CN109449316B - In-doped MoO3Method for producing thin film - Google Patents

In-doped MoO3Method for producing thin film Download PDF

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CN109449316B
CN109449316B CN201811308855.5A CN201811308855A CN109449316B CN 109449316 B CN109449316 B CN 109449316B CN 201811308855 A CN201811308855 A CN 201811308855A CN 109449316 B CN109449316 B CN 109449316B
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moo
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indium
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CN109449316A (en
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王宇
曹蔚然
杨一行
钱磊
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TCL Research America Inc
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    • H—ELECTRICITY
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    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/14—Carrier transporting layers
    • H10K50/15—Hole transporting layers
    • H10K50/155—Hole transporting layers comprising dopants
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    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/17—Carrier injection layers
    • 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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    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract

The invention provides In-doped MoO3A method for preparing a film. The In-doped MoO3The preparation method of the film comprises the following steps: providing indium salts and MoO3Mixing the indium salt and MoO3Dissolving the mixed solution in an organic solvent to form a mixed solution, and adding an inorganic acid into the mixed solution to perform heating treatment to obtain a precursor solution, wherein the heating treatment temperature is 50-80 ℃; providing a substrate, depositing the precursor solution on the substrate by adopting a solution processing method, and then carrying out annealing treatment to obtain In-doped MoO3And the annealing temperature is 150-350 ℃.

Description

In-doped MoO3Method for producing thin film
Technical Field
The invention belongs to the technical field of flat panel display, and particularly relates to In-doped MoO3A method for preparing a film.
Background
In recent years, quantum dot light emitting diodes (QLEDs) using quantum dot materials as light emitting layers have attracted much attention due to their advantages such as high color purity, high light emission quantum efficiency, adjustable light emission color, and long service life, and are currently the main direction of research on new LEDs. Existing QLEDs typically include an anode, a hole injection layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, and a cathode. The hole injection layer is used as a functional layer, and can reduce the injection barrier of holes, so that the carrier migration efficiency is improved.
The polymer material is PEDOT (poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid), which has the advantages of high light transmittance, high work function, flat appearance, good conductivity and the like, and is widely used as a hole injection layer material of the QLED. By adopting PEDOT and PSS to modify ITO, the work function and the flatness of the film can be improved. However, a great deal of research data shows that PEDT PSS has the characteristics of acidity and water absorption, so that the PEDOT PSS serving as a hole injection layer material can corrode ITO and further adversely affect the stability of a QLED device. To solve this problem, researchers have replaced PEDOT with metal oxides such as V2O5、WO3NiO, and MoO3And the like. Wherein, MoO3The material has the advantages of no toxicity, a relatively deep energy level structure, a wide band gap, good electronic barrier property and the like, and becomes a substitute material of PEDOT and PSS. Currently, there have been reports of using molybdenum oxide as a hole injection layer, applied to OPVs and OLEDs. However, since the resistance value of molybdenum oxide itself is high, it affects the charge transfer and injection of the QLED. In order to overcome the problem of too high resistance of molybdenum oxide, researchers have attempted to modify the resistance and transmittance of molybdenum oxide by In-doping the molybdenum oxide by mixing powders of molybdenum oxide and indium oxide and then calcining them In a muffle furnace at high temperatures up to 950 ℃. Obviously, this high temperature calcination approach is not suitable for the preparation of QLED functional layers. Therefore, it is an urgent problem to find a method suitable for QLED, with adjustable work function, and low temperature preparation of In-doped molybdenum oxide.
Disclosure of Invention
The invention aims to provide In-doped MoO3The preparation method of the film aims at solving the problem that the transmission and injection of charges are influenced by the overhigh resistance value of molybdenum oxide and the existing In-doped MoO3The preparation method needs high-temperature calcination and is not suitable for preparing the QLED hole injection layer.
Another object of the present invention is to provide a hole injection layer of In-doped MoO3Thin film QLED.
It is another object of the present invention to provide a hole injection layer of In-doped MoO3A preparation method of a thin film QLED.
The invention is realized by that In is doped with MoO3The preparation method of the film comprises the following steps:
providing indium salts and MoO3Mixing the indium salt and MoO3Dissolving the mixed solution in an organic solvent to form a mixed solution, and adding an inorganic acid into the mixed solution to perform heating treatment to obtain a precursor solution, wherein the heating treatment temperature is 50-80 ℃;
providing a substrate, depositing the precursor solution on the substrate by adopting a solution processing method, and then carrying out annealing treatment to obtain In-doped MoO3And the annealing temperature is 150-350 ℃.
