CN113270564A - QLED device based on electrofluid printed quantum dot light emitting layer and preparation method - Google Patents
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Abstract
The invention discloses a QLED device based on an electrofluid printed quantum dot light emitting layer and a preparation method thereof. The invention adopts electrofluid printing to print a quantum dot array by using a quantum dot solution as an EML functional layer, and realizes three-phase line pinning of ink drops by matching the wettability and the intersolubility of a luminescent functional layer material and a printed material thereof and the evaporation repulsion effect between adjacent ink drops. By means of the electrofluid printing direct writing technology, the constraint of a printing groove is successfully eliminated, the lower limit of ink jet printing and transfer printing technology is broken through, the resolution of a device is successfully improved, the coffee ring printing effect is inhibited, and high-quality printing is achieved.
Description
Technical Field
The invention belongs to the technical field of display, and particularly relates to a QLED device based on an electrofluid printed quantum dot light-emitting layer and a preparation method thereof.
Background
The colloid quantum dot is a novel high-quality photoelectric material with the radius close to the exciton Bohr radius, and the special size effect of the colloid quantum dot enables the colloid quantum dot to realize high-purity three-primary-color luminescence, continuously adjustable spectrum and wide color gamut by adjusting the size. The quantum dot has a good light/heat stability due to a special core-shell structure; meanwhile, the quantum dots also have excellent solution-processable properties, and are popular materials for research in the display field. Quantum dot light emitting diode devices constructed based on quantum dots have also been regarded as a promising technology for replacing organic light emitting diodes. In the past decades, quantum dot light emitting diodes have been developed with great success and rapidity, and are considered as one of the most potential high-quality candidate materials in the display field. Ink jet printing and transfer printing techniques are currently the two most common approaches to the construction of large-size QLEDs. However, the structure and the morphology of a device below 30um are difficult to regulate by ink-jet printing, and the application of the QLED in the field of high-resolution display is limited. In addition, the transfer printing technology has the problems of complicated steps, particle pollution and high requirements on the elastic stamp. The electrohydrodynamic printing is different from the traditional jet printing technology (thermal jet printing, piezoelectric jet printing and the like) and the pneumatic ink-jet printing and the like in a pushing mode, and the electrohydrodynamic printing adopts an electric field to drive to generate superfine jet flow from the top end of a liquid cone (Taylor cone) in a pulling mode to jet out micro liquid drops with the size far smaller than that of a nozzle to be deposited on a substrate. Therefore, the electrofluid printing technology is expected to replace ink jet printing and transfer printing technology to construct large-size QLEDs.
CN201910906165.8 discloses a preparation method of a perovskite quantum dot light-emitting diode and a product. Firstly, carrying out activation treatment on the clean ITO glass surface; depositing a layer of ZnO film and Al on the surface of the activated ITO glass in sequence2O3A film; in Al2O3Spin-coating a quantum dot solution on the surface of the film to obtain a quantum dot film; depositing a layer of Al on the surface of the quantum dot film2O3A film; in Al2O3Sequentially preparing a TPD hole transport layer and MoO on the surface of the film3A hole injection layer and an electrode aluminum. The quantum dot light-emitting layer is prepared by a spin coating process, the preparation method is simple and convenient in process and controllable in thickness, but patterning cannot be realized by the spin coating process, which means that the spin coating process can only prepare a single-color light-emitting device, so that the application of the full-color device in the high-resolution full-color display field is limited due to the fact that the full-color device cannot be prepared.
The documents JIANG C B, ZHONG Z, LIU B, et al, coffee-Ring-Free Quantum Dot Thin Film Using Ink-jet Printing from a Mixed-Solvent System on Modified ZnO Transport Layer for Light Emitting Devices [ J].ACS Applied Materials&Interfaces,2016,26162-26168. CdSe @ ZnS/ZnS are taken as quantum dot layer materials in the literature to prepare the ink-jet printing inverted green light QLED device, the external quantum efficiency of the printed QLED device is 1.1 percent, and the maximum current efficiency is 4.5 cd.A-1Maximum luminance of 12000cd m-2. Ink jet printing is used in the literature to print quantum dot layers, and introduces a vacuum assisted drying method, which alleviates the coffee ring effect of ink jet printing to make the device emit light uniformly throughout. Although the method is suitable for preparing a large-area QLED device, the traditional Piezoelectric Inkjet (PIJ) printing system faces the problem of large volume of inkjet droplets when printing a high-resolution display (when the piezoelectric inkjet droplets are large, and when each layer of material of a display screen is prepared by inkjet printing, because most of organic materials have similar solvent systems, the printed ink is easy to dissolve part or all of lower-layer functional materials on a functional layer deposited on the functional layer, so that the functional layer of the display device is damaged, and the performance of the device is reduced). If the drop volume is to be reduced, the simplest way is to reduce the nozzle diameter, but for the conventional piezoelectric ink jet system, when the nozzle diameter is less than 10 μm, the ink generates a great ejection resistance due to its viscosity and surface tension even if the nozzle is not clogged with the solute.
