CN111384259B - Quantum dot light-emitting diode and preparation method thereof - Google Patents
Quantum dot light-emitting diode and preparation method thereof Download PDFInfo
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- CN111384259B CN111384259B CN201811626894.XA CN201811626894A CN111384259B CN 111384259 B CN111384259 B CN 111384259B CN 201811626894 A CN201811626894 A CN 201811626894A CN 111384259 B CN111384259 B CN 111384259B
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- 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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Abstract
The invention discloses a quantum dot light-emitting diode and a preparation method thereof, wherein the method comprises the following steps: providing an anode; preparing a quantum dot light emitting layer on the anode; preparing a cathode on the quantum dot light-emitting layer to obtain the quantum dot light-emitting diode; the quantum dot light-emitting layer is prepared by the following method: providing a mixed solution, wherein the mixed solution comprises quantum dots, a solvent and an additive, the additive is alkane with 6-13 carbon atoms, and carbon atoms at two ends of a main chain of the alkane are connected with iodine atoms; depositing the mixed solution on an anode to form a film layer, and volatilizing the additive in the film layer to obtain the quantum dot light-emitting layer. The method can reduce the energy transfer of the Dexter between the quantum dots and reduce the energy loss, thereby improving the luminous efficiency of the device.
Description
Technical Field
The invention relates to the field of quantum dot light-emitting devices, in particular to a quantum dot light-emitting diode and a preparation method thereof.
Background
In recent years, with the rapid development of display technologies, quantum dot light emitting diodes (QLEDs) having semiconductor Quantum Dot (QDs) materials as light emitting layers have received much attention. The quantum dot light-emitting diode has the advantages of high color purity, high luminous efficiency, adjustable luminous color, stable device and the like, so that the quantum dot light-emitting diode has wide application prospect in the fields of flat panel display, solid state lighting and the like. Although the performance (including device efficiency and service life) of the existing QLED is greatly improved by the improvement of quantum dot materials and the continuous optimization of the structure of the QLED device, the efficiency of the existing QLED is far from the requirement of industrial production. Wherein the quantum dot layer is a key layer of the QLED device, and the quantum dot layer is formed by a layer of nano particles. The existing problem is that if the concentration of the nano particles is too low, a compact quantum dot layer cannot be formed, namely holes appear, and leakage current can be caused; at too high a concentration, nanoparticle stacking, i.e. cluster formation, can occur, which can lead to Dexter energy transfer (Dexter energy transfer belongs to non-radiative energy transfer), and thus the luminous efficiency of the device is reduced. Therefore, how to prepare a compact and uniform quantum dot layer is an important research direction for improving the luminous efficiency of the QLED.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned deficiencies of the prior art, the present invention aims to provide a quantum dot light emitting diode and a method for manufacturing the same, which aims to solve the problem of low light emitting efficiency of the conventional quantum dot light emitting diode.
The technical scheme of the invention is as follows:
a preparation method of a quantum dot light-emitting diode comprises the following steps:
providing an anode;
preparing a quantum dot light emitting layer on the anode;
preparing a cathode on the quantum dot light-emitting layer to obtain the quantum dot light-emitting diode;
the quantum dot light-emitting layer is prepared by the following method:
providing a mixed solution, wherein the mixed solution comprises quantum dots, a solvent and an additive, the additive is alkane with 6-13 carbon atoms, and carbon atoms at two ends of a main chain of the alkane are connected with iodine atoms;
depositing the mixed solution on an anode to form a film layer, and volatilizing the additive in the film layer to obtain the quantum dot light-emitting layer.
A quantum dot light emitting diode comprising: the quantum dot light-emitting diode comprises an anode, a cathode and a quantum dot light-emitting layer arranged between the anode and the cathode, wherein the quantum dot light-emitting diode is prepared by the preparation method.
Has the advantages that: according to the invention, the quantum dot light-emitting layer is prepared by adopting the mixed solution containing the quantum dots and the additive, the additive is alkane with 6-13 carbon atoms, and the carbon atoms at two ends of the main chain of the alkane are connected with iodine atoms, so that after the mixed solution forms a film layer, the additive exists among the quantum dots, the additive is volatilized from the gaps of the quantum dots under certain conditions, and as the two ends of the long chain of the additive are iodine atoms with larger radius, gaps with the size of about iodine atoms are formed among the quantum dots after volatilization, the energy transfer of Dexter among the quantum dots is reduced, the energy loss is reduced, and the light-emitting efficiency of a device is improved.
