CN113097423B - Preparation method of quantum dot luminescent layer - Google Patents
Preparation method of quantum dot luminescent layer Download PDFInfo
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- CN113097423B CN113097423B CN202110379088.2A CN202110379088A CN113097423B CN 113097423 B CN113097423 B CN 113097423B CN 202110379088 A CN202110379088 A CN 202110379088A CN 113097423 B CN113097423 B CN 113097423B
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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
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- 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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- 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
- H10K71/10—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention relates to a preparation method of a quantum dot luminescent 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 pixelated pattern to obtain the quantum dot luminescent 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 luminescent layer in a large area, and the display device formed by the quantum dot luminescent layer has higher current efficiency and longer 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 luminescent layer.
Background
The research of the organic light emitting diode and the quantum dot light emitting diode is mature gradually, the device efficiency and the level are improved gradually, and due to the colloid property of the quantum dot, the main technology of pixelation of the quantum dot light emitting diode is realized by using a photoetching technology, namely, corresponding pixel bank is prepared on a substrate, then the functional layer is accumulated in the bank by using ink-jet printing, and finally the pixelated quantum dot light emitting device is formed. However, there is no solution to the wide application today due to the complexity of the process, and the development of large area pixelation technology is also urgent.
CN107611021a discloses a method for preparing a high-precision patterned quantum dot luminescent layer and application thereof, and the disclosed method for preparing the high-precision patterned quantum dot luminescent layer comprises the following steps: (1) Coating reverse photoresist on one side of a substrate, and carrying out photoetching treatment on the reverse photoresist so as to form a hollowed-out pattern with an inverted trapezoid longitudinal section; (2) Carrying out hydrophobic treatment on the substrate at the hollowed-out pattern, and depositing a quantum dot film; (3) cross-linking the quantum dot film; (4) stripping the reverse photoresist. The disclosed preparation method uses the reverse photoresist, so that the longitudinal section of the developed photoresist is of an inverted trapezoid structure, the photoresist can be more easily stripped, the precision of the quantum dot luminescent layer graph is higher, and the yield of the method for preparing the quantum dot luminescent layer graph is remarkably improved.
CN109599508A discloses an electroluminescent device and a preparation method thereof, and the preparation method of the electroluminescent device disclosed comprises the following steps: preparing any one or more of a hole transport layer, a quantum dot luminescent layer and an electron transport layer by means of atomization deposition, wherein the preparation of the hole transport layer specifically comprises the following steps: atomizing the ink of the hole transport layer, depositing the ink by a deposition mode through a mask plate, and curing the ink to form a film; the preparation of the quantum dot luminescent layer specifically comprises the following steps: atomizing quantum dot ink, depositing through a mask plate in a deposition mode, and curing to form a film; the preparation of the electron transport layer specifically comprises: and atomizing the ink of the electron transport layer, and curing the ink to form a film after the ink is deposited by a mask plate in a deposition mode. According to the preparation method of the electroluminescent device, any one or more of the hole transport layer, the quantum dot luminescent layer and the electron transport layer is prepared in an atomization deposition mode, and the hole transport layer, the quantum dot luminescent layer and the electron transport layer are pixelated by matching with a mask plate, so that high-pixel display is realized, and the pixel can reach 1000PPI.
Therefore, it is necessary to develop a method that is simple in process and capable of producing a large-area pixelated high-performance quantum dot light emitting layer.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a quantum dot luminescent layer, which is simple in process, and can be used for preparing a pixelized quantum dot luminescent layer in a large area, wherein a display device formed by the quantum dot luminescent layer has higher current efficiency and longer service life of an optical film L70.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a quantum dot luminescent 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 pixelated pattern to obtain the quantum dot luminescent 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 luminescent layer, the quantum dot ink can dissolve the polymer barrier layer, and form pixels at the same time of printing, so that the process is simple, and the pixelated quantum dot luminescent 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, for example 10mg/mL, 20mg/mL, 30mg/mL, 40mg/mL, 50mg/mL, 60mg/mL, etc.
