CN111312908A - OLED device and preparation method thereof - Google Patents
OLED device and preparation method thereof Download PDFInfo
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- CN111312908A CN111312908A CN201911092670.XA CN201911092670A CN111312908A CN 111312908 A CN111312908 A CN 111312908A CN 201911092670 A CN201911092670 A CN 201911092670A CN 111312908 A CN111312908 A CN 111312908A
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- H—ELECTRICITY
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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
- H10K50/125—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light
- H10K50/13—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light comprising stacked EL layers within one EL unit
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- H10K50/00—Organic light-emitting devices
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
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Abstract
The invention discloses an OLED device and a preparation method thereof, wherein the OLED device comprises a first electrode and a second electrode; the electron injection layer is arranged on one side, facing the first electrode, of the second electrode; at least two groups of light emitting structure layers which are laminated between the first electrode and the electron injection layer; and the charge generation layer is arranged between the two adjacent groups of the light emitting structure layers. The OLED device and the preparation method thereof have the advantages that the charge generation layer is added in the two light emitting structure layers, the charge generation layer transmits electrons to one side of the electron transmission layer and transmits holes to one side of the hole transmission layer, so that the light emitting efficiency of the OLED device is improved, and meanwhile, the light emitting structure layers and the charge generation layer are prepared by adopting an ink jet printing method, so that the cost is greatly reduced.
Description
Technical Field
The invention relates to the field of OLED, in particular to an OLED device and a preparation method thereof.
Background
Since OLEDs have advantages of high contrast, large viewing angle, fast response speed, light weight, flexibility, etc., they are widely used in flat panel display devices. At present, the small-size OLED product adopts vacuum evaporation and fine mask technology to realize RGB three-color display, and tends to be mature. However, the large-size OLED product has low yield and is discarded due to the fact that the mask plate is seriously warped and deformed after the size of the mask plate is increased, and the alignment difficulty is increased. Large-size color displays are currently generally realized by white light and color filter technologies. However, the vacuum evaporation white light adopts a multilayer structure, and has the defects of complex equipment and process, high energy consumption, large material waste, high cost and the like. After the organic functional material is prepared into ink by the OLED printing technology, the material is utilized to the maximum extent by solution processing technologies such as silk-screen printing or ink-jet printing, and the like, a fine metal mask plate is not needed, the cost can be effectively reduced, and the method has great advantages in the aspect of preparing large-size OLED panels.
The laminated OLED device has higher luminous efficiency, the luminous efficiency can be multiplied with the number of the laminated units, and more importantly, the service life of the laminated OLED device is longer than that of a single-layer OLED device. At present, the structure of the evaporation white OLED device is generally a laminated device structure, and mass production application is realized. However, the ink-jet printing of stacked devices has not been realized because the mutual solubility between layers in the solution process is problematic, and it is difficult to print one layer to avoid solvent penetration damage to the previous layer.
Disclosure of Invention
In order to solve the technical problems, the invention provides an OLED device and a preparation method thereof, which are used for solving the technical problems of high cost caused by complex process, high energy consumption and large material waste in the prior art for preparing a light emitting structure layer.
The technical scheme for solving the technical problems is as follows: the invention provides an OLED device, which comprises a first electrode and a second electrode; the electron injection layer is arranged on one side, facing the first electrode, of the second electrode; at least two groups of light emitting structure layers which are laminated between the first electrode and the electron injection layer; and the charge generation layer is arranged between the two adjacent groups of the light emitting structure layers.
Further, the light emitting structure layer includes a hole injection layer; a hole transport layer disposed on the hole injection layer; a light emitting layer disposed on the hole transport layer; an electron transport layer disposed on the light emitting layer; the hole injection layer in one light emitting structure layer is arranged on the first electrode, and the electron transmission layer in the other light emitting structure layer is arranged on the electron injection layer.
Further, the charge generation layer comprises a neutral layer arranged on one side of the hole injection layer of one of the light emitting structure layers; and the inorganic semiconductor layer is arranged between the neutral layer and the electron transmission layer of the other light-emitting structure layer.
Further, the thickness of the neutral layer is 5 nm-50 nm, the neutral layer is made of a polymer hole injection material, and the chemical structural formula is as follows:
the values of N and m are 2000-100000.
The thickness of the inorganic semiconductor layer is 5 nm-50 nm, and the material used by the nano particles in the inorganic semiconductor layer comprises at least one of ZnO, ZnMgO and TiOx.