Drawings
Fig. 1 is a schematic structural diagram of a quantum dot light emitting diode according to an embodiment of the present invention.
Detailed Description
The invention provides a quantum dot light-emitting diode and a preparation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a quantum dot light-emitting diode, which comprises the following steps:
providing an anode;
preparing a quantum dot light emitting layer on the anode;
preparing a cathode on the quantum dot light-emitting layer to obtain the quantum dot light-emitting diode;
the quantum dot light-emitting layer is prepared by the following method:
providing a mixed solution, wherein the mixed solution comprises quantum dots, a solvent and an additive, the additive is alkane with 6-13 carbon atoms, and carbon atoms at two ends of a main chain of the alkane are connected with iodine atoms;
depositing the mixed solution on an anode to form a film layer, and volatilizing the additive in the film layer to obtain the quantum dot light-emitting layer.
In the embodiment, the quantum dot light emitting layer is prepared by adopting a mixed solution containing quantum dots and an additive, wherein the additive is alkane with 6-13 carbon atoms, and the carbon atoms at two ends of a main chain of the alkane are connected with iodine atoms, so that the additive exists among the quantum dots after the mixed solution forms a film layer, the additive is volatilized from gaps of the quantum dots under certain conditions, and because two ends of a long chain of the additive are iodine atoms with larger radius, gaps with the size of about iodine atoms are formed among the quantum dots after volatilization, the energy transfer of Dexter among the quantum dots is reduced, the energy loss is reduced, and the light emitting efficiency of a device is improved.
After the mixed solution is deposited, the common solvents (such as n-octane and the like) for dissolving the quantum dots in the mixed solution have low boiling points, and thus can be easily volatilized to form a film layer. And additives selected, for example, 1, 8-diiodooctane, having a boiling point of 168 oCThe additive is difficult to naturally volatilize, but the additive is easy to volatilize under high vacuum when the film layer containing the additive is placed in vacuum, so that the additive is volatilized from the gaps of the quantum dots.
In general, organic solvents have short carbon chains, small molecular weights, are easy to volatilize, have long carbon chains and large molecular weights, are difficult to volatilize, and the molecular weights are greatly increased by adding iodine atoms. In this example, if an alkane containing 5 carbon atoms is selected as the additive, i.e., 1, 5-diiodopentane, its boiling point is about 101oC, has the same volatility as the solvent and cannot play a role. And the alkane containing 14 carbon atoms is selected as the additive, and is difficult to volatilize under vacuum even if two ends are not substituted by iodine. Therefore, the additive in this embodiment is alkane with 6-13 carbon atoms, and carbon atoms at two ends of the main chain of the alkane are connected with iodine atoms. In the present embodiment, the quantum dot light emitting diode has various forms, and the quantum dot light emitting diode has a positive type structure and an inverse type structure, and the present embodiment will be described in detail mainly by taking the quantum dot light emitting diode with the positive type structure as shown in fig. 1 as an example. Specifically, as shown in fig. 1, the quantum dot light emitting diode includes a substrate 1, a bottom electrode 2, a hole injection layer 3, a hole transport layer 4, a quantum dot light emitting layer 5, an electron transport layer 6, and a top electrode 7, which are stacked from bottom to top; the quantum dot light emitting diodeThe preparation method of the tube specifically comprises the following steps:
providing a substrate, and preparing a bottom electrode on the substrate;
preparing a hole injection layer on the bottom electrode;
preparing a hole transport layer on the hole injection layer;
preparing a quantum dot light emitting layer on the hole transport layer;
preparing an electron transport layer on the quantum dot light emitting layer;
preparing a top electrode on the electron transmission layer to obtain the quantum dot light-emitting diode;
the quantum dot light-emitting layer is prepared by the following method:
providing a mixed solution, wherein the mixed solution comprises quantum dots, a solvent and an additive, the additive is alkane with 6-13 carbon atoms, and carbon atoms at two ends of a main chain of the alkane are connected with iodine atoms;
depositing the mixed solution on an anode to form a film layer, and volatilizing the additive in the film layer to obtain the quantum dot light-emitting layer.
In a preferred embodiment, the mixed solution is deposited on an anode, and a solvent in the mixed solution is volatilized to form a film layer; and volatilizing the additive in the film layer under the vacuum condition to obtain the quantum dot light-emitting layer. After the mixed solution is deposited on the anode, the solvent in the mixed solution can be easily volatilized to form a film layer due to the low boiling point. And because the additive is difficult to naturally volatilize, the film layer containing the additive is placed in vacuum, so that the additive can volatilize from the gaps of the quantum dots. In a further preferred embodiment, the additive in the film layer is volatilized under a vacuum of less than 0.01 Pa. Under the condition of high vacuum (less than 0.01 Pa), the additive in the film layer can be volatilized.
