CN116997199A - Electroluminescent device and preparation method thereof - Google Patents
Electroluminescent device and preparation method thereof Download PDFInfo
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- CN116997199A CN116997199A CN202210420916.7A CN202210420916A CN116997199A CN 116997199 A CN116997199 A CN 116997199A CN 202210420916 A CN202210420916 A CN 202210420916A CN 116997199 A CN116997199 A CN 116997199A
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Abstract
The application discloses an electroluminescent device and a preparation method thereof, and belongs to the technical field of electroluminescence. The electroluminescent device comprises an anode, a hole transport layer, a luminescent layer and a cathode which are arranged in a stacked manner, wherein one side part of the luminescent layer adjacent to the hole transport layer is embedded into the hole transport layer. The application can increase the contact between the hole transmission layer and the luminescent layer to increase the hole injection so as to reduce the charge accumulation at the contact interface between the hole transmission layer and the luminescent layer, thereby improving the performance and the service life of the device.
Description
Technical Field
The application relates to the technical field of electroluminescence, in particular to an electroluminescent device and a preparation method thereof.
Background
The existing quantum dot electroluminescent (Quantum Dot Light Emitting Diodes, abbreviated as QLED) device/Organic Light-Emitting Diode (abbreviated as OLED) device is an Organic-inorganic composite device, that is, hole injection and transport are Organic materials, and electron injection and transport are inorganic materials, when forward bias is applied to two ends of the QLED device/OLED device, electrons and holes enter the Light-Emitting layer through the electron transport layer and the hole transport layer respectively; and light is compositely emitted at the light-emitting layer. As such, since the electron transfer efficiency of the inorganic nanoparticles is much greater than that of holes, this causes a large accumulation of charges at the contact interface between the hole transport layer and the light emitting layer, thereby affecting device performance and lifetime.
Disclosure of Invention
In view of the above, the present application provides an electroluminescent device and a method for manufacturing the same, which aims to solve the technical problem that the existing electroluminescent device structure is easy to affect the performance of the device.
The embodiment of the application is realized in that the electroluminescent device comprises an anode, a hole transport layer, a light emitting layer and a cathode which are arranged in a stacked manner, wherein one side part of the light emitting layer adjacent to the hole transport layer is embedded into the hole transport layer.
Optionally, in some embodiments of the present application, the hole transport layer includes a first film layer and a second film layer that are stacked, and a side portion of the light emitting layer adjacent to the hole transport layer is embedded in the second film layer.
Optionally, in some embodiments of the present application, the first film layer and the second film layer are both conductive polymer layers.
Alternatively, in some embodiments of the present application, the conductive polymer used in the conductive polymer layer includes a homopolymer formed from any one of an aniline monomer, a thiophene monomer, and a fluorene monomer, or a copolymer formed from any combination thereof.
Optionally, in some embodiments of the application, the conductive polymer of the first film layer is a crosslinkable polymer; and/or the conductive polymer of the second film layer is a non-crosslinked polymer.
Optionally, in some embodiments of the present application, the thickness of the first film layer is 10nm to 50nm; and/or the thickness of the second film layer is 1 nm-10 nm.
Optionally, in some embodiments of the present application, the anode is a metal oxide electrode or a composite electrode, the metal oxide electrode is at least one selected from ITO, FTO, ATO, AZO, GZO, IZO, MZO and AMO, the composite electrode is AZO/Ag/AZO, AZO/Al/AZO, ITO/Ag/ITO, ITO/Al/ITO, znO/Ag/ZnO, znO/Al/ZnO, tiO2/Ag/TiO2, tiO2/Al/TiO2, znS/Ag/ZnS or ZnS/Al/ZnS; and/or the light emitting layer comprises quantum dots, wherein the quantum dots are selected from at least one of single-structure quantum dots and core-shell structure quantum dots, the single-structure quantum dots are selected from at least one of II-VI compounds, III-V compounds and I-III-VI compounds, the II-VI compounds are selected from at least one of CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe and CdZnSTe, the III-V compounds are selected from at least one of InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP, and the I-III-VI compounds are selected from at least one of CuInS2, cuInSe2 and AgInS 2; the core of the quantum dot with the core-shell structure is selected from any one of the quantum dots with the single structure, and the shell material of the quantum dot with the core-shell structure is selected from at least one of CdS, cdTe, cdSeTe, cdZnSe, cdZnS, cdSeS, znSe, znSeS and ZnS; and/or the cathode is selected from at least one of an Ag electrode, an Al electrode, an Au electrode, a Pt electrode or an alloy electrode.
Optionally, in some embodiments of the present application, the electroluminescent device is further provided with a hole injection layer between the anode and the hole transport layer; and/or, the electroluminescent device is further provided with an electron transport layer between the cathode and the light emitting layer.
Correspondingly, the embodiment of the application also provides a preparation method of the electroluminescent device, which comprises the following steps: providing an anode substrate; a hole transmission layer is arranged on the anode substrate, the hole transmission layer is divided into a semi-wetting zone, wherein 5% -10% of organic solution is remained in the semi-wetting zone according to the total mass of the semi-wetting zone so as to form the semi-wetting zone; providing a luminescent layer on the semi-wetting region; a cathode is disposed on the light emitting layer.
Optionally, in some embodiments of the present application, the step of disposing a hole transport layer on the anode substrate specifically includes: a first film layer is arranged on the anode substrate; and a second film layer is arranged on the first film layer, wherein 5% -10% of organic solution is remained in the second film layer according to the total mass of the second film layer, so that the second film layer forms the semi-wetting zone.
