CN109980107B - CuMO2Preparation method thereof and light-emitting device - Google Patents
CuMO2Preparation method thereof and light-emitting device Download PDFInfo
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- CN109980107B CN109980107B CN201711464350.3A CN201711464350A CN109980107B CN 109980107 B CN109980107 B CN 109980107B CN 201711464350 A CN201711464350 A CN 201711464350A CN 109980107 B CN109980107 B CN 109980107B
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Abstract
The invention provides a CuMO2The preparation method comprises the following steps: providing a cupric salt solution, adding a reducing agent into the cupric salt solution under an inert atmosphere, and generating cuprous ions by the cupric ions in the cupric salt under the action of the reducing agent to obtain a cuprous ion solution; providing an aqueous solution of a salt of M, wherein M is selected from one of Ga, In, Cr and Al, and the pH value of the aqueous solution of the salt of M is 5-6.5; adding the M salt solution into the cuprous ion solution under inert atmosphere, and heating to react to generate CuMO2。
Description
Technical Field
The invention belongs to the technical field of display, and particularly relates to a CuMO2And a method of manufacturing the same, and a light emitting device.
Background
The quantum dot light emitting diode (QLED) has the excellent characteristics of narrow FWHM (full width at half maximum), adjustable color, solution-based preparation and the like, so that it becomes a candidate for next generation display technology. Therefore, different researchers have studied QLEDs from different angles, including studies of QDs (quantum dots), HTL (hole transport layer), ETL (electron transport layer), and electrodes; there are also studies on the structure, performance and stability of the device, and one of the most commercially interesting points in these studies is the stability of the device. In the current QLED device, the acidity and hydroscopicity of the PEDOT/PSS hole injection layer cause damage and attenuation to ITO and the device to different degrees, so that the stability of the device is still to be improved. At the present time replacing PEODT: in the report of PSS, the most used is metal oxide, the materials used for the hole transport layer are limited at present, and the metal oxide having a better hole transport material is not much, mainly binary compound, and is mainly represented by a material concentrated in molybdenum oxide, nickel oxide or copper oxide. Therefore, metal oxide materials having better hole transport properties are under further development.
Disclosure of Invention
The invention aims to provide a CuMO2And a preparation method thereof, aiming at providing a ternary metal oxide material which has better hole transmission performance and can be used for a light-emitting device.
The object of the present invention is to provideA food containing CuMO2The light emitting device of (1).
In order to achieve the purpose, the invention adopts the following technical scheme:
CuMO2The preparation method comprises the following steps:
providing a cupric salt solution, adding a reducing agent into the cupric salt solution under an inert atmosphere, and generating cuprous ions by the cupric ions in the cupric salt under the action of the reducing agent to obtain a cuprous ion solution;
providing an aqueous solution of a salt of M, wherein M is selected from one of Ga, In, Cr and Al, and the pH value of the aqueous solution of the salt of M is 5-6.5; adding the M salt solution into the cuprous ion solution under inert atmosphere, and heating to react to generate CuMO2。
Accordingly, a CuMO2Said CuMO2CuMO prepared for the above process2。
And, a light-emitting device, including positive pole and negative pole, and set up in the positive pole with the lamination between the negative pole, the lamination includes the hole transport layer and luminescent layer of lamination combination, the hole transport layer is set up in the positive pole with between the luminescent layer, and the material of the hole transport layer is the CuMO prepared by above-mentioned method2Wherein M is selected from one of Ga, In, Cr and Al.
The CuMO provided by the invention2The preparation method adopts a solution method, reduces divalent copper ions into cuprous ions, and then the cuprous ions are mixed with an M salt water solution for reaction to prepare CuMO2. The method has mild reaction conditions, and the prepared CuMO2The material has good dispersion performance and can be used as a hole transport layer material of a light-emitting device. Furthermore, when the material is used as a hole transport layer material, the material can be directly prepared on a functional layer or an electrode of a light-emitting device in situ, and the stability of the hole transport layer is improved.
The CuMO provided by the invention2Not only has excellent optical transmittance, but also has a proper energy level structure (the conduction band energy level is about-5.3 eV, which is beneficial to the injection of holes) and higher hole mobility (10)-2-101cm2V-1s-1) When the hole transporting layer is used as a hole transporting layer of a light-emitting device, the mobility of carriers can be improved, the hole injecting capability is mainly improved, and the injection and the transmission of holes and electrons are further balanced. In addition, the CuMO is used2Has better stability, so when the material is used as a light-emitting device, the stability of the device can be improved.