Further in a preferred embodiment, the additive in the film layer is volatilized under vacuum for 0.5 to 24 hours. In this time frame, complete volatilization of the additive can be ensured.
In a preferred embodiment, the additive is 0.1 to 5% by volume of the mixed solution.
In a preferred embodiment, the additive is a linear alkane having 6 to 13 carbon atoms. Further in a preferred embodiment, the additive includes one or more of 1, 6-diiodohexane, 1, 8-diiodooctane, 1, 10-diiododecane, etc., but is not limited thereto.
In another preferred embodiment, the additive is a branched alkane having 6 to 13 carbon atoms, wherein the branched chain has 1 to 2 carbon atoms, in this case, the alkane having 1 to 2 carbon atoms does not reduce the boiling point of the alkane too much to meet the boiling point requirement, and the increase of the branched chain can complicate the spatial structure of the additive, the spatial structure is complicated, and the agglomeration of quantum dot particles can be prevented, so that the Dexter energy transfer between quantum dots can be further reduced.
In a preferred embodiment, the mixed solution includes a solvent for dispersing the quantum dots, and the solvent may be one or more selected from n-hexane, chlorobenzene, toluene, cyclohexane, and the like.
In a preferred embodiment, the quantum dots may be selected from one or more of the common red, green and blue quantum dots.
In a preferred embodiment, the substrate may be a rigid substrate, such as glass, or a flexible substrate, such as one of PET or PI.
In a preferred embodiment, the substrate containing the bottom electrode is pretreated. Taking the substrate containing the bottom electrode as an ITO substrate as an example, the specific pretreatment steps comprise: cleaning the whole ITO substrate with a cleaning agent, preliminarily removing stains on the surface, then sequentially and respectively ultrasonically cleaning in acetone, a cleaning solution, deionized water and isopropanol for 15 min to remove impurities on the surface, and finally drying with high-purity nitrogen to obtain a clean ITO substrate. Further, the clean ITO substrate is treated with ultraviolet-ozone or oxygen plasma to further remove organic substances attached to the surface of the ITO substrate, thereby increasing the work function of the ITO substrate.
In a preferred embodiment, the hole injection layer material may be water-soluble PEDOT: PSS, or other material with good hole injection properties, such as NiO, MoO3、WO3And V2O5And the like. In a preferred embodiment, the hole injection layer has a thickness of 10 to 100 nm.
In a preferred embodiment, the material of the hole transport layer may be selected from materials having good hole transport ability, such as but not limited to Poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine) (TFB), Polyvinylcarbazole (PVK), Poly (N, N ' bis (4-butylphenyl) -N, N ' -bis (phenyl) benzidine) (Poly-TPD), Poly (9, 9-dioctylfluorene-CO-bis-N, N-phenyl-1, 4-Phenylenediamine) (PFB), 4', 4 "-tris (carbazol-9-yl) triphenylamine (TCTA), 4' -bis (9-Carbazol) Biphenyl (CBP), N ' -diphenyl-N, one or more of N ' -bis (3-methylphenyl) -1,1 ' -biphenyl-4, 4' -diamine (TPD), N ' -diphenyl-N, N ' - (1-naphthyl) -1,1 ' -biphenyl-4, 4' -diamine (NPB). In a preferred embodiment, the hole transport layer has a thickness of 1 to 100 nm.
In a preferred embodiment, the material of the electron transport layer may be selected from materials with good electron transport properties, such as but not limited to n-type ZnO, TiO2、Fe2O3、SnO2、Ta2O3One or more of AlZnO, ZnSnO and InSnO. Further in a preferred embodiment, the material of the electron transport layer is selected from n-type ZnO. In a preferred embodiment, the thickness of the electron transport layer is 10 to 60 nm.
In a preferred embodiment, the top electrode may be selected from one of an aluminum (Al) electrode, a silver (Ag) electrode, a gold (Au) electrode, a copper (Cu) electrode, and the like. In a preferred embodiment, the top electrode has a thickness of 60-120 nm.