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 insufficient for dissolving 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 quantum dot ink at each pixel site during the printing process is 10-200pL, e.g., 20pL, 40pL, 60pL, 80pL, 100pL, 120pL, 140pL, 160pL, 180pL, etc.
According to the invention, the volume of the quantum dot ink at each pixel point is 10-200pL, and when printing is performed, the formed quantum dot luminescent layer can be ensured to meet the requirement only by reasonably controlling the volume of the ink at each pixel point, and the volume of the quantum dot ink is too small to be enough to dissolve the polymer barrier layer; the excessive volume of the quantum dot ink and the excessive dissolved polymer affect the effect of the barrier layer, thereby affecting the performance of the device formed by the quantum dot luminescent layer.
Preferably, the quantum dot material comprises any one or a combination of at least two of cadmium quantum dot material, indium quantum dot material or perovskite.
Preferably, the organic solvent comprises any one 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: combinations of an alkane solvent and an alcohol solvent, combinations of an alcohol solvent, an ester solvent and an aromatic hydrocarbon solvent, combinations 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 or a combination of at least two of chlorobenzene, cyclohexylbenzene, or cyclohexylethanol, wherein typical but non-limiting combinations include: chlorobenzene and cyclohexylbenzene, cyclohexylbenzene and cyclohexylethanol, chlorobenzene, cyclohexylbenzene and cyclohexylethanol, and the like.
Preferably, the thickness of the polymeric barrier layer is 2-10nm, such as 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, etc.
The thickness of the polymer barrier layer is 2-10nm, the polymer barrier layer is too thick, the quantum dot ink can not be completely dissolved, and the photoelectric efficiency of a device formed by the quantum dot luminescent layer is poor; the polymer blocking layer is too thin, so that the blocking effect on the quantum dot material is not realized, and the leakage current of a device formed by the quantum dot luminescent layer is larger and the efficiency is lower.
Preferably, the polymer comprises any one or a combination of at least two of polymethyl methacrylate (PMMA), polyvinyl chloride (PVC) or polyvinylpyrrolidone (PVP), wherein typical but non-limiting combinations include: combinations of PMMA and PVC, combinations of PVC and PVP, combinations of 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 inkjet printing and screen printing, a combination of screen printing, spray coating and electrofluidic printing, a combination of inkjet printing, screen printing, spray coating and electrofluidic printing, and the like.
Preferably, the preparation method further comprises two steps of standing and drying in sequence after printing.
Preferably, the time of the standing is 10-60min, such as 20min, 30min, 40min, 50min, etc.
As a preferable technical scheme, the preparation method comprises the following steps:
(1) Coating a polymer on a substrate to form a polymer barrier layer of 2-10nm;
(2) Printing the quantum dot ink with the mass concentration of 1-70mg/mL on the polymer barrier layer according to a pixelated pattern, wherein the volume of the quantum dot ink of each pixel dot is 10-200pL, standing for 10-60min, and drying to obtain the quantum dot luminescent layer.
Compared with the prior art, the invention has the following beneficial effects:
in the preparation process of the quantum dot luminescent layer, pixels are formed during printing, so that the process is simple, the pixelized quantum dot luminescent layer can be prepared in a large area, and a display device formed by the quantum dot luminescent layer has higher current efficiency and the service life of an optical film L70. Under optimized technological parameters, the current efficiency is 1.6cd/cm 2 The optical film L70 has a lifetime of 16 hours or longer.
Drawings
FIG. 1 is a schematic diagram of the preparation process before printing in example 1;
FIG. 2 is a schematic diagram of the preparation process after printing in example 1;
wherein 1-substrate; a 2-polymer barrier layer; 3-quantum dot ink; 4-quantum dot light emitting layer.