Optionally, in some embodiments of the present application, when a first film layer is disposed on the anode substrate, performing a first vacuum reduced pressure drying treatment on the first film layer, and when a second film layer is disposed on the first film layer, performing a second vacuum reduced pressure drying treatment on the second film layer; the first pressure at the time of the first vacuum reduced pressure drying process is less than the second pressure at the time of the second vacuum reduced pressure drying process, and/or the first vacuum reduced pressure drying process lasts for a first duration that is greater than the second duration that the second vacuum reduced pressure drying process lasts.
Optionally, in some embodiments of the present application, the first pressure is less than 10pa, and/or the second pressure is between 1000pa and 10000pa, and/or the first duration is greater than 5min, and/or the second duration is less than 5min.
Optionally, in some embodiments of the present application, when a first film layer is disposed on the anode substrate, a first baking and drying treatment is performed on the first film layer, and when a second film layer is disposed on the first film layer, a second baking and drying treatment is performed on the second film layer; the first temperature at the first bake-drying process is higher than the second temperature at the second bake-drying process, and/or the first bake-drying process lasts for a third duration that is greater than a fourth duration that the second bake-drying process lasts.
Optionally, in some embodiments of the present application, the first temperature is 150 ℃ to 300 ℃, and/or the second temperature is 50 ℃ to 150 ℃, and/or the third duration is 15min to 60min, and/or the fourth duration is 1min to 15min.
Optionally, in some embodiments of the present application, the method further includes the steps of: providing a hole injection layer between the anode substrate and the hole transport layer; and/or an electron transport layer is provided between the cathode and the light emitting layer.
In the application, when the electroluminescent device is provided with a hole transport layer, the hole transport layer is divided into semi-moist areas. Wherein, based on the total mass of the semi-wetting zone, 5% -10% of organic solution is remained in the semi-wetting zone to form the semi-wetting zone. Finally, the electroluminescent device is formed such that a portion of the light-emitting layer adjacent to one side of the hole-transporting layer is embedded in the hole-transporting layer (i.e., a portion of the nanoparticles on the lower surface of the light-emitting layer are correspondingly embedded in the semi-moist region of the hole-transporting layer). Therefore, the application can increase the contact between the hole transmission layer and the luminescent layer (especially the quantum dot luminescent layer of the QLED device) to increase the hole injection so as to reduce the charge accumulation at the contact interface between the hole transmission layer and the luminescent layer (especially the quantum dot luminescent layer of the QLED device), thereby improving the device performance and the service life.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of an electroluminescent device according to an embodiment of the present application.
Fig. 2 is a schematic diagram of another structure of the electroluminescent device shown in fig. 1.
Fig. 3 is a flow chart of a method for manufacturing an electroluminescent device according to an embodiment of the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present application based on the embodiments of the present application. Furthermore, it should be understood that the detailed description is presented herein for purposes of illustration and description only, and is not intended to limit the application. In the present application, unless otherwise specified, terms such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present application, the term "comprising" means "including but not limited to". Various embodiments of the application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
The existing QLED device/OLED device is an organic-inorganic composite device, namely hole injection and transmission are organic materials, electron injection and transmission are inorganic materials, and when forward bias voltage is applied to two ends of the QLED device/OLED device, electrons and holes respectively enter the light-emitting layer through the electron transmission layer and the hole transmission layer; and light is compositely emitted at the light-emitting layer. As such, since the electron transfer efficiency of the inorganic nanoparticles is much greater than that of holes, this causes a large accumulation of charges at the contact interface between the hole transport layer and the light emitting layer, thereby affecting device performance and lifetime.
Based on this, it is necessary to provide a new structural solution for electroluminescent devices, so as to improve the technical problem that the existing electroluminescent device structure easily affects the device performance.
In one embodiment, as shown in fig. 1, the present embodiment provides an electroluminescent device 100, where the electroluminescent device 100 includes an anode 110, a hole transport layer 120, a light emitting layer 130, and a cathode 140 that are stacked, and a portion of one side of the light emitting layer 130 adjacent to the hole transport layer 120 is embedded in the hole transport layer 120.
It should be noted that fig. 1 is only a simple illustration of the layout of the layers of the electroluminescent device, and is not an actual structure of the electroluminescent device. The electroluminescent device may be a QLED device or an OLED device, and when the electroluminescent device is a QLED device, the anode 110 may be a metal oxide electrode or a composite electrode, wherein the metal oxide electrode is at least one selected from ITO, FTO, ATO, AZO, GZO, IZO, MZO and AMO, and the composite electrode is AZO/Ag/AZO, AZO/Al/AZO, ITO/Ag/ITO, ITO/Al/ITO, znO/Ag/ZnO, znO/Al/ZnO, tiO2/Ag/TiO2, tiO2/Al/TiO2, znS/Ag/ZnS or ZnS/Al/ZnS. The light emitting layer 130 may specifically include quantum dots, where the quantum dots are at least one of single-structure quantum dots and core-shell structure quantum dots, the single-structure quantum dots are at least one of group II-VI compounds, group III-V compounds and group I-III-VI compounds, the group II-VI compounds are at least one of CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe and CdZnSTe, the group III-V compounds are at least one of InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP, and the group I-III-VI compounds are at least one of CuInS2, cuInSe2 and AgInS 2. The core of the quantum dot with the core-shell structure is selected from any one of the quantum dots with the single structure, and the shell material of the quantum dot with the core-shell structure is selected from at least one of CdS, cdTe, cdSeTe, cdZnSe, cdZnS, cdSeS, znSe, znSeS and ZnS. The cathode 140 may be at least one selected from an Ag electrode, an Al electrode, an Au electrode, a Pt electrode, and an alloy electrode.