Therefore, there is a need in the art to develop a method for fabricating a quantum dot light emitting layer, which has the advantages of good appearance, uniform light emission, no coffee ring effect, and high printing precision.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide a preparation method of a QLED device based on an electrofluid printed quantum dot light-emitting layer. The method has the advantages of simple operation, easily obtained raw materials, low requirement on equipment and suitability for industrial mass production; the quantum dot device prepared by the method has controllable luminosity and excellent current efficiency.
The invention also aims to provide a QLED device based on the electrofluid printed quantum dot light-emitting layer, which is prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a QLED device based on an electrofluid printed quantum dot light-emitting layer comprises the following steps:
(1) preparing a metal oxide film on an ITO glass substrate electrode as an electron transport layer (ETL functional layer);
(2) printing a quantum dot array on the electron transport layer (ETL functional layer) by adopting electrofluid printing to form a quantum dot solution as a light emitting layer (EML functional layer); wherein the diameter of the quantum dot array is 0.5-20 um, and the interval is 2-15 um;
(3) depositing a hole transport layer (HTL functional layer) on the emission layer (EML functional layer);
(4) depositing a hole injection layer (HIL functional layer) on the hole transport layer (HTL functional layer);
(5) and evaporating a metal electrode on the hole injection layer (HIL functional layer) as a top electrode to obtain the QLED device.
Preferably, the ITO glass substrate electrode in the step (1) needs to be cleaned before use, and the cleaning means that the substrate electrode material is subjected to ultrasonic oscillation for 5-10 min by using isopropanol, tetrahydrofuran, an alkaline cleaning solution, deionized water and isopropanol in sequence.
Preferably, the preparation method of the metal oxide thin film in the step (1) is at least one of spin coating, vacuum evaporation and vacuum sputtering; more preferably vacuum evaporation. The spin coating liquid used by the spin coating method is a metal oxide-ethanol dispersion liquid, the concentration of the metal oxide-ethanol dispersion liquid is 10-30 mg/ml, the spin coating rotating speed is 1000-2500 rpm/min, the time is 20-50 s, and annealing is carried out for 30-60 min at 50-100 ℃ after spin coating film forming.
Preferably, the metal oxide material of step (1) is ZnO nanoparticles, ZnO nanoparticles doped with metal cations, and TiO2At least one of the nanoparticles.
Preferably, the thickness of the metal oxide film in the step (1) is 100-300 nm.
Preferably, the quantum dot material in the quantum dot solution of step (2) is at least one of cadmium quantum dots (CdSe/ZnS QDs), indium phosphide quantum dots (InP/ZnS QDs), zinc selenide quantum dots (ZnSe/ZnS QDs), and lead sulfide quantum dots (PbS QDs).
Preferably, the concentration of the quantum dot solution in the step (2) is 10-20 mg/mL, and the solvent is at least one of n-hexane, chloroform, chlorobenzene and toluene; more preferably at least one of chlorobenzene and toluene.
Preferably, the quantum dot array obtained by electrofluid printing in the step (2) needs annealing and curing to obtain an EML functional layer, wherein the annealing temperature is 50-150 ℃, and the curing time is 10-30 min.
Preferably, the diameter of the quantum dot array in the step (2) is 2.88-14.80 um, and the interval is 3.94-10.79 um.
Preferably, the model of the electrofluid printer used for electrofluid printing in the step (2) is SIJ-S150.
Preferably, the parameters of electrofluid printing in step (2): the voltage is 200-1200V, the voltage frequency is 100-1500 Hz, the voltage waveform is any one of square waves, triangular waves and sine waves, and the moving speed is 5-50 mm/s.
Preferably, the material of the HTL functional layer of step (3) is at least one of 4,4,4, -tris (carbazol-9-yl) triphenylamine (TCTA), N ' -bis (naphthalene-1-yl) -N, N ' -bis (phenyl) benzidine (NPB), and 4,4' -bis (9-Carbazol) Biphenyl (CBP).