The light-emitting device provided by the invention adopts CuMO2As a hole transport layer, the material not only has better hole transport and injection performance, improves the carrier mobility, but also can improve the stability of the device.
Drawings
Fig. 1 is a schematic structural diagram of a positive type QLED device provided in an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an inversion-type QLED device provided in an embodiment of the present invention.
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.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The embodiment of the invention provides a CuMO2The preparation method comprises the following steps:
s01, providing a cupric salt solution, adding a reducing agent into the cupric salt solution under an inert atmosphere, and generating cuprous ions by the cupric ions in the cupric salt under the action of the reducing agent to obtain a cuprous ion solution;
s02, providing an M salt water solution, wherein M is selected from one of Ga, In, Cr and Al, and the pH value of the M salt water solution is 5-6.5; adding the M salt solution into the cuprous ion solution under inert atmosphere, and heating to react to generate CuMO2。
The CuMO provided by the embodiment of the invention2The preparation method adopts a solution method, reduces divalent copper ions into cuprous ions, and then the cuprous ions are mixed with an M salt water solution for reaction to prepare CuMO2. The method has mild reaction conditions, and the prepared CuMO2The material has good dispersion performance and can be used as a hole transport layer material of a light-emitting device. Furthermore, when the material is used as a hole transport layer material, the material can be directly prepared on a functional layer or an electrode of a light-emitting device in situ, and the stability of the hole transport layer is improved.
Specifically, in step S01, the cupric salt in the cupric salt solution is a cupric salt soluble in water, including but not limited to cupric chloride, cupric sulfate, etc., but copper nitrate is not used, so as to avoid nitrate from oxidizing the cuprous ions obtained subsequently. In the embodiment of the invention, the reducing agent is a weak reducing agent so as to avoid that the reducing agent directly reduces bivalent copper ions into a simple metal copper substance. Preferably, the reducing agent is at least one selected from sodium thiosulfate and sodium citrate. Compared with ethylene glycol serving as a reducing agent and the like, the copper-free composite material is green and environment-friendly, has no biological toxicity, can be used in an aqueous phase reaction system, can effectively improve the oxidation-reduction reaction efficiency with bivalent copper ions, and controls the reduction degree of the bivalent copper ions to be limited to formation of cuprous ions rather than reduction to metallic copper simple substances.
In the embodiment of the invention, the reducing agent can be directly added into the cupric salt solution, or the cupric salt solution and the reducing agent solution can be respectively provided and then mixed to obtain the mixed reaction system. The reaction of generating cuprous ions by copper ions in the cupric salt under the action of the reducing agent is carried out in the inert atmosphere. Specifically, when the reducing agent is directly added into the cupric salt solution, the oxygen of the cupric salt solution can be exhausted in an inert gas mode; then, an inert atmosphere is maintained and a reducing agent is added. When the cupric salt solution and the reducing agent solution are respectively provided and then mixed to obtain a mixed reaction system, the oxygen in the cupric salt solution and the oxygen in the reducing agent solution can be respectively exhausted in an inert gas mode, and then the inert atmosphere is kept to mix the cupric salt solution and the reducing agent solution.
In step S02, the M salt in the M salt water solution is a water-soluble M salt, including but not limited to chloride, acetate, etc., and is not a nitrate of M, so as to avoid the nitrate ions oxidizing the cuprous ions. Providing an aqueous solution of a salt of M, M being selected from one of Ga, In, Cr, Al, whereby M ions form [ M (OH)4(H2O)2]-Or M (OH)3.3H2And O. Due to [ M (OH)4(H2O)2]-Or M (OH)3.3H2O is a strong acid weak base salt, and thus, to avoid hydrolysis, the pH of the aqueous M salt solution is 5 to 6.5.
Further, adding the M salt solution into the cuprous ion solution under inert atmosphere, and heating for reaction to generate CuMO2The reaction process is as follows: cu1++[M(OH)4(H2O)2]-→CuMO2+H2O or Cu1++[M(OH)3(H2O)3]0→CuMO2+H3O+。
In the embodiment of the invention, the M salt solution is added into the cuprous ion solution under inert atmosphere, and the CuMO is generated by heating reaction2In the step (2), the heating reaction temperature is 180-250 ℃, and the reaction time is 1-3 hours. If the reaction temperature is too low or the reaction time is too short, the reaction is insufficient, and CuMO cannot be obtained in a high yield2And CuMO2Other impurities are easily introduced, and the purity of the product is reduced. If the reaction temperature is too high or the reaction time is too long, on the one hand, CuMO is formed2The further reaction, such as decomposition reaction, is carried out, and the obtained product has substance attribute change; on the other hand, the CuMO produced2Too large a granule to be usedEffectively dispersed and used as a hole transport material.