In this way, in the electroluminescent device of the embodiment of the present application, the hole transport layer 120 is partially embedded in the side of the light emitting layer 130 adjacent to the hole transport layer 120, so that the nanoparticles (especially the quantum dot nanoparticles of the quantum dot light emitting layer) in the light emitting layer 130 are partially embedded in the hole transport layer 120, so that the contact between the hole transport layer 120 and the light emitting layer 130 (especially the quantum dot light emitting layer of the QLED device) can be increased, the hole injection is increased, and the charge accumulation at the contact interface between the hole transport layer 120 and the light emitting layer 130 (especially the quantum dot light emitting layer of the QLED device) is reduced, thereby improving the device performance and service life.
In some examples, as shown in fig. 1, the hole transport layer 120 includes a first film layer 121 and a second film layer 122 that are stacked, where the first film layer 121 is disposed adjacent to the anode 110, and the second film layer 122 is disposed adjacent to the light emitting layer 130, and at this time, a portion of one side of the light emitting layer 130 adjacent to the hole transport layer 120 is embedded in the hole transport layer 120, which is embodied as a portion of one side of the light emitting layer 130 adjacent to the hole transport layer 120 is embedded in the second film layer 122. In this way, when the first film 121 and the second film 122 are manufactured twice in sequence to form the hole transport layer 120 together, only the manufacturing process of the second film 122 needs to be changed, so that the second film 122 is in a semi-wet state (i.e. 5% -10% of organic solution is remained in the second film 122 based on the total mass of the second film 122), and when the light emitting layer 130 is prepared on the second film 122 in the semi-wet state, one side of the prepared light emitting layer 130 adjacent to the hole transport layer 120 is partially embedded into the second film 122.
In some examples, as shown in fig. 1, the first film layer 121 and the second film layer 122 may be conductive polymer layers. The conductive polymer used in the conductive polymer layer comprises a homopolymer formed by any one of aniline monomer, thiophene monomer and fluorene monomer or a copolymer formed by any combination of the aniline monomer, thiophene monomer and fluorene monomer. The conductive polymers used for the first film 121 and the second film 122 may be the same or different.
In some examples, the conductive polymer of the first film layer 121 may be a crosslinkable polymer, that is, a crosslinked group (the crosslinked group is a functional group that is not reacted, that is, a network polymer formed by a chain polymer through other functional groups under certain conditions, which can reduce the solubility of the polymer in a solvent and can further undergo a chemical reaction under conditions of high temperature, etc., and the crosslinked group may be a double bond, a cyclobutene, or an epoxy group). Because of the interfacial compatibility problem in preparing the film structure of the two-layer film, the conductive polymer of the first film 121 is a crosslinkable polymer, which can effectively avoid damage to the surface of the first film 121 when the second film 122 is disposed.
In some examples, the conductive polymer of the second film layer 122 may be a non-crosslinked polymer, that is, the conductive polymer does not contain a crosslinking group. The second film 122 is beneficial to the subsequent preparation of the light-emitting layer 130 (especially the quantum dot light-emitting layer of the QLED device) on the second film 122, and the light-emitting layer 130 (especially the quantum dot light-emitting layer of the QLED device) is better partially embedded into the second film 122, i.e. the embedding effect is improved. Meanwhile, the conductive polymer of the first film 121 is a crosslinkable polymer, and the conductive polymer of the second film 122 is a non-crosslinked polymer, so that the thickness of the particles embedded in the light emitting layer (especially, the quantum dot particles of the quantum dot light emitting layer of the QLED device) can be effectively controlled, for example, the total thickness of the hole transporting layer 120 is 25nm, the thickness of the first film 121 is 20nm, and then the maximum embedded thickness of the quantum dot is 5nm.
In addition, there are two general methods for crosslinking or non-crosslinking the same conductive polymer, the first method is to prepare a crosslinkable polymer using a monomer containing a crosslinking group before polymerization, and prepare a non-crosslinked polymer using a monomer not containing a crosslinking group, for example, to form a crosslinkable polymer: the crosslinkable polymer can be formed by copolymerizing a conductive structural unit (such as an aniline monomer, a thiophene unit, or a fluorene unit, etc.) containing no crosslinking group with a conductive structural unit (such as an aniline monomer, a thiophene unit, or a fluorene unit, etc.) containing a crosslinking group (such as a double bond, a cyclobutene, or an epoxy group, etc.) or with a nonconductive structural unit (such as a styryl group or a methylene group, etc.), wherein the structural unit containing a crosslinking group may be 1 to 5% in the corresponding polymer; the second method is to introduce a crosslinking group by a subsequent reaction with a side chain after the preparation of the conductive polymer is completed, so that the non-crosslinked polymer becomes a crosslinkable polymer.
In some examples, the thickness of the first film layer 121 may be specifically 10nm to 50nm, and the thickness of the second film layer 122 may be specifically 1nm to 10nm, so that the total thickness of the hole transport layer 120 formed by stacking the two layers may be specifically 11nm to 60nm, so as to meet the requirements of the electroluminescent device 100 on the hole transport layer 120.