Is different from the preparation of In-doped MoO by high-temperature calcination3Powder mode, In-doped MoO provided by the embodiment of the invention3The preparation method of the film adopts a low-temperature method to prepare In-doped MoO3The thin film can be used for forming a hole injection layer in the QLED, and is particularly suitable for preparing the QLED hole injection layer based on an ITO substrate. In-doped MoO prepared by the method of the embodiment of the invention3The film effectively reduces the resistance of the molybdenum oxide and improves the charge transmission by changing the doping proportion of indium on the premise of ensuring that the molybdenum oxide crystal lattice does not change; meanwhile, by changing the doping proportion of indium, the work function of molybdenum oxide can be changed, so that the molybdenum oxide has better energy level matching and applicability, the injection barrier of carriers is reduced, the injection capacity of the carriers is improved, the electron and hole are well balanced and compounded, and the efficiency of the device is improved.
Drawings
FIG. 1 shows an In-doped MoO according to an embodiment of the present invention3A schematic diagram of a preparation method of the film;
FIG. 2 shows an In-doped hole injection layer according to an embodiment of the present inventionMoO3QLED structure schematic diagram of thin film.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
With reference to fig. 1, an embodiment of the present invention provides an In-doped MoO3The preparation method of the film comprises the following steps:
s01, providing indium salt and MoO3Mixing the indium salt and MoO3Dissolving the mixed solution in an organic solvent to form a mixed solution, and adding an inorganic acid into the mixed solution to perform heating treatment to obtain a precursor solution, wherein the heating treatment temperature is 50-80 ℃;
s02, providing a substrate, depositing the precursor solution on the substrate by adopting a solution processing method, and then annealing to obtain In-doped MoO3And the annealing temperature is 150-350 ℃.
Specifically, In the step S01, In-doped MoO is obtained for preparation3The film is provided with a doping source indium salt. As a preferred embodiment, the indium salt is In (NO)3)3·H2O、InCl3·4H2At least one of O. The optimized indium salt can realize high-efficiency doping under the low-temperature condition of the embodiment of the invention without high-temperature treatment, so that In-doped MoO with better performance and capable of being used for QLED film forming is obtained3A film.
Due to said indium salts, e.g. In (NO)3)3·H2O、InCl3·4H2O is hydrolyzed in water to affect doping, and thus, the indium salt and MoO are dissolved in the examples of the present invention3The solvent of (a) is a non-aqueous solvent. The organic solvent only needs to be satisfied to well realize the indium salt and MoO3And (3) dissolving. As a preferred embodiment, the organic solvent is dimethoxyethanol. The preferred organic solvent can be used simultaneouslySufficiently dissolving the indium salt and MoO3And prevent the indium salt from hydrolyzing.
Mixing the indium salt and MoO3The form of dissolving in the organic solvent to form a mixed solution is not limited, and the indium salt and MoO may be3After mixing, dissolving the mixture in the organic solvent to form a mixed solution; the indium salt and MoO may also be used3Respectively dissolving the components in the organic solvent and mixing to form a mixed solution.
In the mixed solution of the embodiment of the invention, the MoO3The mass percentage concentration of the compound has great influence on the performance of the compound after film forming and film forming. In particular, if said MoO3If the mass percentage concentration of (b) is too low, it is difficult to function as a hole injection layer; if MoO3If the mass percentage concentration of (a) is too high, the viscosity of the mixed solution is too high to uniformly form a film. As a preferred embodiment, in the mixed solution, the MoO3The mass percentage concentration of the active carbon is 0.02-5%.
In the embodiment of the invention, the mol percentage of indium is equal to the obtained In-doped MoO3The film properties are greatly affected. Specifically, if the molar percentage of indium is too low, the resulting doped thin film has a limited decrease in resistance, and the hole injection level cannot be significantly increased; if the mole percentage of the indium is too high, that is, the doped indium is too much, the molybdenum oxide lattice may be changed and deformed, and the performance of the molybdenum oxide lattice may be affected, and the molybdenum oxide lattice cannot be used as a hole injection material. As a preferred embodiment, the mol percent of the indium in the mixed solution is 1-15% based on the total mol content of the indium and the molybdenum as 100%. According to the embodiment of the invention, the electric conductivity of the molybdenum oxide can be improved by adjusting the mol percentage content of the indium and reducing the resistance of the molybdenum oxide, so that the charge injection capability of the molybdenum oxide can be improved; in addition, by adjusting the doping proportion of the indium, the work function of the molybdenum oxide can be adjusted and controlled within a certain range, and the injection barrier of carriers is reduced. As a specific example, the mole percent of indium is 7.5% based on 100% total mole content of indium and molybdenum.
