CN113097423A - Preparation method of quantum dot light-emitting layer - Google Patents
Preparation method of quantum dot light-emitting layer Download PDFInfo
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- CN113097423A CN113097423A CN202110379088.2A CN202110379088A CN113097423A CN 113097423 A CN113097423 A CN 113097423A CN 202110379088 A CN202110379088 A CN 202110379088A CN 113097423 A CN113097423 A CN 113097423A
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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
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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
- 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
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/10—OLED displays
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
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Abstract
The invention relates to a preparation method of a quantum dot light-emitting layer, which comprises the following steps: coating a polymer on a substrate to form a polymer barrier layer, and printing quantum dot ink on the polymer barrier layer according to a pixelized pattern to obtain a quantum dot light-emitting layer; the quantum dot ink includes a combination of a quantum dot material and an organic solvent. The preparation method provided by the invention is simple in process, and can be used for preparing the pixelized quantum dot light-emitting layer in a large area, and a display device formed by the quantum dot light-emitting layer has higher current efficiency and the service life of the optical film L70.
Description
Technical Field
The invention relates to the technical field of display, in particular to a preparation method of a quantum dot light-emitting layer.
Background
The researches of organic light emitting diodes and quantum dot light emitting diodes are mature gradually, the efficiency and the level of the device are improved gradually, and due to the colloid characteristic of quantum dots, the mainstream pixelization technology of the quantum dot light emitting diodes is realized by utilizing the photoetching technology, namely, a corresponding pixel bank is prepared on a substrate, ink-jet printing is utilized, functional layers are stacked in the bank, and finally the pixelized quantum dot light emitting device is formed. However, due to the complexity of the process, there is no widespread application of the method, and the development of large-area pixelation technology is urgent.
CN107611021A discloses a method for preparing a high-precision patterned quantum dot light-emitting layer and its application, the disclosed method for preparing a high-precision patterned quantum dot light-emitting layer comprises: (1) coating reverse photoresist on one side of the substrate, and carrying out photoetching treatment on the reverse photoresist so as to form a hollow-out pattern with an inverted trapezoid longitudinal section; (2) carrying out hydrophobic treatment on the substrate at the hollow pattern, and depositing a quantum dot film; (3) performing crosslinking treatment on the quantum dot film; (4) the reverse photoresist is stripped. According to the preparation method disclosed by the invention, after the reverse photoresist is used, the longitudinal section of the developed photoresist is of an inverted trapezoid structure, so that the photoresist can be more easily stripped, the precision of the quantum dot light-emitting layer graph is higher, and the yield of the method for preparing the quantum dot light-emitting layer graph is obviously improved.
CN109599508A discloses an electroluminescent device and a method for manufacturing the same, the method for manufacturing the electroluminescent device includes: preparing any one or more of a hole transport layer, a quantum dot light-emitting layer and an electron transport layer by means of atomization deposition, wherein the preparation of the hole transport layer specifically comprises: atomizing the hole transport layer ink, depositing the hole transport layer ink on a mask plate in a deposition mode, and curing to form a film; the preparation of the quantum dot light-emitting layer specifically comprises the following steps: atomizing the quantum dot ink, depositing the quantum dot ink on a mask plate in a deposition mode, and curing to form a film; the preparation of the electron transport layer specifically comprises: after the ink of the electron transport layer is atomized, the ink is deposited on a mask plate in a deposition mode and then is solidified into a film. The preparation method of the electroluminescent device disclosed by the invention utilizes an atomization deposition mode to prepare any one or more of a hole transport layer, a quantum dot light-emitting layer and an electron transport layer, and is matched with a mask to realize the pixelation of the hole transport layer, the quantum dot light-emitting layer and the electron transport layer, so that high-pixel display is realized, and the pixel can reach 1000 PPI.
Therefore, it is necessary to develop a method for preparing a large-area pixellated high-performance quantum dot light-emitting layer with a simple process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a quantum dot light-emitting layer, wherein the preparation method is simple in process, a pixelized quantum dot light-emitting layer can be prepared in a large area, and a display device formed by the quantum dot light-emitting layer has high current efficiency and the service life of an optical film L70.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a quantum dot light-emitting layer, which comprises the following steps: coating a polymer on a substrate to form a polymer barrier layer, and printing quantum dot ink on the polymer barrier layer according to a pixelized pattern to obtain a quantum dot light-emitting layer;
the quantum dot ink includes a combination of a quantum dot material and an organic solvent.