In some examples, as shown in fig. 2, electroluminescent device 100 may be further provided with a hole injection layer 150 in particular between anode 110 and hole transport layer 120; and or, the electroluminescent device 100 may be further provided with an electron transport layer 160 between the cathode 140 and the light emitting layer 130 in particular, to realize the basic light emitting function of the electroluminescent device 100. The material of the hole injection layer 150 may be at least one of TFB, PVK, poly-TPD, TCTA, CBP, and the material of the electron transport layer 160 may be at least one of ZnO, znMgO, znMgLiO, znInO, zrO, zrO2, tiO2, snO2, ta2O3, niO, tiLiO, alq3, 3- (biphenyl-4-yl) -5- (4-tert-butylphenyl) -4-phenyl-4H-1, 2, 4-triazole, 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene, 2- (4 '-tert-butylphenyl) -5- (4' -biphenyl) -1,3, 4-oxadiazole, 2, 9-dimethyl-4, 7-diphenyl-1, 10-phenanthroline, and 4, 7-diphenyl-1, 10-phenanthroline.
In one embodiment, as shown in fig. 3, the present embodiment provides a method for manufacturing an electroluminescent device, which specifically includes the following steps:
step S110: an anode substrate is provided.
Specifically, the preparation method of the present embodiment is mainly applied to the preparation process of the electroluminescent device in the foregoing embodiment, and thus, taking the electroluminescent device 100 of fig. 1 as an example, each method step of the present embodiment will be described correspondingly.
As shown in fig. 1, an anode substrate is provided, and the anode substrate may specifically be a substrate on which an anode 110 is evaporated or sputtered, and when the prepared electroluminescent device is in a bottom emission structure, the anode may be a conductive transparent oxide such as ITO, IZO, AZO, IGZO, and when the prepared quantum dot electroluminescent device is in a top emission structure, the anode may also be a metal such as Ag, au, al, mg, or a metal alloy.
Step S120: and arranging a hole transmission layer on the anode substrate, wherein the hole transmission layer is divided into a semi-wetting region, and 5% -10% of organic solution is remained in the semi-wetting region by the total mass of the semi-wetting region so as to form the semi-wetting region.
Specifically, as shown in fig. 3, a hole transport layer 120 is disposed on the anode substrate, where the hole transport layer 120 is divided into semi-moist areas, and the specific manner of disposing the hole transport layer 120 may be to dispose a first film layer 121 on the anode 110 of the anode substrate, and then dispose a second film layer 122 on the first film layer 121, so as to form the hole transport layer 120 divided into semi-moist areas through the first film layer 121 and the second film layer 122 together.
As shown in fig. 1, a first film layer 121 is disposed on an anode 110 of an anode substrate, and specifically, the first film layer 121 may be prepared by a solution method, that is, an organic solution containing a conductive polymer is spin-coated, ink-jet printed, or slit-coated on the substrate, and dried (may be vacuum reduced pressure drying or baking drying) to obtain the first film layer 121. The conductive polymer may specifically include a homopolymer formed from any one of an aniline monomer, a thiophene monomer, and a fluorene monomer, or a copolymer formed from any combination thereof. The thickness of the finally prepared first film layer 121 may be specifically 10nm to 50nm. Meanwhile, in order to effectively avoid damage to the surface of the first film 121 when the second film 122 is disposed, the conductive polymer of the first film 121 is a crosslinkable polymer, i.e. the conductive polymer thereof contains crosslinking groups.
As shown in fig. 1, the second film layer 122 is disposed on the first film layer 121, specifically, the second film layer 122 may be prepared by a solution method, that is, an organic solution containing a conductive polymer is spin-coated, ink-jet printed or slit-coated on the first film layer 121, and a drying treatment (may be a vacuum decompression drying treatment or a baking drying treatment) is performed to obtain the second film layer 122, and wherein, based on the total mass of the second film layer 122, 5% -10% of the organic solution remains in the second film layer 122, so that the second film layer 122 forms the semi-moist area. The conductive polymer may specifically include a homopolymer formed from any one of polyaniline, polythiophene, and polyfluorene, or a copolymer formed from any combination thereof. The thickness of the finally prepared second film 122 may be specifically 1nm to 10nm. Meanwhile, in order to facilitate the subsequent preparation of the light emitting layer 130 (especially the quantum dot light emitting layer of the QLED device) on the second film 122, the light emitting layer 130 (especially the quantum dot light emitting layer of the QLED device) is better partially embedded into the second film 122, i.e. the embedding effect is improved, and the conductive polymer of the second film 122 is a non-crosslinked polymer, i.e. the conductive polymer does not contain a crosslinking group.
As can be seen from the above, when the first film layer 121 and the second film layer 122 are both provided, the drying treatment may be vacuum reduced pressure drying treatment or baking drying treatment, and in this case, in order to make the first film layer 121 completely dry, 5% -10% of the organic solution is remained in the second film layer 122 based on the total mass of the second film layer 122, so that the second film layer 122 is in a semi-moist state.