Further, adding the M salt solution into the cuprous ion solution, and heating to react to generate CuMO2After the step (2), the obtained CuMO is also added2Carrying out cleaning treatment, wherein the cleaning treatment method comprises the following steps: sequentially adopting ammonia water, nitric acid and deionized water to carry out a reaction to obtain CuMO2Washing is carried out. Through this washing sequence, the weak acid remaining in the reaction system is neutralized by aqueous ammonia, and then other impurities generated in the reaction, such as cuprous oxide or copper, are dissolved by nitric acid, and further the salt formed by the dissolution of nitric acid is removed by water.
Further, the obtained CuMO can be used2Dispersed in an alcohol solution.
Correspondingly, the embodiment of the invention also provides a CuMO2Said CuMO2CuMO prepared for the above process2。
The CuMO provided by the embodiment of the invention2Not only has excellent optical transmittance, but also has a proper energy level structure (the conduction band energy level is about-5.3 eV, which is beneficial to the injection of holes) and higher hole mobility (10)-2-101cm2V-1s-1) When the hole transporting layer is used as a hole transporting layer of a light-emitting device, the mobility of carriers can be improved, the hole injecting capability is mainly improved, and the injection and the transmission of holes and electrons are further balanced. In addition, the CuMO is used2Has better stability, so when the material is used as a light-emitting device, the stability of the device can be improved.
And, a light-emitting device, including positive pole and negative pole, and set up in the positive pole with the lamination between the negative pole, the lamination includes the hole transport layer and luminescent layer of lamination combination, the hole transport layer is set up in the positive pole with between the luminescent layer, and the material of the hole transport layer is the CuMO prepared by above-mentioned method2Wherein M is selected from one of Ga, In, Cr and Al.
The light-emitting device provided by the embodiment of the invention adopts the CuMO2As a hole transport layer, the hole transport layerThe method has the advantages of good hole transmission and injection performance, carrier mobility improvement and device stability improvement.
The light-emitting device further comprises an electronic function layer, wherein the electronic function layer is at least one of an electron transport layer and an electron injection layer.
The light-emitting layer provided by the embodiment of the invention is a quantum dot light-emitting layer or an organic light-emitting layer. When the light-emitting layer is a quantum dot light-emitting layer, the light-emitting device is correspondingly a QLED device; when the light emitting layer is an organic layer, the light emitting device corresponds to an OLED (organic light emitting diode) device. Preferably, the light emitting device is a QLED device.
In the embodiment of the present invention, the QLED device may be a positive QLED device or an inverted QLED device. As a specific embodiment, as shown in fig. 1, the QLED device is a positive QLED device, and includes a substrate 1, an anode 2 bonded to a surface of the substrate 1, and a hole injection layer 3, a hole transport layer 4, a quantum dot light emitting layer 5, an electron transport layer 6, and a cathode 7 sequentially disposed on the anode 2. As another embodiment, as shown in fig. 2, the QLED device is an inverted QLED device, and includes a substrate 1, a cathode 7 standing on the surface of the substrate, and an electron transport layer 6, a quantum dot light emitting layer 5, a hole transport layer 4, a hole injection layer, and an anode 2 sequentially disposed on the surface of the cathode 7.
Specifically, the selection of the substrate 1 is not critical, and a hard substrate including, but not limited to, a glass plate or a flexible substrate may be used.
The anode 2 may be selected from doped metal oxides including, but not limited to, one or more of indium-doped tin oxide (ITO), fluorine-doped tin oxide (FTO), antimony-doped tin oxide (ATO), aluminum-doped zinc oxide (AZO), gallium-doped zinc oxide (GZO), indium-doped zinc oxide (IZO), magnesium-doped zinc oxide (MZO), aluminum-doped magnesium oxide (AMO), and may also be selected from a composite electrode sandwiching a metal between doped or undoped transparent metal oxides including, but not limited to, AZO/Ag/AZO, AZO/Al/AZO, ITO/Ag/ITO, ITO/Al/ITO, ZnO/Ag/ZnO, ZnO/Al/ZnO, TiO/Al/ITO, and/or Al/AZO, and may be selected from a group of doped or undoped transparent metal oxides2/Ag/TiO2、 TiO2/Al/TiO2One or more of ZnS/Ag/ZnS, ZnS/Al/ZnS.