In the preparation process of the quantum dot light-emitting layer, the quantum dot ink can dissolve the polymer barrier layer, and form pixels during printing, so that the process is simple, and the pixelized quantum dot light-emitting layer can be prepared in a large area.
Preferably, the mass concentration of the quantum dot material in the quantum dot ink is 1-70mg/mL, such as 10mg/mL, 20mg/mL, 30mg/mL, 40mg/mL, 50mg/mL, 60mg/mL, and the like.
The mass concentration of the quantum dot material is 1-70mg/mL, the mass concentration of the quantum dot material is too high, and the quantum dot ink is not enough to dissolve the polymer barrier layer; the mass concentration of the quantum dot material is too low, and the light performance of the formed quantum dot light-emitting layer is poor.
Preferably, the volume of the quantum dot ink at each pixel point position in the printing process is 10-200pL, such as 20pL, 40pL, 60pL, 80pL, 100pL, 120pL, 140pL, 160pL, 180pL, etc.
The volume of the quantum dot ink at each pixel point position is 10-200pL, when the quantum dot light-emitting layer is printed, the volume of the ink at each pixel point position is reasonably controlled to ensure that the formed quantum dot light-emitting layer meets the requirement, and the volume of the quantum dot ink is too small to dissolve the polymer barrier layer; the volume of the quantum dot ink is too large, the dissolved polymer is too large, and the effect of the barrier layer is influenced, so that the performance of a device formed by the quantum dot light-emitting layer is influenced.
Preferably, the quantum dot material comprises any one of cadmium-based quantum dot material, indium-based quantum dot material or perovskite or a combination of at least two of them.
Preferably, the organic solvent includes any one of or a combination of at least two of an alkane solvent, an alcohol solvent, an ester solvent, or an aromatic hydrocarbon solvent, wherein typical but non-limiting combinations include: a combination of an alkane solvent and an alcohol solvent, a combination of an alcohol solvent, an ester solvent and an aromatic hydrocarbon solvent, a combination of a hydrocarbon solvent, an alcohol solvent, an ester solvent and an aromatic hydrocarbon solvent, and the like.
Preferably, the organic solvent comprises any one of chlorobenzene, cyclohexylbenzene or cyclohexylethanol or a combination of at least two thereof, wherein typical but non-limiting combinations include: combinations of chlorobenzene and cyclohexylbenzene, cyclohexylbenzene and cyclohexylethanol, chlorobenzene, cyclohexylbenzene and cyclohexylethanol, and the like.
Preferably, the polymeric barrier layer has a thickness of 2-10nm, such as 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, and the like.
The thickness of the polymer barrier layer is 2-10nm, the polymer barrier layer is too thick, the quantum dot ink cannot be completely dissolved, and the photoelectric efficiency of a device formed by the quantum dot light-emitting layer is poor; the polymer barrier layer is too thin, so that the barrier effect on the quantum dot material cannot be achieved, and the device formed by the quantum dot light-emitting layer has large leakage current and low efficiency.
Preferably, the polymer comprises any one of or a combination of at least two of Polymethylmethacrylate (PMMA), polyvinyl chloride (PVC) or polyvinylpyrrolidone (PVP), with typical but non-limiting combinations including: combinations of PMMA and PVC, PVC and PVP, PMMA, PVC and PVP, and the like.
Preferably, the printing means comprises any one or a combination of at least two of inkjet printing, screen printing, spray coating or electrofluidic printing, wherein typical but non-limiting combinations include: a combination of ink jet printing and screen printing, a combination of screen printing, spray coating and electrofluid printing, a combination of ink jet printing, screen printing, spray coating and electrofluid printing, and the like.
Preferably, the preparation method further comprises the two operations of standing and drying in sequence after the printing.
Preferably, the standing time is 10-60min, such as 20min, 30min, 40min, 50min, etc.