In one aspect, taking the above drying process as an example of vacuum reduced pressure drying process, the following adjustment may be made to the drying process steps of providing the first film layer 121 and providing the second film layer 122: when the first film layer 121 is provided on the anode substrate, the first film layer 121 is subjected to a first vacuum reduced pressure drying process, and when the second film layer 122 is provided on the first film layer 121, the second film layer 122 is subjected to a second vacuum reduced pressure drying process. At this time, it is necessary to ensure that the first pressure at the time of the first vacuum reduced pressure drying process is smaller than the second pressure at the time of the second vacuum reduced pressure drying process, and/or that the first vacuum reduced pressure drying process lasts for a first duration longer than the second duration for which the second vacuum reduced pressure drying process lasts. That is, for those skilled in the art, the pressure during the vacuum reduced pressure drying process may be controlled to be different, the duration of the vacuum reduced pressure drying process may be controlled to be different, or the pressure and duration of the vacuum reduced pressure drying process may be controlled to be different, so that when the first film layer 121 is completely dried, 5% -10% of the organic solution is remained in the second film layer 122 based on the total mass of the second film layer 122, so that the second film layer 122 is in a semi-moist state. The first pressure may be specifically smaller than 10pa, and the second pressure may be specifically 1000pa to 10000pa. The first duration may be specifically greater than 5 minutes, and the second duration may be specifically less than 5 minutes. Taking the case that the pressure and duration of the vacuum reduced pressure drying process are simultaneously controlled to be different, the first vacuum reduced pressure drying process may be specifically performed to maintain the first film 121 at a pressure of 10pa for 10min, the second vacuum reduced pressure drying process may be specifically performed to maintain the second film 122 at a pressure of 5000pa for 4min, so that about 8% of the organic solution remains in the second film 122 based on the total mass of the second film 122 under the condition that the first film 121 is completely dried, and the second film 122 is in a semi-moist state.
On the other hand, taking the above drying process as an example, the drying process steps of providing the first film layer 121 and providing the second film layer 122 may be adjusted as follows: when the first film 121 is provided on the anode substrate, the first film 121 is subjected to a first bake-drying process, and when the second film 122 is provided on the first film 121, the second film 122 is subjected to a second bake-drying process. At this time, it is necessary to ensure that the first temperature at the time of the first bake-drying process is higher than the second temperature at the time of the second bake-drying process, and/or that the third duration of the first bake-drying process is longer than the fourth duration of the second bake-drying process. That is, for those skilled in the art, the temperature and duration of the two vacuum baking and drying processes may be controlled to be different, or the duration of the two baking and drying processes may be controlled to be different, so that the second film 122 is in a semi-moist state when the first film 121 is completely dried, and 5% -10% of the organic solution is remained in the second film 122 based on the total mass of the second film 122. The first temperature may be 150-300 deg.C, and the second temperature may be 50 deg.C
About 150 ℃. The third duration is specifically 15min to 60min, and the fourth duration is specifically 1min to 15min. Taking the example that the temperature and duration of the baking and drying process are different, the first baking and drying process may be performed on the first film 121 at 250 ℃ for 30min, the second baking and drying process may be performed on the second film 122 at 100 ℃ for 8min, so that about 6% of the organic solution remains in the second film 122 based on the total mass of the second film 122 when the first film 121 is completely dried, and the second film 122 is in a semi-moist state.
Step S130: and a light-emitting layer is arranged on the second film layer in the semi-moist state.
Specifically, as shown in fig. 1, the light-emitting layer 130 is disposed on the hole-transporting layer 120, specifically, the light-emitting layer 130 may be formed by a solution method, that is, a compound solution containing a light-emitting layer material is spin-coated, ink-jet printed or slit-coated on the second film 122 in a semi-wet state, at this time, since the second film 122 is in a semi-wet state, the light-emitting layer 130 (especially, the quantum dot light-emitting layer of the QLED device) to be formed is partially embedded into the second film 122, then, a baking drying treatment is performed to obtain the light-emitting layer 130, and after the baking temperature of the baking drying treatment is 100-180 ℃, at this time, both the light-emitting layer 130 and the second film 122 are completely dried, and at this time, the light-emitting layer 130 (especially, the quantum dot light-emitting layer of the QLED device) is partially embedded into the second film 122 of the hole-transporting layer 120, so as to increase the contact between the hole-transporting layer 120 and the light-emitting layer 130, increase the hole injection, and reduce the charge accumulation at the contact interface between the hole-transporting layer 120 and the light-emitting layer 130, thereby improving the performance and the service life of the device.
In addition, when the electroluminescent device is a QLED device, the light-emitting layer material may specifically include a quantum dot, where the quantum dot is at least one of a quantum dot with a single structure and a quantum dot with a core-shell structure, the single structure quantum dot is at least one of a group II-VI compound, a group III-V compound, and a group I-III-VI compound, the group II-VI compound is at least one of CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe and CdZnSTe, the group III-V compound is at least one of InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP, and the group I-III-VI compound is at least one of CuInS2, cuInSe2, and AgInS 2. The core of the quantum dot with the core-shell structure is selected from any one of the quantum dots with the single structure, and the shell material of the quantum dot with the core-shell structure is selected from at least one of CdS, cdTe, cdSeTe, cdZnSe, cdZnS, cdSeS, znSe, znSeS and ZnS. The solvent of the above compound solution may include any one of toluene, chlorobenzene and cyclohexylbenzene, or other aromatic hydrocarbon-containing compounds, and the thickness of the finally prepared light-emitting layer 130 may be 10nm to 50nm.
Step S140: a cathode is disposed on the light-emitting layer.
Specifically, as shown in fig. 1, the cathode 140 is prepared on the light emitting layer 130, specifically, the cathode 140 may be disposed on the light emitting layer 130 by evaporation or sputtering, and the cathode 140 may be a metal electrode such as Al, ag, mg, etc. When the electroluminescent device is prepared in a bottom emission structure, the thickness of the cathode 140 may be specifically 80nm to 150nm, and when the electroluminescent device is prepared in a top emission structure, the thickness of the cathode 140 may be specifically 5nm to 40nm.