Preferably, the thickness of the HTL functional layer in the step (3) is 20-60 nm.
Preferably, the deposition processes of steps (3) and (4) are at least one of vacuum evaporation and spin coating.
Preferably, the HIL functional layer material in the step (4) is at least one of polymer PEDOT, PSS, molybdenum oxide, nickel oxide and cuprous thiocyanate.
Preferably, the thickness of the HIL functional layer in the step (4) is 5-10 nm.
Preferably, the top electrode in step (5) is one of Al, Ag, Cu, Au or an alloy electrode, wherein the alloy is an alloy of at least two elements of Al, Ag, Cu and Au.
Preferably, the thickness of the top electrode in the step (5) is 100-300 nm.
Preferably, after the top electrode is prepared in step (5), the QLED device can be obtained by packaging, which is a conventional operation in the art and can be packaged by using epoxy resin.
The QLED device based on the electrofluid printed quantum dot light-emitting layer is manufactured by the method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the method for printing the quantum dot layer by the electrofluid is simple in preparation process. The method is beneficial to preparing a micro-nano structure by printing, and realizes three-phase line pinning of ink drops by matching the wettability and the intersolubility degree of the luminescent functional layer material and a printing stock thereof and the evaporation repulsion effect between adjacent ink drops. The restriction of the printing groove is successfully removed through the electrofluid printing direct writing technology. Therefore, the lower limit of ink-jet printing and transfer printing technologies can be broken through, and the resolution of the device can be successfully improved. In addition, the amino on the surface of the substrate can be coordinated with the surface of the quantum dot to play a role in fixing the quantum dot, so that the coffee ring effect of printing is inhibited, and high-quality printing is realized. The device has a certain controllable range of chromaticity and luminous efficiency, and has wide application scenes.
Drawings
Fig. 1 is a schematic structural diagram of a quantum dot light-emitting device.
FIG. 2 is a diagram of the morphology of an EML functional layer quantum dot array.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Those who do not specify specific conditions in the examples of the present invention follow conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents and the like which are not indicated for manufacturers are all conventional products which can be obtained by commercial purchase.
The materials used in the following examples are as follows:
the ITO glass is purchased from south glass company, and the sheet resistance is 15-20 omega/□. The cadmium quantum dots are purchased from Pujiafu photoelectric company of Guangdong Jiangmen. The quantum dot structure is a CdSe/CdS/CdZnS core-shell structure, the surface of the quantum dot structure is passivated by oleylamine, and the quantum dot structure is finally dispersed in a toluene solvent, wherein the concentration of the quantum dot structure is 20 mg/ml. 4,4,4, -tris (carbazol-9-yl) triphenylamine TCTA is available from Cianbolate. Zinc oxide (ZnO), molybdenum oxide (MoO)3) Purchased from Sigma.
The model of the electrofluid printer used for electrofluid printing is SIJ-S150.
Example 1
(1) Cleaning an ITO glass substrate electrode: and putting the ITO substrate into an ultrasonic cleaner, and sequentially performing ultrasonic oscillation on the recovered isopropanol, the recovered tetrahydrofuran, the alkaline cleaning solution, the deionized water and the isopropanol for 10min respectively.
(2) Spin coating a ZnO film as an ETL functional layer: dissolving zinc oxide (ZnO) in ethanol with a concentration of 30mg/ml, filtering the prepared ZnO solution with a 0.2um filter head, sucking 60uL of the solution, spin-coating for 30s at 2500rpm/min, forming a film, placing on an annealing plate, and annealing at 60 ℃ for 30 min.
(3) Printing a quantum dot array on the ETL functional layer by adopting electrofluid printing to obtain an EML functional layer, wherein the EML functional layer comprises the following components in percentage by weight: the CdSe/CdS ZnS core-shell structure red light quantum dots are dispersed in a toluene solution, and the mass concentration is 20 mg/ml; parameters of electrofluid printing: the voltage is 700V, the voltage waveform is triangular wave, the voltage frequency is 1000Hz, and the moving speed is 50 mm/s. Annealing and curing: the annealing temperature is 150 ℃, the curing time is 30min, and the diameters and the intervals of the obtained quantum dot arrays are respectively 2.88um and 10.79 um. The dot array structure is shown in fig. 2.