As a preferred technical scheme, the preparation method comprises the following steps:
(1) coating a polymer on a substrate to form a polymer barrier layer of 2-10 nm;
(2) printing the quantum dot ink with the mass concentration of 1-70mg/mL on the polymer barrier layer according to a pixelized pattern, wherein the volume of the quantum dot ink of each pixel point is 10-200pL, standing for 10-60min, and drying to obtain the quantum dot light-emitting layer.
Compared with the prior art, the invention has the following beneficial effects:
in the preparation process of the quantum dot light-emitting layer, the pixels are formed while printing, the process is simple, the pixelized quantum dot light-emitting layer can be prepared in a large area, and a display device formed by the quantum dot light-emitting layer has high current efficiency and the service life of an optical film L70. Under optimized process parameters, the current efficiency is 1.6cd/cm2Above, the service life of the optical film L70 is more than 16hThe above.
Drawings
FIG. 1 is a schematic diagram of a production process before printing in example 1;
FIG. 2 is a schematic view of the preparation process after printing of example 1;
wherein 1-a substrate; 2-a polymeric barrier layer; 3-quantum dot ink; 4-quantum dot light emitting layer.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a quantum dot light-emitting layer, which comprises the following steps, and the specific processes are shown in fig. 1-fig. 2:
(1) coating a polymer (PMMA, purchased from Merland, with the mark of 9011-14-7) on a substrate 1 with an ITO film on the surface to form a 5nm polymer barrier layer 2;
(2) and (2) spraying quantum dot ink 3 (the quantum dot material is CdZnSe/ZnS, the organic solvent is chlorobenzene and cyclohexylbenzene with the mass ratio of 1: 1) with the mass concentration of 35mg/mL according to a pixelized pattern, wherein the volume of the quantum dot ink at each pixel point is 100pL, then carrying out ink-jet printing on the polymer barrier layer, standing for 40min, and drying to obtain the quantum dot light-emitting layer 4.
Example 2
The embodiment provides a preparation method of a quantum dot light-emitting layer, which comprises the following steps:
(1) coating a polymer (PMMA, purchased from Merland, with the mark of 9011-14-7) on a substrate with an ITO film on the surface to form a 2nm polymer barrier layer;
(2) and (2) spraying quantum dot ink (the quantum dot material is CdZnSe/ZnS, the organic solvent is cyclohexyl ethanol) with the mass concentration of 1mg/mL according to a pixelized pattern, wherein the volume of the quantum dot ink at each pixel point is 200pL, performing ink-jet printing on the polymer barrier layer, standing for 60min, and drying to obtain the quantum dot light-emitting layer.
Example 3
The embodiment provides a preparation method of a quantum dot light-emitting layer, which comprises the following steps:
(1) coating a polymer (PMMA, purchased from Merland, with the mark of 9011-14-7) on a substrate with an ITO film on the surface to form a 10nm polymer barrier layer;
(2) and (2) spraying quantum dot ink (CdZnSe/ZnS, wherein the organic solvent is chlorobenzene and cyclohexylbenzene in a mass ratio of 1: 1) with a mass concentration of 70mg/mL according to a pixelized pattern, wherein the volume of the quantum dot ink at each pixel point is 10pL, performing ink-jet printing on the polymer barrier layer, standing for 10min, and drying to obtain the quantum dot light-emitting layer.
Examples 4 to 5
Examples 4 to 5 are different from example 1 in that the mass concentrations of the quantum dot inks are 0.5mg/mL and 75mg/mL, respectively, and the rest is the same as example 1.
Examples 6 to 7
Examples 6 to 7 are different from example 1 in that the volumes of the quantum dot inks are 5pL and 250pL, respectively, and the rest is the same as example 1.
Examples 8 to 9
Examples 8-9 differ from example 1 in that the polymeric barrier layers had thicknesses of 1nm and 12nm, respectively, and were otherwise identical to example 1.
Comparative example 1
This comparative example is different from example 1 in that the preparation method of the quantum dot light emitting layer is a photolithography method, and the preparation method includes the steps of:
and (2) spin-coating a photoresist on the substrate, depositing quantum dots (the quantum dot material is CdZnSe/ZnS) on the photoresist and the exposed surface of the substrate after mask development, dissolving the photoresist, and developing the quantum dots to obtain the quantum dot light-emitting layer.