In this way, in the electroluminescent device manufactured by the method for manufacturing an electroluminescent device according to the embodiment of the present application, the manufacturing process of the second film layer 122 of the hole transport layer 120 is optimized, so that the second film layer 122 is in a semi-moist state, and when the light emitting layer 130 (especially the quantum dot light emitting layer of the QLED device) of the electroluminescent device 100 is manufactured, the nano particles (especially the quantum dot nano particles of the quantum dot light emitting layer) in the light emitting layer 130 are partially embedded into the second film layer 122 in the semi-moist state, so that the contact between the hole transport layer 120 and the light emitting layer 130 (especially the quantum dot light emitting layer of the QLED device) can be increased, and the hole injection can be increased, so as to reduce the charge accumulation at the contact interface between the hole transport layer 120 and the light emitting layer 130 (especially the quantum dot light emitting layer of the QLED device), thereby improving the device performance and service life.
In addition, referring to fig. 2, in the method for manufacturing an electroluminescent device of the present embodiment, a hole injection layer 150 may be disposed between an anode substrate and a hole transport layer 120, where the hole injection layer 150 is disposed on the anode substrate 110 (specifically, the hole injection layer 150 may be formed by spin-coating, ink-jet printing or slit coating a solution containing a hole injection material on the anode substrate 110, and baking and drying the solution to obtain the hole injection layer, and the baking temperature of the baking and drying treatment is 180-250 ℃, and the thickness of the hole injection layer 150 may be 10-60 nm.
Referring to fig. 2, in the method for manufacturing an electroluminescent device of the present embodiment, an electron transport layer 160 may be disposed between a cathode 140 and a light emitting layer 130, the electron transport layer 160 may be disposed on the light emitting layer 130 (specifically, the process of disposing may be spin coating, ink jet printing or slit coating a solution containing an electron transport material on the light emitting layer 130, and baking and drying treatment is performed to obtain an electron injection layer 160. The electron transport material is a metal oxide ZnxMgyO, where x is 0.9 and y is 0.1. The baking temperature of the baking and drying treatment may be specifically 60 ℃ to 150 ℃, the thickness of the finally manufactured electron injection layer 160 may be specifically 10nm to 100 nm), and then the cathode 140 is disposed on the electron transport layer 160 by the method steps.
The technical solutions and effects of the present application will be described in detail by way of specific examples, comparative examples and experimental examples, which are only some examples of the present application, and are not intended to limit the present application in any way.
Example 1
The embodiment provides an electroluminescent device and a method for manufacturing the same, and the electroluminescent device structure is shown in fig. 2, where the electroluminescent device of the embodiment includes an anode 110, a hole injection layer 150, a hole transport layer 120, a light emitting layer 130, an electron transport layer 160, and a cathode 140 that are sequentially stacked.
The preparation method of the electroluminescent device in the embodiment comprises the following steps:
a hole injection layer 150 is disposed on the anode 110 of the anode substrate, the hole injection layer 150 is made of polythiophene, and the thickness of the hole injection layer 150 is 40nm;
a hole transport layer 120 is disposed on the hole injection layer 150, specifically, a first film 121 is disposed on the hole injection layer 150, and then a second film 122 is disposed on the first film 121 to form the hole transport layer 120 together with the second film 122 through the first film 121, wherein the first film 121 is a crosslinkable copolymer formed by copolymerizing aniline monomer and aniline monomer containing double bonds, the molar ratio of aniline monomer containing double bonds in the copolymer is 3%, the thickness of the first film 121 is 50nm, the second film 122 is a non-crosslinked homopolymer formed by aniline monomer, the thickness of the second film 122 is 1nm, and an organic solution accounting for 10% of the total mass remains in the second film 122;
A luminescent layer 130 is arranged on the hole transport layer 120, the luminescent layer 130 is specifically a quantum dot luminescent layer of a QLED device, the quantum dot material adopted by the luminescent layer is CdZnSe, and the thickness is 40nm;
an electron transport layer 160 is prepared on the light emitting layer 130, and the electron transport layer 160 is made of metal oxide Zn x Mg y O, where x is 0.9 and y is 0.1, the electron transport layer 160 has a thickness of 80nm.
A cathode 140 is disposed on the electron transport layer 160, the cathode 140 is an Al cathode, and the thickness of the cathode 140 is 120nm.
The current efficiency of the electroluminescent device of example 1 was 44cd/A at 1000nits, and the lifetime of the decay 5% was 9000h.
Example 2
The electroluminescent device of this embodiment 2 is different from the electroluminescent device of embodiment 1 only in the arrangement of the layers of the hole transport layer 120, specifically, the organic solution accounting for 10% of the total mass remains in the second layer 122 of embodiment 1, and the organic solution accounting for 5% of the total mass remains in the second layer 122 of embodiment 2.
The current efficiency of the electroluminescent device of example 2 was found to be 42cd/A at 1000nits, and the lifetime of the device was found to be 8500h at a decay of 5%.
Example 3
The electroluminescent device of this embodiment 3 is different from the electroluminescent device of embodiment 1 only in the arrangement of the layers of the hole transport layer 120, specifically, the first layer 121 of embodiment 1 is a crosslinkable copolymer formed by copolymerizing an aniline monomer and an aniline monomer containing a double bond, and the first layer 121 of this embodiment 3 is a non-crosslinked homopolymer formed by copolymerizing an aniline monomer.