The hole injection layer 3 may be NiO, CuO, CuS, MoO3Any one of the above; or at least one of TFB, PVK, Poly-TPD, TCTA and CBP.
The material of the hole transport layer 4 is the CuMO2Or CuMO2The conventional hole transport material can be any one of NiO, CuO and CuS; or at least one of TFB, PVK, Poly-TPD, TCTA and CBP. The thickness of the hole transport layer 4 is 20 to 30 nm. Too thin a hole transport layer 4 is less conductive and causes hole-electron imbalance; too large a thickness of the hole transport layer 4 is disadvantageous for hole transport into the light emitting layer.
The material of the quantum dot light-emitting layer 5 can be at least one of common red, green, blue and yellow light quanta and infrared and ultraviolet light quantum dots, and specifically can be one or more selected from II-VI compounds, III-V compounds, II-V compounds, III-VI compounds, IV-VI compounds, I-III-VI compounds, II-IV-VI compounds or IV elementary substances. The thickness of the quantum dot light-emitting layer 4 is 10-100 nm.
The electron transport layer 6 is a metal oxide having electron transport properties, such as TiO2、ZnO、SnO2And the like. The thickness of the electron transport layer 6 is 30 to 60 nm.
The cathode 7 may be made of metal or alloy such as Ag, Al, Cu, Au, etc.
Correspondingly, the embodiment of the invention also provides a preparation method of the QLED device.
As an embodiment, the method for manufacturing the QLED device includes the steps of:
E01. providing an anode substrate, and sequentially preparing a hole injection layer on the anode substrate;
E02. depositing CuMO on the hole injection layer2Preparing a hole transport layer;
E03. and sequentially preparing a quantum dot light-emitting layer, an electron transport layer and a cathode on the hole transport layer.
As another embodiment, the method for manufacturing a QLED device includes the steps of:
providing a cathode substrate, and sequentially preparing an electron transmission layer and a quantum dot light emitting layer on the cathode substrate;
preparing a hole transport layer on the quantum dot light emitting layer;
and Q03, sequentially preparing a hole injection layer and an anode on the hole transport layer.
Specifically, in the above two methods, the materials of the layers are as described above, and are not described herein for brevity.
Depositing CuMO2The method comprises a chemical method and a physical method, wherein the physical method comprises a physical coating method and a solution processing method. Specifically, the chemical method comprises: chemical vapor deposition, continuous ionic layer adsorption and reaction, anodic oxidation, electrolytic deposition, and coprecipitation. The physical coating method comprises the following steps: thermal evaporation coating, electron beam evaporation coating, magnetron sputtering, multi-arc ion coating, physical vapor deposition, atomic layer deposition, pulsed laser deposition, and the like. The solution processing method comprises a spin coating method, a printing method, a dip-coating method, a soaking method, a spraying method, a rolling coating method, a casting method, a slit coating method and a strip coating method. In the embodiment of the invention, a solution processing method is preferably adopted to prepare the uniform and compact interface modification layer. Further preferably, the CuMO is deposited2Thereafter, annealing treatment is carried out at 70 to 9 ℃, more preferably at 80 ℃.
In the embodiment of the invention, the cathode and the anode can be realized by adopting a mask evaporation method, and the hole injection layer, the quantum dot light-emitting layer and the electron transport layer can be realized by adopting a conventional deposition method, in particular, the method for preparing the interface modification layer can be referred to.
The anode substrate or the cathode substrate further comprises a cleaning treatment before the functional material is deposited. Preferably, the anode substrate or the cathode substrate is sequentially placed in acetone, washing solution, deionized water and isopropanol for ultrasonic cleaning, and each ultrasonic cleaning step lasts for 10-20 minutes, and more preferably for about 15 minutes. And after the ultrasonic treatment is finished, the anode substrate or the cathode substrate is placed in a clean oven to be dried for later use.
The following description will be given with reference to specific examples.