In the embodiment of the invention, in order to prevent the indium salt from being inHydrolysis occurs during the heating process, and inorganic acid is dropped into the mixed solution. In a preferred embodiment, the inorganic acid is one of hydrochloric acid and nitric acid. As a specific example, when the indium salt is In (NO)3)3·H2When O is generated, dropwise adding nitric acid; as another preferred embodiment, when the indium salt is InCl3·4H2And when O is generated, hydrochloric acid is added dropwise.
In the embodiment of the invention, in order to prevent the reaction liquid from being adversely affected by water vapor, the heating is preferably carried out by adopting an oil bath heating mode. The oil bath heating mode can not only avoid indium salt hydrolysis caused by the introduction of water vapor, but also provide a mild heating condition, so that the mixed solution is heated uniformly. Specifically, the temperature of the heat treatment in the embodiment of the invention is 50-80 ℃. If the temperature is too high, the organic solvent such as dimethoxyethanol solution volatilizes, so that the viscosity of the mixed solution is too high and the uniform film formation is difficult; if the temperature is too low, it is difficult to realize the indium salt and MoO3And (4) uniformly mixing. The heating time is 50-70min, specifically 60 min. After being mixed by adopting a low-temperature heating mode, In-doped MoO can be obtained3Precursor solution of the film.
In the step S02, the precursor solution is deposited on the substrate by a solution processing method, where the solution processing method includes spin coating, drop coating, dipping, and the like. Because the In-doped MoO is adopted In the embodiment of the invention3When the film is used for preparing a QLED hole injection layer, other functional layers and electrodes are prepared on the hole injection layer, so that the thin and flat hole injection layer is beneficial to the preparation of a subsequent layer structure. In-doped MoO for obtaining thin and flat3The solution processing method of the thin film according to the embodiment of the present invention is preferably a spin coating method. When the In-doped MoO is prepared by the spin coating method3When the film is formed, the In-doped MoO can be controlled by adjusting the rotating speed3The thickness of the film. As a preferred embodiment, the spin coating speed is 2000-6000rpm, thereby obtaining a suitable In-doped MoO3The thickness of the film.
Embodiments of the invention the deposition of the coating on the substrateAnd annealing the precursor solution, wherein the annealing temperature is specifically 150-350 ℃. Preferably, the time of the annealing treatment is 15-30 min. The annealing treatment can remove the organic solvent and realize the doping of the indium in the molybdenum oxide structure. As a specific example, the annealing temperature is 250 ℃ and the time is 30 min. The annealing treatment according to the embodiment of the present invention may be performed in air or in an inert atmosphere such as nitrogen. Of course, different annealing atmospheres can result In the In doped MoO having different performance differences3A film.
As a preferred embodiment of the present invention, InCl is used3·4H2O as an indium salt, 0.0220g of the InCl3·4H2O and 0.144g of said MoO3Dissolving the mixture in dimethoxyethanol to prepare a mixed solution, wherein the mol percentage of indium is 7.5 percent based on the total mol content of indium and molybdenum as 100 percent. And dropwise adding two drops of hydrochloric acid into the mixed solution, and then heating and stirring in an oil bath at the temperature of 80 ℃ for 1h to obtain a precursor solution. Depositing the precursor solution on an ITO substrate by using a spin coating method, and heating and annealing at 250 ℃ for 30min to prepare In-doped MoO3A film.
Is different from the preparation of In-doped MoO by high-temperature calcination3Powder mode, In-doped MoO provided by the embodiment of the invention3The preparation method of the film adopts a low-temperature method to prepare In-doped MoO3The thin film can be used for forming a hole injection layer in the QLED, and is particularly suitable for preparing the QLED hole injection layer based on an ITO substrate. In-doped MoO prepared by the method of the embodiment of the invention3The film effectively reduces the resistance of the molybdenum oxide and improves the charge transmission by changing the doping proportion of indium on the premise of ensuring that the molybdenum oxide crystal lattice does not change; meanwhile, by changing the doping proportion of indium, the work function of molybdenum oxide can be changed, so that the molybdenum oxide has better energy level matching and applicability, the injection barrier of carriers is reduced, the injection capacity of the carriers is improved, the electron and hole are well balanced and compounded, and the efficiency of the device is improved.