Performance testing
The following tests were performed after depositing functional layers on the quantum dot light emitting layers described in examples 1-9 and comparative example 1 to form QLED devices: (ii) a
(1) Testing the current efficiency of the device: current efficiency is unity luminance/current density;
(2) half peak width: peak width at half the spectral peak height;
(3) optical film L70 lifetime: that is, at normal temperature lighting (25 ℃), the illumination parameter nit of the display device is used with the operating time that is maintained until the luminous intensity decays to 70% of the initial value.
The test results are summarized in table 1.
TABLE 1
The data in the table 1 are analyzed, and the current efficiency of the quantum dot light-emitting layer prepared by the method is 0.3cd/cm2As described above, the life of the optical film L70 was 0.5h or more, and the current efficiency was 1.6cd/cm in examples 1 to 32The service life of the optical diaphragm L70 is more than 16h, so that the preparation method provided by the invention is simple in process, the pixelized quantum dot luminescent layer can be prepared in a large area, and the obtained device has high current efficiency and the service life of the optical diaphragm L70.
Analysis of comparative example 1 and example 1 shows that the performance of comparative example 1 is inferior to that of example 1, and the comprehensive performance of the device formed by the quantum dot light-emitting layer prepared by the method of the invention is better.
As can be seen from the analysis of examples 4-5 and example 1, the performances of examples 4-5 are inferior to example 1, and the comprehensive performances of the device formed by the quantum dot light-emitting layer prepared by the quantum dot ink with the mass concentration of 1-70mg/mL are proved to be better.
As can be seen from the analysis of examples 6-7 and example 1, the performances of examples 6-7 are inferior to that of example 1, and the comprehensive performances of devices formed by quantum dot light-emitting layers prepared by quantum dot ink with the volume ranging from 10pL to 200pL are better.
Analysis of examples 8-9 and example 1 shows that examples 8-9 are inferior to example 1 in performance, demonstrating that the overall performance of devices formed from quantum dot light emitting layers prepared with polymer barrier layer thicknesses in the range of 2-10nm is better.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a quantum dot light-emitting layer is characterized by comprising the following steps: coating a polymer on a substrate to form a polymer barrier layer, and printing quantum dot ink on the polymer barrier layer according to a pixelized pattern to obtain a quantum dot light-emitting layer;
the quantum dot ink includes a combination of a quantum dot material and an organic solvent.
2. The preparation method according to claim 1, wherein the mass concentration of the quantum dot material in the quantum dot ink is 1 to 70 mg/mL.
3. The preparation method according to claim 1 or 2, wherein the volume of the quantum dot ink at each pixel position in the printing process is 10-200 pL.
4. A production method according to any one of claims 1 to 3, wherein the quantum dot material includes any one of a cadmium-based quantum dot material, an indium-based quantum dot material, or perovskite, or a combination of at least two thereof.
5. The production method according to any one of claims 1 to 4, wherein the organic solvent comprises any one of an alkane solvent, an alcohol solvent, an ester solvent or an aromatic hydrocarbon solvent or a combination of at least two of them;
preferably, the organic solvent comprises any one of chlorobenzene, cyclohexylbenzene or cyclohexylethanol or a combination of at least two thereof.
6. The production method according to any one of claims 1 to 5, wherein the thickness of the polymer barrier layer is 2 to 10 nm;
preferably, the polymer comprises any one of or a combination of at least two of polymethylmethacrylate, polyvinyl chloride or polyvinylpyrrolidone.
7. The method according to any one of claims 1 to 6, wherein the printing comprises any one of ink-jet printing, screen printing, spraying, or electrohydrodynamic printing or a combination of at least two thereof.
8. The production method according to any one of claims 1 to 7, further comprising performing two operations of standing and drying in this order after printing.
9. The method according to claim 8, wherein the standing time is 10 to 60 min.
10. The production method according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) coating a polymer on a substrate to form a polymer barrier layer of 2-10 nm;
(2) printing the quantum dot ink with the mass concentration of 1-70mg/mL on the polymer barrier layer according to a pixelized pattern, wherein the volume of the quantum dot ink of each pixel point is 10-200pL, standing for 10-60min, and drying to obtain the quantum dot light-emitting layer.
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