The current efficiency of the electroluminescent device of example 3 was found to be 36cd/A at 1000nits, and the lifetime of the decay 5% was 6200h.
Example 4
The electroluminescent device of this embodiment 4 is different from the electroluminescent device of embodiment 1 only in that the layer arrangement of the hole transport layer 120 is different from that of the hole transport layer, specifically, the second layer 122 of embodiment 1 is a non-crosslinked homopolymer formed by aniline monomer, and the second layer 122 of embodiment 4 is a crosslinkable copolymer formed by copolymerizing aniline monomer and aniline monomer containing double bonds, wherein the molar ratio of aniline monomer containing double bonds in the copolymer is 3%.
The current efficiency of the electroluminescent device of example 4 was 36cd/A at 1000nits, and the lifetime of the device was 6500h after 5% decay.
Example 5
The electroluminescent device of this embodiment 5 is different from the electroluminescent device of embodiment 1 only in the arrangement of the layers of the hole transport layer 120, specifically, the thickness of the first layer 121 of embodiment 1 is 50nm, the thickness of the second layer 122 is 1nm, and the thickness of the first layer 121 of this embodiment 5 is 30nm, and the thickness of the second layer 122 is 5nm.
The current efficiency of the electroluminescent device of example 5 was found to be 42cd/A at 1000nits, and the lifetime of the device was found to be 8500h after decay by 5%.
Example 6
The electroluminescent device of this embodiment 6 is different from the electroluminescent device of embodiment 1 only in the arrangement of the layers of the hole transport layer 120, specifically, the thickness of the first layer 121 of embodiment 1 is 50nm, the thickness of the second layer 122 is 1nm, and the thickness of the first layer 121 of this embodiment 6 is 10nm, and the thickness of the second layer 122 is 10nm.
The current efficiency of the electroluminescent device of example 6 was found to be 41cd/A at 1000nits, and the lifetime of the decay 5% was 8000h.
Example 7
The electroluminescent device of this embodiment 2 is different from the electroluminescent device of embodiment 1 only in the arrangement of the layers of the hole transport layer 120, specifically, the thickness of the first layer 121 of embodiment 1 is 50nm, the thickness of the second layer 122 is 1nm, and the thickness of the first layer 121 of embodiment 5 is 60nm, and the thickness of the second layer 122 is 15nm.
The current efficiency of the electroluminescent device of example 6 was 36cd/A at 1000nits, and the lifetime of the decay 5% was 6500h.
Example 8
The electroluminescent device of this embodiment 8 is different from the electroluminescent device of embodiment 1 only in that the layer arrangement of the hole transport layer 120 is different from that of the first layer 121 of embodiment 1, specifically, the first layer 121 of embodiment 1 is a crosslinkable copolymer formed by copolymerizing an aniline monomer and an aniline monomer containing a double bond, and the first layer 121 of embodiment 8 is a crosslinkable copolymer formed by copolymerizing an aniline monomer and a thiophene monomer containing a double bond, wherein the molar ratio of the thiophene monomer containing a double bond in the copolymer is 3%.
The current efficiency of the electroluminescent device of example 3 was 44cd/A at 1000nits, and the lifetime of the decay 5% was 8900h.
Example 9
The electroluminescent device of this embodiment 9 is different from the electroluminescent device of embodiment 1 only in that the layer arrangement of the hole transport layer 120 is different from that of the hole transport layer, specifically, the second layer 122 of embodiment 1 is a non-crosslinked homopolymer formed by aniline monomer, and the first layer 121 of this embodiment 8 is a non-crosslinked copolymer formed by copolymerization of aniline monomer and fluorene monomer.
The current efficiency of the electroluminescent device of example 3 was 44cd/A at 1000nits, and the lifetime of the decay 5% was 8900h.
Comparative example 1
The electroluminescent device of this comparative example 1 differs from the electroluminescent device of example 1 only in the hole transport layer 120 provided therewith, and at the same time, the hole transport layer is provided in the following manner: the hole transport layer 120 was disposed on the hole injection layer 150 by ink-jet printing, and the hole transport layer 120 was formed of only a homopolymer of polyaniline, and the thickness of the hole transport layer 120 was 40nm, i.e., the hole transport layer of comparative example 1 was a conventional structure prepared conventionally.
The current efficiency of the electroluminescent device of the comparative example is 35cd/A at 1000nits, and the lifetime of the electroluminescent device of the comparative example after 5% decay is 6000h.
By comparing the comparative example 1 with the examples 1 to 9, it can be demonstrated that the current efficiency (i.e., device performance) and the service life of the electroluminescent device prepared by the preparation method of the embodiment of the present application are greatly improved compared with the conventional electroluminescent device. By comparison of examples 1-9, it can be demonstrated that when the first layer 121 of the hole transport layer 120 is a crosslinkable polymer and the second layer 122 is a non-crosslinked polymer, the thicknesses of the first layer 121 and the second layer 122 are within the values given in the above claims, and the values of the organic solution remaining in the second layer 122 are also within the values given in the above claims, the current efficiency (i.e., device performance) and the service life thereof are greatly improved. When the first film 121 is made of a non-crosslinked polymer, or the second film is made of a crosslinkable polymer, or the thicknesses of the first film 121 and the second film 122 are not within the range of values given in the above claims, the current efficiency (i.e., device performance) and the life-span of the device are reduced to different extents.