The preparation method of each layer can be a chemical method or a physical method, wherein the chemical method comprises one or more of but not limited to a chemical vapor deposition method, a continuous ion layer adsorption and reaction method, an anodic oxidation method, an electrolytic deposition method and a coprecipitation method; physical methods include, but are not limited to, physical coating methods or solution methods, wherein solution methods include, but are not limited to, spin coating, printing, knife coating, dip-coating, dipping, spraying, roll coating, casting, slot coating, bar coating; physical coating methods include, but are not limited to, one or more of thermal evaporation coating, electron beam evaporation coating, magnetron sputtering, multi-arc ion coating, physical vapor deposition, atomic layer deposition, pulsed laser deposition.
The embodiment of the present invention further provides a quantum dot light emitting diode, including: the quantum dot light-emitting diode comprises an anode, a cathode and a quantum dot light-emitting layer arranged between the anode and the cathode, wherein the quantum dot light-emitting diode is prepared by the preparation method provided by the embodiment of the invention.
In a preferred embodiment, the thickness of the quantum dot light emitting layer is 10 to 60 nm.
The following describes in detail the method for manufacturing a quantum dot light emitting diode according to an embodiment of the present invention with reference to specific examples.
In a first specific embodiment, the quantum dot light emitting diode device is prepared by the following steps:
firstly, placing a patterned ITO substrate in acetone, washing liquor, deionized water and isopropanol in sequence for ultrasonic cleaning, wherein each step of ultrasonic cleaning lasts for about 15 minutes. And after the ultrasonic treatment is finished, the ITO substrate is placed in a clean oven to be dried for later use.
And after the ITO substrate is dried, treating the surface of the ITO substrate for 5 minutes by using ultraviolet-ozone to further remove organic matters attached to the surface of the ITO substrate and improve the work function of the ITO substrate.
Then, PSS, a hole injection layer PEDOT, which has a thickness of 30nm, was deposited on the ITO substrate treated in the above step, and the substrate was heated on a heating stage at 150 ℃ for 30 minutes to remove moisture, which was done in air.
Next, the dried substrate coated with the hole injection layer was placed in a nitrogen atmosphere, a hole transport layer material TFB was deposited as a layer having a thickness of 30nm, and the substrate was placed on a heating stage at 150 ℃ for 30 minutes to remove the solvent.
After the wafer treated in the previous step was cooled, a quantum dot solution containing 0.1% (v/v) 1, 8-diiodooctane was spin-coated on the hole transport layer, which was then placed on a 1X 10 substrate-3Pa for 2 hours under vacuum, the thickness was about 20 nm.
Subsequently, a ZnO electron transporting layer was deposited, and after the deposition was completed, the wafer was heated on a heating stage at 80 ℃ for 30 minutes to a thickness of 30 nm.
And finally, placing the sheets with the deposited functional layers in an evaporation bin, and thermally evaporating a layer of 100nm silver as a cathode through a mask plate, thereby completing the preparation of the device.
In a second embodiment, the quantum dot light emitting diode device is prepared by the following steps:
firstly, placing a patterned ITO substrate in acetone, washing liquor, deionized water and isopropanol in sequence for ultrasonic cleaning, wherein each step of ultrasonic cleaning lasts for about 15 minutes. And after the ultrasonic treatment is finished, the ITO substrate is placed in a clean oven to be dried for later use.
And after the ITO substrate is dried, treating the surface of the ITO substrate for 5 minutes by using ultraviolet-ozone to further remove organic matters attached to the surface of the ITO substrate and improve the work function of the ITO substrate.
Then, PSS, a hole injection layer PEDOT, which has a thickness of 30nm, was deposited on the ITO substrate treated in the above step, and the substrate was heated on a heating stage at 150 ℃ for 30 minutes to remove moisture, which was done in air.
Next, the dried substrate coated with the hole injection layer was placed in a nitrogen atmosphere, a layer of the hole transport layer material PVK was deposited to a thickness of 30nm, and the substrate was placed on a heating stage at 150 ℃ for 30 minutes to remove the solvent.
After the wafer treated in the previous step is cooled, a quantum dot solution containing 2% (v/v) 1, 8-diiodooctane is spin-coated on the hole transport layerThen it was placed at 1X 10-3Pa for 4 hours under vacuum, the thickness was about 20 nm.
Subsequently, a ZnO electron transporting layer was deposited, and after the deposition was completed, the wafer was heated on a heating stage at 80 ℃ for 30 minutes to a thickness of 30 nm.
And finally, placing the sheet on which the functional layers are deposited in an evaporation bin, and thermally evaporating a layer of 100nm aluminum as a cathode through a mask plate, so that the device is prepared.