Further, the thickness of the hole injection layer is 20 nm-200 nm, and the material of the hole injection layer comprises at least one of organic small molecule materials, polymer materials or inorganic oxide semiconductor materials; the hole transport layer is 20-200 nm thick and is made of poly [ (9, 9-dioctyl fluorene-2, 7-diyl) -co- (4,4'- (N- (4-sec-butylphenyl) diphenylamine) ], (N, N' -bis (4- (6- ((3-ethyl oxetan-3-yl) methoxy) -hexyloxy) phenyl-N, N '-bis (4-methoxyphenyl) biphenyl-4, 4' -diamine) ], the light emitting layer is an organic light emitting layer with a thickness of 20-100 nm, the electron transport layer is 20-60 nm thick and is made of a small molecule cross-linking material, and the cross-linking material comprises propylene oxide groups, styrene groups, trifluoroethylene ether groups, and a metal oxide layer, At least one crosslinking group of a benzocyclobutene group and a uracil group.
Further, the thickness of the electron injection layer is 0.5 nm-10 nm, and the material of the electron injection layer comprises at least one of LiF, NaF and Liq; the first electrode is an anode and is made of indium tin oxide; the second electrode is a cathode, the thickness of the second electrode is 100 nm-200 nm, and the second electrode is made of at least one of aluminum, silver, magnesium-silver alloy and indium zinc oxide.
The invention also provides a preparation method of the OLED device, which comprises the steps of preparing a layer of first electrode; preparing a first light-emitting structure layer on the first electrode in an ink jet printing mode; preparing a charge generation layer on the first light emitting structure layer; preparing a second light emitting structure layer on the charge generation layer by an ink jet printing mode; forming an electron injection layer on the second light emitting structure layer by a vacuum evaporation method; and forming a cathode layer on the electron injection layer by vacuum evaporation.
Further, the first light emitting structure layer is prepared by printing organic small molecule material ink or inorganic oxide semiconductor material ink on the anode layer, drying the printed ink in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a hole injection layer; printing a polymer material ink on the hole injection layer. After vacuum drying and film forming, removing residual solution by adopting a thermal annealing process to form a hole transport layer; printing organic light-emitting layer material ink on the hole transport layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a light-emitting layer; and printing small-molecule cross-linking material ink on the luminous layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form an electron transmission layer.
Further, the charge generation layer is specifically prepared by the following steps: printing inorganic oxide nano particle ink on the electronic transmission layer of the first light-emitting structure layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form an inorganic oxide semiconductor layer; and printing neutral polymer ink on the inorganic oxide semiconductor layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a neutral layer.
Further, the preparation step of the neutral polymer ink comprises the step of mixing an acidic polymer material with a sodium hydroxide solution to form a mixed solution until the pH value of the mixed solution is greater than or equal to 7.
The invention has the advantages that: according to the OLED device and the preparation method thereof, the charge generation layer is added in the two light emitting structure layers, the charge generation layer transmits electrons to one side of the electron transmission layer and transmits holes to one side of the hole transmission layer, so that the light emitting efficiency of the OLED device is improved, and meanwhile, the light emitting structure layers and the charge generation layer are prepared by adopting an ink jet printing method, so that the cost is greatly reduced.
Drawings
The invention is further explained below with reference to the figures and examples.
Fig. 1 is a schematic diagram of an OLED device in an embodiment.
Fig. 2 is a schematic diagram of an OLED device in a preferred embodiment.
In the drawings
10 an OLED device; 110 a first electrode;
120 light emitting structure layer; 1201 a first light emitting structure layer;
1202 a second light emitting structure layer; 130 a charge generation layer;
140 an electron injection layer; 150 a second electrode;
121 a hole injection layer; 122 a hole transport layer;
123 a light emitting layer; 124 an electron transport layer;
130 a charge generation layer; 131 a semiconductor layer;
132 a neutral layer;
Detailed Description
The following description of the embodiments refers to the accompanying drawings for illustrating the specific embodiments in which the invention may be practiced. The directional terms used in the present invention, such as "up", "down", "front", "back", "left", "right", "top", "bottom", etc., refer to the directions of the attached drawings. Accordingly, the directional terms used are used for explanation and understanding of the present invention, and are not used for limiting the present invention.
Examples
As shown in fig. 1, in the present embodiment, the OLED device 10 of the present invention includes a first electrode 110, an electron injection layer 140, a light emitting structure layer 120, a charge generation layer 130, and a second electrode 150.
The first electrode 110 is an anode and is made of indium tin oxide.
The light emitting structure layer 120 includes a first light emitting structure layer 1201 and a second light emitting structure layer 1202.
The first and second light emitting structure layers 1201 and 1202 each include a hole injection layer 121, a hole transport layer 122, a light emitting layer 123, and an electron transport layer 124.
