S03, the second functional layer is formed on the quantum dot light emitting layer by a conventional method. In some embodiments, the second functional layer is prepared on the quantum dot light emitting layer by a solution process. Specifically, a solution of a second functional material is formed on the quantum dot light emitting layer, and the second functional layer is obtained through drying treatment. When the second functional layer comprises a plurality of thin film layers, each thin film layer is prepared on the quantum dot light-emitting layer in sequence.
In some embodiments, the bottom electrode substrate is an anode substrate, the second functional layer is an electron functional layer, and the electron functional layer is an electron transport layer. In this case, a second functional layer is prepared on the quantum dot light emitting layer, including: and forming an electron transport material on the quantum dot light emitting layer to prepare the electron transport layer.
In some embodiments, the bottom electrode substrate is an anode substrate, the second functional layer is an electron functional layer, and the electron functional layer includes an electron injection layer and an electron transport layer. In this case, a second functional layer is prepared on the quantum dot light emitting layer, including: forming an electron injection material on the quantum dot light-emitting layer to prepare an electron injection layer; an electron transport material is formed on the electron injection layer to prepare an electron transport layer.
In some embodiments, the bottom electrode substrate is a cathode substrate, the second functional layer is a hole functional layer, and the hole functional layer includes a hole injection layer and a hole transport layer. In this case, a second functional layer is prepared on the quantum dot light emitting layer, including: forming a hole injection material on the quantum dot light-emitting layer to prepare a hole injection layer; and forming a hole transport material on the hole injection layer to prepare a hole transport layer.
The top electrode is formed on the second functional layer by conventional methods such as evaporation.
In the quantum dot light-emitting device with the laminated structure, current carriers are injected into a light-emitting layer through a transmission layer via a cathode and an anode to carry out composite light-emitting, the light-emitting layer is made of inorganic nanoparticles with a core-shell structure and a surface organic ligand, electrons and holes need to respectively cross interface barriers of the electron transmission layer/the light-emitting layer and the hole transmission layer/the light-emitting layer, the electrons and the holes are injected into a quantum dot core through a shell layer after passing through the quantum dot surface organic ligand to carry out composite light-emitting, in the whole process, the current carriers need to overcome the interface barriers, the surface organic ligand and the shell layer resistance, and the number of the current carriers effectively injected into a light-emitting core is in direct proportion to the performance of the quantum dot light-emitting diode device.
The film morphology and the performance of the quantum dot light-emitting diode device are greatly influenced by the organic ligand of the quantum dot light-emitting layer, and particularly, the organic ligand is an insulating and non-conducting substance, so that the charge injection and transmission efficiency of the quantum dot light-emitting diode device can be reduced by the longer organic ligand. In view of this, in the process of manufacturing a quantum dot light emitting diode device according to the embodiments of the present application, a heating process is performed during or after the device manufacturing process, so as to improve the performance of a light emitting layer formed by quantum dots having a relatively long organic ligand with a carbon number of 4 to 12 on the surface. On one hand, partial fusion can occur between quantum dots in the light-emitting layer and between organic ligands of the light-emitting layer and adjacent functional layers on the upper side and the lower side at the interface through heating treatment, so that the interface potential barrier between the quantum dots and the functional layers is effectively optimized; on the other hand, the heating treatment shortens the distance between the functional layer and the light-emitting main body, reduces the insulativity of the organic ligand, improves the injection and transmission efficiency of current carriers, reduces the internal equivalent resistance of the device, and improves the stability and the reliability of the device in a working state; meanwhile, the quantum dots distributed in the luminescent layer can more uniformly fill the existing space vacancies under thermal induction, increase the flatness of the luminescent layer of the quantum dots, and can effectively avoid direct recombination of electrons and holes tunneling through the quantum dot film layer, thereby improving the performance of the device.
Although the film thickness of the functional layer is nanometer to micron, the loss in the heat transfer process causes the fusion effect of the upper and lower interfaces of the quantum dot, so the heating temperature and time need to be changed according to the change of the film thickness of the luminescent layer of the quantum dot. Specifically, in the quantum dot light-emitting diode device, the thickness of the light-emitting layer influences the exciton concentration in the light-emitting recombination region and the film-forming quality of the light-emitting layer and the interface, and different thicknesses of the light-emitting layer uniformly optimize and improve the exciton concentration in the recombination region and the film-forming quality of the light-emitting layer and the interface by introducing a heating treatment process.