Detailed Description
To facilitate understanding of the present invention, examples are set forth below. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a preparation method of a quantum dot light-emitting layer, which comprises the following steps, and the specific process is shown in fig. 1-2:
(1) A polymer (PMMA, purchased from microphone, with the trade name of 9011-14-7) is coated on a substrate 1 with an ITO film on the surface to form a polymer barrier layer 2 with the thickness of 5 nm;
(2) And 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 pixelation pattern, wherein the volume of the quantum dot ink at each pixel point is 100pL, then performing ink jet printing on the polymer barrier layer, standing for 40min, and drying to obtain the quantum dot luminescent 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 microphone and having the mark of 9011-14-7) on a substrate with an ITO film on the surface to form a 2nm polymer barrier layer;
(2) Spraying quantum dot ink with the mass concentration of 1mg/mL (the quantum dot material is CdZnSe/ZnS, the organic solvent is cyclohexyl ethanol) according to the pixelated 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 luminescent 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 microphone and having the mark of 9011-14-7) on a substrate with an ITO film on the surface to form a 10nm polymer barrier layer;
(2) Spraying quantum dot ink (CdZnSe/ZnS, chlorobenzene and cyclohexylbenzene with the mass ratio of 1:1) with the mass concentration of 70mg/mL according to a pixelated pattern, spraying the volume of the quantum dot ink at each pixel point of 10pL, performing ink-jet printing on the polymer barrier layer, standing for 10min, and drying to obtain the quantum dot luminescent layer.
Examples 4 to 5
Examples 4-5 differ from example 1 in that the mass concentrations of the quantum dot ink were 0.5mg/mL and 75mg/mL, respectively, with the remainder being the same as example 1.
Examples 6 to 7
Examples 6-7 differ from example 1 in that the quantum dot ink volumes are 5pL and 250pL, respectively, with the remainder being the same as example 1.
Examples 8 to 9
Examples 8-9 differ from example 1 in that the polymer barrier layers have thicknesses of 1nm and 12nm, respectively, with the remainder being the same as example 1.
Comparative example 1
The difference between the present comparative example and example 1 is that the preparation method of the quantum dot light emitting layer is a photolithography method, and the preparation method includes the following steps:
spin-coating photoresist on a substrate, depositing quantum dots (the quantum dot material is CdZnSe/ZnS) on the photoresist and the exposed substrate surface after mask development, dissolving the photoresist, and developing the quantum dots to obtain the quantum dot luminescent layer.
Performance testing
Functional layers were deposited on the quantum dot light emitting layers described in examples 1-9 and comparative example 1, and after formation of the QLED devices, the following tests were performed: the method comprises the steps of carrying out a first treatment on the surface of the
(1) Device current efficiency test: current efficiency = unit brightness/current density;
(2) Half-width: peak width at half of spectral peak height;
(3) Optical film L70 lifetime: that is, the lighting parameter nit of the display device was used at normal temperature lighting (25 ℃) using an operating time that was sustained until the luminous intensity decayed to 70% of the initial value.
The test results are summarized in table 1.
TABLE 1
As can be seen from an analysis of the data in Table 1, the present invention is described inThe current efficiency of the quantum dot luminescent layer prepared by the method is 0.3cd/cm 2 The optical film L70 has a lifetime of 0.5h or more, wherein the current efficiency in examples 1 to 3 is 1.6cd/cm 2 The service life of the optical film L70 is more than 16 hours, so that the preparation method disclosed 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 higher current efficiency and the service life of the optical film L70.
As can be seen from analysis of comparative example 1 and example 1, the performance of comparative example 1 is not as good as that of example 1, and it is proved that the quantum dot luminescent layer prepared by the method of the present invention has better comprehensive performance.
As can be seen from analysis of examples 4-5 and example 1, the performance of examples 4-5 is not as good as that of example 1, and the device comprehensive performance formed by the quantum dot luminescent layer prepared by the quantum dot ink with the mass concentration in the range of 1-70mg/mL is better.
As can be seen from analysis of examples 6-7 and example 1, examples 6-7 do not perform as well as example 1, and the quantum dot luminescent layer prepared by the volume of the quantum dot ink in the range of 10-200pL has better comprehensive performance.