And, with reference to FIG. 2, the practice of the inventionThe embodiment provides a QLED, which comprises an anode 1, a hole injection layer 2, a quantum dot light-emitting layer 4 and a cathode 6 which are sequentially stacked, wherein the hole injection layer 2 is In-doped MoO prepared by the method3A film.
Further, in order to improve the carrier mobility of the QLED, as a preferred embodiment, the QLED further includes at least one of a hole transport layer 3, an electron transport layer 5, and an electron injection layer (not shown).
As a preferred embodiment, as shown In fig. 2, the QLED includes an anode 1, a hole injection layer 2, a hole transport layer 3, a quantum dot light emitting layer 4, an electron transport layer 5 and a cathode 6, which are sequentially stacked, wherein the hole injection layer 2 is an In-doped MoO prepared by the above method3A film.
Specifically, the anode 1 may be disposed on a substrate 0, and the substrate 0 may be a substrate conventional in the art, such as a glass substrate. The anode 1 may be patterned ITO.
The hole injection layer 2 In the embodiment of the invention is In-doped MoO prepared by the method3A film. As a preferred embodiment, the thickness of the hole injection layer is 5-20nm, and if the thickness is too high, the resistance of the QLED device itself is too large, which is not favorable for injecting holes, and thus the efficiency of the QLED device is reduced; if the thickness is too thin, it is difficult to achieve full coverage of the ITO substrate, resulting in formation of a rough thin film, which is likely to cause defects, and thus, the efficiency of the device is reduced.
The hole transport layer 3 may be made of at least one of TFB, PVK, Poly-TPD, TCTA, and CBP, or may be made of other high-performance hole transport materials. The quantum dot light-emitting layer 4 can be made of a cadmium-containing or cadmium-free quantum dot material. The electron transport layer 5 can be made of n-type ZnO with high electron transport performance, can also be made of metal materials such as Ca, Ba and the like with low work function, and can also be made of CsF, LiF and CsCO3And Alq3And (e) a compound material. The electron injection layer may be made of an electron injection material that is conventional in the art. The cathode 6 can be prepared from metal silver and aluminum.
In-doped MoO prepared by the method is adopted In the QLED provided by the embodiment of the invention3The film is used as a hole injection layer, and therefore, has better energy level matching and applicability. In particular, In-doped MoO3The film can effectively reduce a hole injection barrier, so that electrons and holes are combined in a better balance mode, and the efficiency of the QLED device is improved.
The QLED provided by the embodiment of the invention can be prepared by the following method.
Correspondingly, the embodiment of the invention provides a preparation method of a QLED, which comprises the following steps:
providing an ITO substrate, and cleaning the ITO substrate;
q02. depositing In-doped MoO on the ITO substrate according to the method3A thin film forming a hole injection layer;
and Q03, sequentially preparing a quantum dot light-emitting layer and a cathode on the hole injection layer.
Specifically, in the step Q01, the ITO substrate is a patterned ITO substrate. In order to improve the work function of the ITO and facilitate the preparation of the hole injection layer, the ITO substrate is cleaned before depositing a hole injection material. As a specific example, the cleaning treatment may be performed by the following method:
wiping the patterned ITO substrate by using dry dust-free cloth and wet dust-free cloth in sequence to remove large dust and particles on the surface;
then, sequentially placing the ITO substrate in a cleaning solution, ultrapure water, acetone water and isopropanol for ultrasonic cleaning, wherein the ultrasonic time is 10-20min, specifically 15 min;
and after the ultrasonic treatment is finished, drying the ITO substrate, and specifically, placing the ITO substrate in a clean oven for drying for later use.
Further, in order to further remove organic substances attached to the surface of the ITO substrate and increase the work function of ITO, as a preferred embodiment, the cleaning process includes performing an ultraviolet ozone treatment or an oxygen plasma treatment on the ITO substrate. As a specific example, the ITO substrate is treated with the ultraviolet ozone for 15 min.
In the step Q02, In-doped MoO is deposited on the ITO substrate3The method of film is described above and will not be described herein for brevity.