Example 1
CuMO2The preparation method comprises the following steps:
dissolving 5mmol of copper chloride into 5ml of water to prepare a copper chloride solution (A solution), and introducing inert gas to remove oxygen dissolved in the water; then, a weak reducing agent such as 10mmol of sodium thiosulfate is dissolved in 5ml of water to prepare a weak reducing agent solution (B solution), and an inert gas is introduced to remove oxygen. Dissolving 5mmol gallium chloride in 5ml water solution, regulating pH to 5-6.5, preparing solution C, and introducing large amount of inert gas to eliminate oxygen dissolved in water.
Adding the solution B into the solution A, stirring and reacting to reduce the bivalent copper into monovalent copper, and reacting completely; immediately, add solution C and stir well. And then adding the obtained mixed solution into a reaction kettle, heating at 200 ℃ for reaction for 2h, finally washing the precipitate obtained by the reaction with ammonia water, nitric acid and deionized water, and then dispersing the precipitate into an alcohol solution.
Example 2
CuMO2The preparation method comprises the following steps:
dissolving 5mmol of copper acetate into 5ml of water to prepare a copper chloride solution (solution A), and introducing inert gas to remove oxygen dissolved in the water; then, a weak reducing agent, such as 10mmol sodium citrate, is dissolved in 5ml water to prepare a weak reducing agent solution (B solution), and inert gas is introduced to remove oxygen in the solution. Dissolving 5mmol gallium acetate in 5ml water solution, adjusting pH to 5-6.5, preparing solution C, and introducing large amount of inert gas to remove oxygen dissolved in water.
Adding the solution B into the solution A, stirring and reacting to reduce the bivalent copper into monovalent copper, and reacting completely; solution C was added immediately and stirred well. And then adding the obtained mixed solution into a reaction kettle, heating at 200 ℃ for reaction for 2h, finally washing the precipitate obtained by the reaction with ammonia water, nitric acid and deionized water, and then dispersing the precipitate into an alcohol solution. .
Example 3
A preparation method of a QLED device comprises the following steps:
depositing a hole injection layer on the ITO substrate, and annealing for 15min at 150 ℃;
deposition of the CuMO from example 1 on a hole-injecting layer2Annealing at 150 ℃ for 30min to prepare a hole transport layer;
preparing a quantum dot light-emitting layer on the hole transport layer, depositing an electron transport layer on the quantum dot light-emitting layer, and preparing a cathode on the electron transport layer.
Example 4
A preparation method of a QLED device comprises the following steps:
preparing an electron transmission layer and a quantum dot light emitting layer on an ITO substrate;
depositing the CuMO obtained in example 1 on the quantum dot light emitting layer2Annealing at 150 ℃ for 30min to prepare a hole transport layer;
and sequentially preparing a hole injection layer and an anode on the hole transport layer.
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 (5)
1. CuMO2The preparation method is characterized by comprising the following steps:
providing a cupric salt solution, adding a reducing agent into the cupric salt solution under an inert atmosphere, and generating cuprous ions by the cupric ions in the cupric salt under the action of the reducing agent to obtain a cuprous ion solution;
providing an M salt solution in which M ions form [ M (OH)4(H2O)2]-And/or M (OH)3·3H2O, wherein M is selected from one of Ga, In, Cr and Al, and the pH value of the aqueous solution of the M salt is 5-6.5; adding the M salt aqueous solution into the cuprous ion solution under inert atmosphere, and heating for reaction to generate CuMO2。
2. The CuMO of claim 12The preparation method is characterized in that the M salt solution is added into the cuprous ion solution under inert atmosphere, and the CuMO is generated by heating reaction2In the step (2), the heating reaction temperature is 180-250 ℃, and the reaction time is 1-3 hours.
3. The CuMO of claim 12The method for producing (1), wherein the reducing agent is at least one selected from sodium thiosulfate and sodium citrate.
4. The CuMO according to any one of claims 1-32The preparation method of (1) is characterized in that the cupric salt in the cupric salt solution is a cupric salt soluble in water and is not cupric nitrate; and/or
The M salt in the M salt water solution is M salt which can be dissolved in water and is not nitrate of M.
5. The CuMO according to any one of claims 1-32The preparation method is characterized in that the M salt solution is added into the cuprous ion solution and is heated to react to generate CuMO2After the step (2), the obtained CuMO is also added2Carrying out cleaning treatment, wherein the cleaning treatment method comprises the following steps: sequentially adopting ammonia water, nitric acid and deionized water to carry out a reaction to obtain CuMO2Washing is carried out.
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