As can be seen from analysis of examples 8-9 and example 1, examples 8-9 perform less well than example 1, demonstrating that the quantum dot light-emitting layer prepared with a polymer barrier layer thickness in the range of 2-10nm provides a better overall device performance.
The applicant states that the detailed method of the present invention is illustrated by the above examples, but the present invention is not limited to the detailed method described above, i.e. it does not mean that the present invention must be practiced in dependence upon the detailed method described above. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (6)
1. The preparation method of the quantum dot luminescent layer is characterized by comprising the following steps of: coating a polymer on a substrate to form a polymer barrier layer, printing quantum dot ink on the polymer barrier layer according to a pixelated pattern, dissolving the polymer barrier layer at a printing position by the quantum dot ink, and forming pixels while printing to obtain the quantum dot luminescent layer;
the polymer comprises any one or a combination of at least two of polymethyl methacrylate, polyvinyl chloride or polyvinylpyrrolidone;
the quantum dot ink comprises a combination of a quantum dot material and an organic solvent;
the mass concentration of the quantum dot material in the quantum dot ink is 1-70mg/mL, the volume of the quantum dot ink at each pixel point in the printing process is 10-200pL, and the thickness of the polymer barrier layer is 2-10nm;
the quantum dot material comprises any one or a combination of at least two of cadmium quantum dot material, indium quantum dot material or perovskite;
the organic solvent comprises any one or a combination of at least two of alkane solvents, alcohol solvents, ester solvents or aromatic hydrocarbon solvents.
2. The method according to claim 1, wherein the organic solvent comprises any one or a combination of at least two of chlorobenzene, cyclohexylbenzene, and cyclohexylethanol.
3. The method of claim 1, wherein the printing comprises any one or a combination of at least two of inkjet printing, screen printing, spray coating, or electrofluidic printing.
4. The production method according to claim 1, further comprising a step of sequentially performing a standing and drying operation after printing.
5. The method according to claim 4, wherein the standing time is 10 to 60 minutes.
6. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:
(1) Coating a polymer on a substrate to form a polymer barrier layer of 2-10nm;
(2) Printing the quantum dot ink with the mass concentration of 1-70mg/mL on the polymer barrier layer according to a pixelated pattern, wherein the volume of the quantum dot ink of each pixel dot is 10-200pL, standing for 10-60min, and drying to obtain the quantum dot luminescent layer.
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| WO2015105027A1 (en) * | 2014-01-09 | 2015-07-16 | 株式会社村田製作所 | Light emitting device and method for manufacturing light emitting device |
| CN106129090B (en) * | 2016-07-22 | 2019-01-25 | 华南理工大学 | A kind of linear pixel defines layer structure and preparation method thereof |
| CN107611021A (en) * | 2017-08-10 | 2018-01-19 | 南方科技大学 | Prepare the method and its application of the quantum dot light emitting layer of patterns of high precision |
| CN107644951A (en) * | 2017-10-20 | 2018-01-30 | 东莞理工学院 | A kind of preparation method for printing OLED display screen |
| CN107785504B (en) * | 2017-10-20 | 2020-08-25 | 东莞理工学院 | Preparation method of OLED device |
| CN109768173A (en) * | 2018-12-25 | 2019-05-17 | 武汉理工大学 | A kind of full inkjet printing inverted structure light emitting diode with quantum dots preparation method |
| CN111384307B (en) * | 2018-12-29 | 2021-04-09 | Tcl科技集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| CN110724412B (en) * | 2019-10-12 | 2022-10-04 | 纳晶科技股份有限公司 | Printing method of quantum dot ink |
| CN111534151A (en) * | 2020-05-14 | 2020-08-14 | 深圳市华星光电半导体显示技术有限公司 | Quantum dot ink, display panel and manufacturing method of display panel |
| CN112251076B (en) * | 2020-09-27 | 2022-10-14 | 南京邮电大学 | Ink for ink-jet printing luminescent material, luminescent film and application |
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