In the step Q03, a quantum dot light-emitting layer and a cathode are sequentially prepared on the hole injection layer to obtain a QLED, and further preferably, a hole transport layer is prepared on the hole injection layer before the quantum dot light-emitting layer is prepared; and/or preparing an electron transport layer and/or an electron injection layer on the quantum dot light emitting layer before preparing the cathode.
The preparation of the hole transport layer can be accomplished in a manner conventional in the art. As a specific example, the ITO substrate deposited with the composite hole injection layer is transferred into a glove box filled with nitrogen, wherein the oxygen content and the water content of the glove box are both lower than 0.1ppm, and a hole transport material is deposited by a spin coating method; the ITO substrate on which the hole injection material is deposited is subjected to a heating process on a heating plate to remove the solvent and to effect crosslinking of the layer, so as to facilitate deposition of quantum dots as described below.
The preparation of the quantum dot light emitting layer can be realized by adopting a conventional mode in the field. The quantum dot material comprises any one of common red, green and blue, and other quantum dots such as yellow quantum dots can also be selected. When the quantum dot light-emitting layer is prepared, whether heating treatment is carried out or not is selected according to the property of the quantum dot material, and the quantum dot material which is quenched by heating is not subjected to heating treatment.
The hole transport layer and/or the hole injection layer may be prepared using methods conventional in the art.
And placing the ITO substrate with the prepared functional layers in an evaporation chamber, and thermally evaporating a cathode through a mask plate.
Further, in order to prevent the influence of penetration of water and oxygen on the performance of the QLED, as a preferred embodiment, the cathode is subjected to a sealing treatment after deposition. The encapsulation process can be performed using conventional machine encapsulation or can be performed using simple manual encapsulation. Specifically, the packaging treatment is carried out in an atmosphere with both oxygen content and water content lower than 0.1ppm, so as to protect the stability of the device.
According to the preparation method of the QLED provided by the embodiment of the invention, In-doped MoO can be realized In a low-temperature heating mode3And the preparation of the thin film endows the hole injection layer with excellent charge injection performance, thereby improving the efficiency of the QLED device. In addition, the preparation method of the QLED is simple and reliable in process, and industrial production can be realized.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (9)

1. In-doped MoO3The preparation method of the film comprises the following steps:
providing indium salts and MoO3Mixing the indium salt and MoO3Dissolving the indium salt in an organic solvent to form a mixed solution, and adding an inorganic acid into the mixed solution and then performing heating treatment to obtain a precursor solution, wherein the inorganic acid is used for preventing the indium salt from hydrolyzing; the temperature of the heating treatment is 50-80 ℃, and the MoO is added into the mixed solution3The mass percentage concentration of the active carbon is 0.02-5%;
providing a substrate, depositing the precursor solution on the substrate by adopting a solution processing method, and then carrying out annealing treatment to obtain In-doped MoO3And the temperature of the annealing treatment is 150-350 ℃.
2. The In-doped MoO of claim 13The preparation method of the film is characterized in that the annealing treatment time is 15-30 min.
3. The In-doped MoO of claim 13The preparation method of the film is characterized In that the indium salt is In (NO)3)3·H2O、InCl3·4H2At least one of O; and/or
The organic solvent is dimethoxyethanol.
4. The In-doped MoO of claim 33The preparation method of the film is characterized in that the inorganic acid is one of hydrochloric acid and nitric acid.
5. The In-doped MoO of claim 43A method for producing a thin film, characterized in that the indium salt and MoO are mixed3Dissolving In organic solvent to form mixed solution, and adding inorganic acid into the mixed solution to obtain indium salt In (NO)3)3·H2And O, wherein the inorganic acid is nitric acid.
6. The In-doped MoO of claim 43A method for producing a thin film, characterized in that the indium salt and MoO are mixed3Dissolving the indium salt in an organic solvent to form a mixed solution, and adding an inorganic acid into the mixed solution, wherein the indium salt is InCl3·4H2And O, wherein the inorganic acid is hydrochloric acid.
7. The In-doped MoO of any of claims 1 to 63The preparation method of the thin film is characterized in that the mol percentage of indium in the mixed solution is 1-15% based on the total mol content of indium and molybdenum as 100%.
8. The In-doped MoO of any of claims 1 to 63The method for producing a film is characterized in that the heating treatment is carried out by an oil bath heating method.
9. The In-doped MoO of any of claims 1 to 63A method for preparing a thin film, wherein the solution processing method is one selected from spin coating, drop coating and dipping methods.
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