When the thickness of the quantum dot light-emitting layer is thick, the interface between the light-emitting layer and the upper and lower functional layers needs relatively higher heating plate temperature and longer processing time, the performance of the device is poor, and at the same time, the quantum dots of the light-emitting layer and the functional layer materials on the upper and lower sides may be damaged at high temperature. After the thickness of the quantum dot light-emitting layer is reduced, the temperature difference between the upper transmission layer interface and the lower transmission layer interface is gradually reduced, the loss of heat between quantum dot stacking layers is reduced, and the required heating temperature and time are both reduced. Therefore, in some embodiments, the thickness of the quantum dot light emitting layer is 8-30 nm, the temperature of the heating treatment is 80-140 ℃, and the heating time is 1-30 min. The distance between the quantum dots stacked in the light-emitting layer is determined by the length of the surface ligand, and the light-emitting layer and the adjacent upper and lower transmission layers are also separated by the surface ligand, so that when the thickness of the quantum dot light-emitting layer is within the range, the effect achieved by heating can be effectively improved. At this time, the transport layer adjacent to the light emitting layer is partially fused by the surface organic ligand under the driving of heat transferred from the outside. In some embodiments, the heating treatment temperature is 60-150 ℃, and the heating time is 10-120 min.
It should be noted that in the quantum dot light emitting device with the stacked structure, since the light emitting layer in the device structure uses red, green and blue quantum dot materials with different particle sizes, the interface barriers generated by the energy level structure of the light emitting layer material are different, resulting in different carrier injection efficiency, and the exciton level difference of the effective recombination inside the light emitting layer is large. According to the embodiment of the invention, the exciton concentration in the light emitting region is regulated and controlled through optimizing the thickness of the light emitting layer, and a heating treatment process is introduced, so that the space arrangement of the laminated quantum dots and the interface morphology between the light emitting layer and the adjacent transmission layer are improved, and the photoelectric performance of the quantum dot light emitting diode is further improved. In some embodiments, the quantum dot light emitting layer is a red quantum dot light emitting layer, and the particle size of the red quantum dots is 10-16 nm; in some embodiments, the quantum dot light emitting layer is a green light quantum dot light emitting layer, and the particle size of the green light quantum dots is 8-12 nm; in some embodiments, the quantum dot light emitting layer is a blue light quantum dot light emitting layer, and the particle size of the blue quantum dots is 5-10 nm. On the basis, the thickness of the light-emitting layer of the quantum dot light-emitting diode device is based on the grain diameter of the used quantum dot.
The inventor finds that the growth of a gradient wide band gap shell layer on the outer layer of the selected quantum dot core is beneficial to exciton confinement of the quantum dot core and simultaneously reduces potential barriers for injecting charges into a luminescent core, and in addition, the shell layer material with proper lattice matching degree and gradient band gap width is selected on the outer layer of the crystal core, so that defects caused by lattice stress can be avoided, and non-radiative recombination energy loss is reduced. Thus, in some embodiments, the quantum dot material is selected to be CdxZn1-xSe/ZnSe1-ySyThe material is/ZnS, wherein the values of x and y meet the following requirements: x is more than or equal to 0 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 1. By adjusting the values of x and y, the wavelength interval can be set between 450-650 nm. In one embodiment, the quantum dot luminescent core CdxZn1-xSe, wavelength about 465nm when x is 0.2; when x is 0.35, the wavelength is about 530 nm; when x is 0.6, the wavelength is about 620 nm; at this time, the quantum dot luminescent cores of red, green and blue used in the embodiments of the present invention are obtained. Growing gradient ZnSe on the outer layer of quantum dot luminescent core1-ySyAnd (3) an alloy shell layer, wherein y is 0 at the beginning, namely the ZnSe shell layer close to the crystal nucleus has higher lattice matching degree with the CdZnSe nucleus, the y value is 0 to 1 along with the growth of the shell layer, and the ZnS component in the shell layer is gradually increased until the thinner ZnS shell layer grows at the outermost layer. The quantum dot structure obtained by the method realizes the constraint of crystal nucleus excitons through the cladding of the shell layer, simultaneously reduces the resistance of the wide band gap potential barrier of the shell layer to the injection of the charges into the crystal nucleus as far as possible, and can effectively realize the effect of the shell layer on the protection of the crystal nucleus without generating great influence on the injection of the charges.