The hole injection layer 121 has a thickness of 20nm to 200nm, and is made of a polymer material, such as poly [ (9, 9-dioctylfluorene-2, 7-diyl) -co- (4,4'- (N- (4-sec-butylphenyl) diphenylamine) ] (TFB) or a small-molecule cross-linked hole injection layer material, such as (N, N' -bis (4- (6- ((3-ethyloxetan-3-yl) methoxy) -hexyloxy) phenyl-N, N '-bis (4-methoxyphenyl) biphenyl-4, 4' -diamine (QUPD), which is a chemical reaction that allows cross-coupling between segments of cross-linking groups, such as propylene oxide groups, styrene groups, and trifluoroethylene ether groups, under ultraviolet light or high temperature, benzocyclobutene radical and uracil radical. The molecular structural formula is as follows:
wherein the value range of n and m is 2000-100000.
The hole transport layer 122 is disposed on the hole injection layer 121, has a film thickness ranging from 20nm to 200nm, and is made of a polymer material, such as poly [ (9, 9-dioctylfluorene-2, 7-diyl) -co- (4,4' - (N- (4-sec-butylphenyl) diphenylamine) ] (TFB), and has a molecular structural formula:
the material of the hole transport layer 122 can also be a small molecule cross-linked hole transport layer material, such as (N, N ' -bis (4- (6- ((3-ethyloxetan-3-yl) methoxy) -hexyloxy) phenyl-N, N ' -bis (4-methoxyphenyl) biphenyl-4, 4' -diamine (QUPD), having the molecular formula:
the crosslinking is a chemical reaction of cross-coupling between chain segments of crosslinking groups such as propylene oxide groups, styrene groups, trifluorovinyl ether groups, benzocyclobutene groups, uracil groups and the like under ultraviolet light or high temperature.
The light-emitting layer 123 is provided on the hole transport layer 122, and has a film thickness in the range of 20nm to 100nm, preferably 80 nm. The material of the light emitting layer 123 is a host and guest doped material system, wherein the host material is a host material with a molecular weight greater than 1000, and may be a small molecule host material such as 3,3 ', 6, 6' -tetrakis (9-phenyl-9H-carbazol-3-yl) benzophenone (tczbp), and its molecular structural formula:
or a polymeric host material such as poly (9-vinylcarbazole) PVK, having the molecular structure:
the guest material is a fluorescent luminescent material such as MADN, and the molecular structural formula of the guest material is as follows:
phosphorescent light emitting materials such as ir (mppy)3, having a molecular formula:
or a thermally activated delayed fluorescence material such as 4tCzIPN, having a molecular formula:
the electron transport layer 124 is disposed on the light emitting layer 123, and has a film thickness ranging from 20nm to 60nm, and is made of a small molecule cross-linked material, such as an epoxypropane group, a styrene group, a trifluorovinyl ether group, a benzocyclobutene group, and a uracil group.
The first light emitting structure layer 1201 is attached to the first electrode 110, and specifically, the hole injection layer 121 of the first light emitting structure layer 1201 is attached to the first electrode 110.
The first light emitting structure layer 1201 and the second light emitting structure layer 1202 are stacked, and a charge generation layer 130 is disposed between the first light emitting structure layer 1201 and the second light emitting structure layer 1202 for better electron transfer.
Specifically, the charge generation layer 130 includes a semiconductor layer 131 and a neutral layer 132.
The semiconductor layer 131 is an inorganic oxide semiconductor layer, has a film thickness ranging from 5nm to 50nm, is made of nano-particles of ZnO, ZnMgO or TiOx, and is disposed on the electron transport layer 124 side of the first light emitting structure layer 1201 to transport electrons to the electron transport layer 124.
The neutral layer 132 is a neutral polymer layer, has a film thickness ranging from 5nm to 50nm, and the neutral layer 132 is disposed on the hole injection layer 121 side of the second light emitting structure layer 1202 and is configured to transfer holes to the hole injection layer 121.
The electron injection layer 140 is disposed on the electron transport layer 124 side of the second light emitting structure layer 1202 for transferring electrons to the electron transport layer 124.
The second electrode 150 is a cathode, the thickness of the film is 10nm to 200nm, and the material is a low work function metal material or a low work function metal alloy or a transparent metal oxide. Such as aluminum, silver, magnesium-silver alloy, indium-zinc oxide, etc., for providing electrons.
As shown in fig. 2, in another preferred embodiment of the present invention, the light emitting structure layer 120 further includes a third light emitting structure layer 1203, wherein the same structure as the charge generation layer 130 is disposed between the second light emitting structure layer 1202 and the third light emitting structure layer 1203.