The electroluminescent device and the preparation method thereof provided by the embodiment of the present application are described in detail, and specific examples are applied to illustrate the principle and the implementation of the present application, and the description of the above embodiments is only used to help understand the method and the core idea of the present application; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present application, the present description should not be construed as limiting the present application.
Claims (15)
1. An electroluminescent device comprising an anode, a hole transport layer, a light emitting layer, and a cathode, wherein the light emitting layer is partially embedded in the hole transport layer at a side adjacent to the hole transport layer.
2. The electroluminescent device of claim 1, wherein the hole transport layer comprises a first film layer and a second film layer that are stacked, and a side portion of the light emitting layer adjacent to the hole transport layer is partially embedded in the second film layer.
3. The electroluminescent device of claim 2, wherein the first film layer and the second film layer are both conductive polymer layers.
4. An electroluminescent device according to claim 3, wherein the conductive polymer used in the conductive polymer layer comprises a homopolymer formed from any one or any combination of aniline monomer, thiophene monomer, and fluorene monomer.
5. An electroluminescent device according to claim 3 or 4, characterized in that the conductive polymer of the first film layer is a crosslinkable polymer; and/or the conductive polymer of the second film layer is a non-crosslinked polymer.
6. The electroluminescent device of claim 1, wherein the first film layer has a thickness of 10nm to 50nm; and/or the thickness of the second film layer is 1 nm-10 nm.
7. The electroluminescent device of claim 1, wherein the anode is a metal oxide electrode selected from at least one of ITO, FTO, ATO, AZO, GZO, IZO, MZO and AMO, or a composite electrode of AZO/Ag/AZO, AZO/Al/AZO, ITO/Ag/ITO, ITO/Al/ITO, znO/Ag/ZnO, znO/Al/ZnO, tiO2/Ag/TiO2, tiO2/Al/TiO2, znS/Ag/ZnS, or ZnS/Al/ZnS;
and/or the light-emitting layer comprises quantum dots, an The quantum dot is selected from at least one of single-structure quantum dot and core-shell structure quantum dot, the single-structure quantum dot is selected from at least one of II-VI compound, III-V compound and I-III-VI compound, the II-VI compound is selected from at least one of CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe and CdZnSTe, the III-V compound is selected from at least one of InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP, and the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 At least one of (a) and (b); the core of the quantum dot with the core-shell structure is selected from any one of the quantum dots with the single structure, and the shell material of the quantum dot with the core-shell structure is selected from at least one of CdS, cdTe, cdSeTe, cdZnSe, cdZnS, cdSeS, znSe, znSeS and ZnS;
and/or the cathode is selected from at least one of an Ag electrode, an Al electrode, an Au electrode, a Pt electrode or an alloy electrode.
8. The electroluminescent device of claim 1, further provided with a hole injection layer between the anode and the hole transport layer; and/or, the electroluminescent device is further provided with an electron transport layer between the cathode and the light emitting layer.
9. A method for manufacturing an electroluminescent device, comprising the steps of:
providing an anode substrate;
a hole transport layer is arranged on the anode substrate, the hole transport layer is divided into semi-moist areas,
wherein, based on the total mass of the semi-wetting zone, 5% -10% of organic solution is remained in the semi-wetting zone to form the semi-wetting zone;
providing a luminescent layer on the semi-wetting region;
a cathode is disposed on the light emitting layer.
10. The method according to claim 9, wherein the step of disposing a hole transport layer on the anode substrate specifically comprises:
a first film layer is arranged on the anode substrate;
and a second film layer is arranged on the first film layer, wherein 5% -10% of organic solution is remained in the second film layer according to the total mass of the second film layer, so that the second film layer forms the semi-wetting zone.
11. The method according to claim 10, wherein when a first film layer is provided on the anode substrate, a first vacuum reduced pressure drying treatment is performed on the first film layer, and when a second film layer is provided on the first film layer, a second vacuum reduced pressure drying treatment is performed on the second film layer; the first pressure at the time of the first vacuum reduced pressure drying process is less than the second pressure at the time of the second vacuum reduced pressure drying process, and/or the first vacuum reduced pressure drying process lasts for a first duration that is greater than the second duration that the second vacuum reduced pressure drying process lasts.
12. The method of claim 11, wherein the first pressure is less than 10pa, and/or the second pressure is between 1000pa and 10000pa, and/or the first duration is greater than 5min, and/or the second duration is less than 5min.
13. The method according to claim 10, wherein when a first film layer is provided on the anode substrate, a first bake-drying treatment is performed on the first film layer, and when a second film layer is provided on the first film layer, a second bake-drying treatment is performed on the second film layer; the first temperature at the first bake-drying process is higher than the second temperature at the second bake-drying process, and/or the first bake-drying process lasts for a third duration that is greater than a fourth duration that the second bake-drying process lasts.
14. The method of preparation according to claim 13, wherein the first temperature is 150-300 ℃, and/or the second temperature is 50-150 ℃, and/or the third duration is 15-60 min, and/or the fourth duration is 1-15 min.
15. The method according to any one of claims 9 to 14, further comprising the steps of:
Providing a hole injection layer between the anode substrate and the hole transport layer; and/or an electron transport layer is provided between the cathode and the light emitting layer.
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| CN202210420916.7A CN116997199A (en) | 2022-04-20 | 2022-04-20 | Electroluminescent device and preparation method thereof |
| PCT/CN2022/142639 WO2023202142A1 (en) | 2022-04-20 | 2022-12-28 | Hole transport thin film, electroluminescent device, and preparation method therefor |
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