In the embodiment of the application, the influence of the content of the ligand on the surface of the quantum dot on the selection of the heating treatment process is large, and the steric hindrance of the quantum dot with the higher content of the ligand on the surface is larger, so that the obvious fusion effect is more difficult to generate on the interface. In some embodiments, the mass percentage of the organic ligand in the quantum dot material is 5% to 20%. If the mass percentage of the organic ligand exceeds 20%, the density of the organic ligand wrapped by the quantum dot outer layer is too high, the fusion process of the luminescent layer and the interface of an adjacent functional layer such as a transmission layer is difficult to occur, and the effect of improving the interface potential barrier cannot be generated; however, when the weight percentage of the ligand is less than 5%, the dispersibility of the quantum dot in the solvent is also drastically reduced.
According to the embodiment of the application, the device with the quantum dot light emitting layer is subjected to heating treatment, the functional layer distance can be shortened, and the carrier injection and transmission efficiency is improved. Meanwhile, the quantum dots distributed in the quantum dot light-emitting layer can more uniformly fill the existing space vacancies under thermal induction, increase the flatness of the quantum dot light-emitting layer, and effectively avoid direct recombination of electrons and holes tunneling through the quantum dot film layer, thereby improving the performance of the device. It should be understood that the device subjected to heat treatment in the embodiment of the present application refers to a device having a quantum dot light emitting layer, and may be a device after the quantum dot light emitting layer is prepared, or may be a device after a second functional layer is prepared on the quantum dot light emitting layer, or may be a device having a bottom electrode, a first functional layer, a quantum dot light emitting layer, a second functional layer, and a top electrode after being prepared.
In the embodiment of the present application, there may be a plurality of options for the time node of the heating process. In some embodiments, the heating treatment may be performed after the quantum dot light emitting layer is prepared on the first functional layer, that is, the heating treatment may be performed after the quantum dot light emitting layer is prepared or before the top electrode is prepared. In some embodiments, it may be selected that the quantum dot light emitting layer is completely prepared on the first functional layer, and the second functional layer is prepared on the quantum dot light emitting layer and then subjected to a heating treatment, that is, the heating treatment occurs after the second functional layer is prepared or before the top electrode is prepared. In some embodiments, it may be selected that the quantum dot light emitting layer is completely prepared on the first functional layer, the second functional layer is prepared on the quantum dot light emitting layer, and the top electrode is prepared on the second functional layer and then subjected to a heating treatment, that is, the heating treatment occurs after the top electrode is prepared. In some embodiments, after the top electrode is prepared and before the quantum dot light emitting diode is packaged, the obtained device is subjected to heating treatment; in some embodiments, after the top electrode is prepared and the quantum dot light emitting diode is encapsulated, the resulting device is subjected to a heating process.
In the embodiment of the application, the heating mode of the heating treatment can be heating by a hot plate, an oven, infrared heating and other heating modes. The hot plate heating has a uniform and stable heat supply system, and in some embodiments, the heating process is performed by using the hot plate heating method to reduce the difference of heat obtained in the quantum dot light emitting layer and adjacent upper and lower interfaces. In some embodiments, the quantum dot light emitting diode is a front bottom emission device, and sequentially comprises a glass substrate, an ITO anode, a hole injection layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, and a cathode, which are stacked, and when a hot plate is used for heating after the quantum dot light emitting layer is prepared, the glass substrate is placed on a heating surface of the hot plate by using the hot plate as a heating tool, and heat is transferred to a hole transport layer/light emitting layer interface through the glass substrate, the ITO anode, the hole injection layer, and the hole transport layer, and then reaches the light emitting layer/electron transport layer interface through the inside of the light emitting layer.
In some embodiments, after the preparation of the top electrode is completed, the method further includes performing an encapsulation process on the obtained light emitting diode. Of course, the heating process may be performed after the device is completely encapsulated.