(4) And (3) evaporating an HTL functional layer: the substrate is introduced into an organic cavity of micromolecule evaporation equipment to deposit micromolecule HTLs, and the method specifically comprises the following steps: when the air pressure in the cavity is reduced to 1 x 10-4After Pa, TCTA was evaporated at 220 ℃ to a final thickness of 60 nm.
(5) After HTL deposition, the substrate is integrally transferred to a metal cavity from a mask plate to be evaporated with molybdenum oxide (MoO)3). The evaporation rate of the molybdenum oxide is controlled to be 0.01-0.1 nm/s, and the final thickness is about 8 nm.
(6) And transferring the substrate which is evaporated with the HIL from the micromolecule evaporation equipment to an Edward evaporation cavity to deposit a metal aluminum electrode (Al). The air pressure in the vacuum chamber is reduced to 5 x 10-4After Pa, evaporation was started. The evaporation rate of 10nm before the aluminum electrode is controlled to be 0.01-0.03 nm/s, and then the evaporation rate is controlled to be 0.1-0.3 nm/s until the final thickness is about 100 nm.
(7) And (3) dropwise adding a proper amount of epoxy resin on the device with the metal electrode evaporated, then covering a glass cover plate, slightly pressing the glass cover plate to enable the epoxy resin to completely cover the device, adjusting the glass cover plate to just cover the device, and finally placing the device in ultraviolet curing equipment for exposure for 5 minutes to enable the epoxy resin to be completely cured.
The maximum current efficiency was measured to be 3.7cd/A and the maximum luminance was measured to be 3840cd/m using the silicon photodiode highlighting photometer calibration test protocol2。
Example 2
The difference from example 1 is that: and (4) dissolving the quantum dots in chlorobenzene in the step (3), wherein the mass concentration of the solution is 20 mg/ml.
The maximum current efficiency and the maximum brightness of the test scheme are measured to be 4.0cd/A and 6234cd/m respectively by adopting the silicon photodiode and the brightness meter for calibration2。
Example 3
The difference from example 1 is that: the ZnO film was prepared by vacuum deposition (Edwards, UK, Metal vacuum deposition System Auto 500 System).
The maximum current efficiency was measured to be 4.2cd/A and the maximum brightness was 8921cd/m using a silicon photodiode highlighting photometer calibration test protocol2。
Example 4
The difference from example 1 is that: the voltage of the printer was 1500V, the moving speed was 10mm/s, and the resulting quantum dot arrays were 14.80um and 3.94um in diameter and spacing.
The maximum current efficiency was measured to be 4.3cd/A and the maximum luminance was measured to be 9573cd/m using a silicon photodiode highlighting photometer calibration test protocol2。
Comparative example 1
The difference from embodiment 1 is that: the ITO electrode substrate is patterned, wherein the size of a pixel groove on the substrate is 250um to 50um, and the quantum dot light-emitting layer is printed in an ink-jet printing mode. But the upper layer and the lower layer in the manufactured QLED device have the problems of mutual dissolution and permeation.
The maximum current efficiency was 2.8cd/A and the maximum luminance was 2507cd/m using the test protocol for silicon photodiode highlighting photometer calibration2。
The method for printing the quantum dot layer by the electrofluid is simple in preparation process. The method is beneficial to printing and preparing the micro-nano structure, so that the lower limit of ink jet printing and transfer printing technology can be broken through, and the resolution of the device is successfully improved. Meanwhile, the brightness of the device can be customized by controlling the process parameters, and the device has low brightness and relatively soft visual light as in example 1. Example 4 the device was bright and visually the light was relatively bright. Therefore, the electrofluid printing preparation method has adjustable device brightness and wide application scenes.
In addition, the devices printed by electrofluid keep high current efficiency. The reduction of the pixel point size is beneficial to relieving the problem of mutual dissolution between the upper layer and the lower layer in the QLED device prepared by the solution method in the prior art, so that the QLED device with stable performance is obtained.