In a third specific embodiment, the quantum dot light emitting diode device is prepared by the following steps:
firstly, placing a patterned ITO substrate in acetone, washing liquor, deionized water and isopropanol in sequence for ultrasonic cleaning, wherein each step of ultrasonic cleaning lasts for about 15 minutes. And after the ultrasonic treatment is finished, the ITO substrate is placed in a clean oven to be dried for later use.
And after the ITO substrate is dried, treating the surface of the ITO substrate for 5 minutes by using ultraviolet-ozone to further remove organic matters attached to the surface of the ITO substrate and improve the work function of the ITO substrate.
Then, PSS, a hole injection layer PEDOT, which has a thickness of 30nm, was deposited on the ITO substrate treated in the above step, and the substrate was heated on a heating stage at 150 ℃ for 30 minutes to remove moisture, which was done in air. .
Next, the dried substrate coated with the hole injection layer was placed in a nitrogen atmosphere, a layer of the hole transport layer material PVK was deposited to a thickness of 30nm, and the substrate was placed on a heating stage at 150 ℃ for 30 minutes to remove the solvent.
After the wafer treated in the previous step was cooled, a quantum dot solution containing 5% (v/v) 1, 8-diiodooctane was spin-coated on the hole transport layer, which was then placed at 1X 10-4Pa for 8 hours under vacuum, and the thickness is about 20 nm.
Subsequently, a ZnO electron transporting layer was deposited, and after the deposition was completed, the wafer was heated on a heating stage at 80 ℃ for 30 minutes to a thickness of 30 nm.
And finally, placing the sheet on which the functional layers are deposited in an evaporation bin, and thermally evaporating a layer of 100nm aluminum as a cathode through a mask plate, so that the device is prepared.
In summary, the invention provides a quantum dot light emitting diode and a preparation method thereof. According to the invention, the quantum dot light-emitting layer is prepared by adopting the mixed solution containing the quantum dots and the additive, the additive is alkane with 6-13 carbon atoms, and the carbon atoms at two ends of the main chain of the alkane are connected with iodine atoms, so that after the mixed solution forms a film layer, the additive exists among the quantum dots, the additive is volatilized from the gaps of the quantum dots under certain conditions, and as the two ends of the long chain of the additive are iodine atoms with larger radius, gaps with the size of about iodine atoms are formed among the quantum dots after volatilization, the energy transfer of Dexter among the quantum dots is reduced, the energy loss is reduced, and the light-emitting efficiency of a device is improved.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of a quantum dot light-emitting diode is characterized by comprising the following steps:
providing an anode;
preparing a quantum dot light emitting layer on the anode;
preparing a cathode on the quantum dot light-emitting layer to obtain the quantum dot light-emitting diode;
the quantum dot light-emitting layer is prepared by the following method:
providing a mixed solution, wherein the mixed solution comprises quantum dots, a solvent and an additive, the additive is straight-chain alkane with 6-13 carbon atoms or branched-chain alkane with 6-13 carbon atoms, the carbon atoms of the branched chain are 1-2, and the carbon atoms at two ends of the main chain of the alkane are connected with iodine atoms;
depositing the mixed solution on an anode to form a film layer, and volatilizing the additive in the film layer to obtain the quantum dot light-emitting layer.
2. The method of claim 1, wherein the mixed solution is deposited on an anode, and a solvent in the mixed solution is volatilized to form a film; and volatilizing the additive in the film layer under the vacuum condition to obtain the quantum dot light-emitting layer.
3. The method for preparing a quantum dot light-emitting diode according to claim 2, wherein the additive in the film layer is volatilized under a vacuum condition of less than 0.01 Pa; and/or the presence of a gas in the gas,
and volatilizing the additive in the film layer under the vacuum condition for 0.5-24 hours.
4. The method of claim 1, wherein the additive is 0.1-5% by volume of the mixed solution.
5. The method of claim 1, wherein the additive comprises one or more of 1, 6-diiodohexane, 1, 8-diiodooctane, and 1, 10-diiododecane.
6. A quantum dot light emitting diode comprising: the quantum dot light-emitting diode comprises an anode, a cathode and a quantum dot light-emitting layer arranged between the anode and the cathode, and is characterized in that the quantum dot light-emitting diode is prepared by the preparation method of any one of claims 1 to 5.
7. The quantum dot light-emitting diode of claim 6, wherein the quantum dot light-emitting layer has a thickness of 10-60 nm.
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