The following description will be given with reference to specific examples.
Example 1
A preparation method of a quantum dot light-emitting diode comprises the following steps:
spin coating PEDOT on the anode ITO: PSS, preparing a hole injection layer; spin-coating TFB on the hole injection layer to prepare a hole transport layer; spin coating Cd on hole transport layer0.6Zn0.4Se/ZnSeS/ZnS red quantum dot, Cd0.6Zn0.4Se/ZnSeS/ZnS red quantum dot surface ligand is octyl mercaptan, the mass percentage of the ligand is 8 percent, and the preparation method is characterized in thatA quantum dot light emitting layer; spin-coating ZnO on the quantum dot light-emitting layer to prepare an electron transmission layer; and evaporating Al to prepare a cathode, and packaging to form the quantum dot electroluminescent device. The electroluminescent wavelength of the red quantum dot is 630nm, the half-peak width is 22nm, the particle size is 14nm, and the film thickness of the quantum dot luminescent layer is 28 nm.
And (3) placing the well-packaged device on a hot plate at 100 ℃ for baking for 30 min.
In this embodiment 1, before the heat treatment, the stacking of quantum dots in the light emitting layer in the device structure is shown in fig. 2, and after the heat treatment, the interface fusion between the light emitting layer and the adjacent transport layer in the device structure is shown in fig. 3.
Example 2
The difference between the preparation method of the quantum dot light-emitting diode and the embodiment 1 is that: the quantum dot material in the quantum dot light-emitting layer is Cd0.35Zn0.65The quantum dot electroluminescent material comprises Se/ZnSeS/ZnS green quantum dots, wherein a ligand on the surface of each quantum dot is n-octylamine, the mass percentage of the ligand is 15%, the electroluminescent wavelength of each green quantum dot is 533nm, the half-peak width is 25nm, the particle size is 10nm, and the film thickness of a luminescent layer of each quantum dot is 20 nm; and spin coating Cd on the hole transport layer0.35Zn0.65Se/ZnSeS/ZnS green quantum dots, preparing a quantum dot light emitting layer, and then placing a sample on a hot plate at 120 ℃ for baking for 20 min.
Example 3
The difference between the preparation method of the quantum dot light-emitting diode and the embodiment 1 is that: the quantum dot material in the quantum dot light-emitting layer is Cd0.2Zn0.8The quantum dot electroluminescent device comprises Se/ZnSeS/ZnS blue quantum dots, wherein a ligand on the surface of each quantum dot is dodecyl mercaptan, the mass percentage of the ligand is 10%, the electroluminescent wavelength of each blue quantum dot is 473nm, the half-peak width of each blue quantum dot is 22nm, the particle size of each blue quantum dot is 8nm, and the film thickness of a quantum dot light-emitting layer is 20 nm; and spin coating Cd on the hole transport layer0.2Zn0.8Se/ZnSeS/ZnS blue quantum dots, preparing a quantum dot light emitting layer, and then placing a sample on a hot plate at 130 ℃ for baking for 30 min.
Comparative example 1
The quantum dot light emitting diode device of comparative example 1 was prepared in substantially the same manner as in example 1 except that: and completing the manufacture of the device without heating treatment.
Comparative example 2
The method of making the quantum dot light emitting diode device of comparative example 2 is substantially the same as example 1 except that: the mass percentage of the ligand is 25 percent.
Comparative example 3
The quantum dot light emitting diode device of comparative example 3 was prepared substantially the same as in example 1 except that: the heating temperature is 50 deg.C, and the heating time is 100 min.
The photoelectric properties and the lifetime of the quantum dot light emitting diode devices prepared in examples 1 to 3 and comparative examples 1 to 3 were tested, and the lifetime of the devices was tested by using a 128-channel lifetime testing system customized by new field of vision, guangzhou. The system is constructed by driving a QLED by a constant voltage and constant current source and testing the change of voltage or current; a photodiode detector and test system for testing the variation of brightness (photocurrent) of the QLED; the luminance meter test calibrates the luminance (photocurrent) of the QLED. The test results are shown in table 1 below, where EL denotes the peak position of the electroluminescence of the quantum dot light emitting diode device, FWHM denotes the full width at half maximum, EQE denotes the external quantum efficiency of the quantum dot light emitting diode device, CE denotes the current efficiency of the quantum dot light emitting diode device, and T denotes95@1000nit denotes the operating life of the quantum dot light emitting diode device in the constant current mode, i.e., the time taken for the luminance to decay to 95% at 1000 nit.