Comparing example 1 with comparative example 1, and with the quantum dot array topography of fig. 2, it can be seen that compared with the inkjet printing technology, the deposition of the pixel points by electrofluid printing does not need to prepare a substrate with patterned pixel pits in advance, thereby saving the preparation cost. Meanwhile, the pixel point size of electrofluid printing is small, the coffee ring effect of printing is inhibited, and high-quality printing is realized. If the quantum dot solution in the embodiment is replaced by other quantum dot solutions, the preparation of the full-color device can be realized.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a QLED device based on an electrofluid printed quantum dot light-emitting layer is characterized by comprising the following steps:
(1) preparing a metal oxide film on an ITO glass substrate electrode as an electron transmission layer;
(2) printing a quantum dot array on the electron transport layer by adopting electrofluid printing, wherein the quantum dot array is printed by adopting a quantum dot solution and serves as a light emitting layer; wherein the diameter of the quantum dot array is 0.5-20 um, and the interval is 2-15 um;
(3) depositing a hole transport layer on the light emitting layer;
(4) depositing a hole injection layer on the hole transport layer;
(5) and evaporating a metal electrode on the hole injection layer to be used as a top electrode to obtain the QLED device.
2. The method for preparing a QLED device based on electrofluid printing of a quantum dot light-emitting layer according to claim 1, wherein the parameters of the electrofluid printing in the step (2): the voltage is 200-1200V, the voltage frequency is 100-1500 Hz, the voltage waveform is any one of square waves, triangular waves and sine waves, and the moving speed is 5-50 mm/s.
3. The preparation method of the QLED device based on the electrofluid printed quantum dot light-emitting layer according to claim 1, wherein the concentration of the quantum dot solution in the step (2) is 10-20 mg/mL, and the solvent is at least one of n-hexane, chloroform, chlorobenzene and toluene.
4. The method for preparing a QLED device based on electrofluid printed quantum dot light emitting layer according to claim 1, wherein the metal oxide materials in the step (1) are ZnO nanoparticles, ZnO nanoparticles doped with metal cations and TiO2At least one of nanoparticles;
the quantum dot material in the quantum dot solution in the step (2) is at least one of cadmium quantum dots, indium phosphide quantum dots, zinc selenide quantum dots and lead sulfide quantum dots;
the material of the HTL functional layer in the step (3) is at least one of 4,4, 4-tri (carbazole-9-yl) triphenylamine, N ' -di (naphthalene-1-yl) -N, N ' -di (phenyl) benzidine and 4,4' -di (9-carbazole) biphenyl;
the HIL functional layer material in the step (4) is at least one of polymer PEDOT, PSS, molybdenum oxide, nickel oxide and cuprous thiocyanate;
and (5) enabling the top electrode to be one of Al, Ag, Cu, Au or an alloy electrode, wherein the alloy is an alloy of at least two elements of Al, Ag, Cu and Au.
5. The method for preparing a QLED device based on electrofluid printed quantum dot light emitting layer according to claim 1, wherein the metal oxide thin film prepared in the step (1) is at least one of spin coating, vacuum evaporation and vacuum sputtering;
and (4) performing at least one of vacuum evaporation and spin coating on the substrate by the deposition process.
6. The method for preparing a QLED device based on electrofluid printed quantum dot light-emitting layer according to claim 3 or 5, characterized in that, the method for preparing the metal oxide film in the step (1) is vacuum evaporation;
the diameter of the quantum dot array in the step (2) is 2.88-14.80 um, and the interval is 3.94-10.79 um;
the solvent of the quantum dot solution in the step (2) is at least one of chlorobenzene and toluene
And (4) performing vacuum evaporation on the deposition processes in the steps.
7. The preparation method of the QLED device based on the electrofluid printed quantum dot light-emitting layer according to claim 1, characterized in that the thickness of the metal oxide thin film in the step (1) is 100-300 nm;
the thickness of the hole transport layer in the step (3) is 20-60 nm;
the thickness of the hole injection layer in the step (4) is 5-10 nm;
and (5) the thickness of the top electrode is 100-300 nm.
8. The preparation method of the QLED device based on the electrofluid printed quantum dot light emitting layer according to claim 1, characterized in that the quantum dot array obtained by the electrofluid printing in the step (2) is further subjected to annealing and curing to obtain the light emitting layer, wherein the annealing temperature is 50-150 ℃, and the curing time is 10-30 min.
9. The preparation method of the QLED device based on the electrofluid printed quantum dot light emitting layer according to claim 1, characterized in that the ITO glass substrate electrode in the step (1) is further subjected to cleaning treatment before use, and the cleaning treatment comprises the step of ultrasonically oscillating the substrate electrode material for 5-10 min by using isopropanol, tetrahydrofuran, alkaline cleaning solution, deionized water and isopropanol in sequence;
and (5) after the top electrode is prepared, packaging to obtain the QLED device.
10. A QLED device based on an electrofluid printed quantum dot light emitting layer made by the method of any one of claims 1 to 9.
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Application publication date: 20210817 |