TABLE 1
As can be seen from table 1, the quantum dot light emitting diodes prepared in the examples of the present application have better external quantum efficiency and service life, compared to the comparative examples, which are attributed to: after the device with the quantum dot light emitting layer prepared is heated, the organic ligands on the surface of the stacked quantum dots and the adjacent functional layers are fused with each other at the interface, so that the transmission efficiency of carriers in the light emitting layer and the interface is effectively increased, the equivalent resistance in the device is reduced, and the stability and the reliability of the device in a working state are improved; meanwhile, a buffer layer is formed at the interface of the quantum dot light-emitting layer and the functional layers at two adjacent sides, so that the interface potential barrier between the light-emitting layer and the functional layers at two adjacent sides can be flattened, the carrier injection efficiency can be improved, and the photoelectric performance of the device can be improved.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A preparation method of a quantum dot light-emitting diode is characterized by comprising the following steps:
providing a bottom electrode substrate, and preparing a first functional layer on the bottom electrode substrate;
forming a quantum dot material with an organic ligand bonded on the surface on the first functional layer to prepare a quantum dot light-emitting layer, wherein the number of carbon atoms of the organic ligand is 4-12;
preparing a second functional layer on the quantum dot light-emitting layer, preparing a top electrode on the second functional layer to obtain a quantum dot light-emitting diode,
the device is subjected to a heat treatment,
the bottom electrode substrate is an anode substrate, the first functional layer is a hole functional layer, the second functional layer is an electron functional layer, and the top electrode is a cathode; or
The bottom electrode substrate is a cathode substrate, the first functional layer is an electron functional layer, the second functional layer is a hole functional layer, and the top electrode is an anode.
2. The method for preparing a quantum dot light-emitting diode according to claim 1, wherein the temperature of the heating treatment is 60 ℃ to 150 ℃ and the heating time is 10 min to 120 min.
3. The method for preparing the quantum dot light-emitting diode of claim 1, wherein the mass percentage of the organic ligand in the quantum dot material is 5-20%.
4. The method for preparing a quantum dot light-emitting diode according to any one of claims 1 to 3, wherein the thickness of the quantum dot light-emitting layer is 8 to 30nm, the temperature of the heating treatment is 80 to 140 ℃, and the heating time is 1 to 30 min.
5. The method for preparing a quantum dot light-emitting diode according to claim 4, wherein the quantum dot light-emitting layer is a red light quantum dot light-emitting layer, and the particle size of the red light quantum dot is 10 to 16 nm; and/or
The quantum dot light-emitting layer is a green light quantum dot light-emitting layer, and the particle size of the green light quantum dot is 8-12 nm; and/or
The quantum dot light-emitting layer is a blue light quantum dot light-emitting layer, and the particle size of the blue quantum dot is 5-10 nm.
6. The method of any of claims 1 to 3, wherein the heating occurs after the quantum dot light emitting layer is prepared or before the second functional layer is prepared.
7. The method of any of claims 1 to 3, wherein the heating occurs after the second functional layer is formed or before the top electrode is formed.
8. The method of any of claims 1 to 3, wherein the heating occurs after the top electrode is fabricated.
9. The method of any one of claims 1 to 3, wherein the organic ligand is selected from the group consisting of carboxyl-, amine-, thiol-, and phosphine-containing ligands.
10. The method for preparing the quantum dot light-emitting diode as claimed in any one of claims 1 to 3, wherein the quantum dot material is CdxZn1-xSe/ZnSe1-ySyThe material is/ZnS, wherein the values of x and y meet the following requirements: x is more than or equal to 0 and less than or equal to 1, and y is more than or equal to 0 and less than or equal to 1; and/or
The electron function layer comprises at least one of an electron injection layer, an electron transport layer and a hole blocking layer; and/or
The hole function layer includes at least one of a hole injection layer, a hole transport layer, and an electron blocking layer.
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