In order to better explain the present invention, this embodiment further provides a method for manufacturing an OLED device, including:
preparing a layer of first electrode; preparing a group of first light emitting structure layers on the first electrode; preparing a charge generation layer on the first light emitting structure layer; preparing a group of second light emitting structure layers on the charge generation layer; forming an electron injection layer on the second light emitting structure layer by a vacuum evaporation method; and forming a cathode layer on the electron injection layer by vacuum evaporation.
The preparation steps of the first light-emitting structure layer are as follows:
printing organic micromolecular material ink or inorganic oxide semiconductor material ink on the anode layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a hole injection layer, wherein the thermal annealing temperature range is 80-250 ℃.
Printing a polymer material ink on the hole injection layer. After vacuum drying and film forming, removing residual solution by adopting a thermal annealing process to form a hole transport layer, wherein the thermal annealing temperature range is 80-250 ℃.
Printing organic light-emitting layer material ink on the hole transport layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a light-emitting layer, wherein the thermal annealing temperature range is 80-180 ℃.
Printing micromolecule cross-linking material ink on the luminous layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form an electron transmission layer, wherein the thermal annealing temperature range is 80-150 ℃.
The charge generation layer is prepared by the following specific steps:
printing inorganic oxide nanoparticle ink on the electronic transmission layer of the first light-emitting structure layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form an inorganic oxide semiconductor layer, wherein the thermal annealing temperature range is 80-150 ℃.
Printing neutral polymer ink on the inorganic oxide semiconductor layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a neutral layer, wherein the thermal annealing temperature range is 80-150 ℃.
The preparation steps of the neutral polymer ink comprise:
mixing an acidic polymer material with a sodium hydroxide solution to form a mixed solution until the pH value of the mixed solution is greater than or equal to 7.
The step of preparing the second light emitting structure layer is the same as the step of preparing the first light emitting structure layer, except that the hole injection layer of the second light emitting structure layer is prepared on the neutral layer.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An OLED device, comprising
A first electrode and a second electrode;
the electron injection layer is arranged on one side, facing the first electrode, of the second electrode;
at least two groups of light emitting structure layers which are laminated between the first electrode and the electron injection layer;
and the charge generation layer is arranged between the two adjacent groups of the light emitting structure layers.
2. The OLED device of claim 1,
the light emitting structure layer comprises
A hole injection layer;
a hole transport layer disposed on the hole injection layer;
a light emitting layer disposed on the hole transport layer;
an electron transport layer disposed on the light emitting layer;
the hole injection layer in one light emitting structure layer is arranged on one side of the first electrode close to the second electrode, and the electron transmission layer in the other light emitting structure layer is arranged on the electron injection layer.
3. The OLED device of claim 2,
the charge generation layer comprises
The neutral layer is arranged on one side of the hole injection layer of one of the light-emitting structure layers;
and the inorganic semiconductor layer is arranged on one side of the neutral layer, which is far away from the light-emitting structure layer.
4. The OLED device of claim 3,
the thickness of the neutral layer is 5 nm-50 nm, the neutral layer is made of a polymer hole injection material, and the chemical structural formula is as follows:
the values of N and m are 2000-100000;
the thickness of the inorganic semiconductor layer is 5 nm-50 nm, and the material used by the nano particles in the inorganic semiconductor layer comprises at least one of ZnO, ZnMgO and TiOx.
5. The OLED device of claim 2,
the thickness of the hole injection layer is 20 nm-200 nm, and the material of the hole injection layer comprises at least one of organic micromolecule material, polymer material or inorganic oxide semiconductor material;
the thickness of the hole transport layer is 20-200 nm, and the material of the hole transport layer comprises poly [ (9, 9-dioctyl fluorene-2, 7-diyl) -co- (4,4'- (N- (4-sec-butylphenyl) diphenylamine) ], (N, N' -bis (4- (6- ((3-ethyl oxetan-3-yl) methoxy) -hexyloxy) phenyl-N, N '-bis (4-methoxyphenyl) biphenyl-4, 4' -diamine) ];
the light-emitting layer is an organic light-emitting layer, and the thickness of the light-emitting layer is 20 nm-100 nm;
the thickness of the electron transmission layer is 20 nm-60 nm, the material of the electron transmission layer comprises a micromolecule crosslinking material, and the crosslinking material comprises at least one crosslinking group of epoxypropane groups, styrene groups, trifluorovinyl ether groups, benzocyclobutene groups and uracil groups.
6. The OLED device of claim 1,
the thickness of the electron injection layer is 0.5 nm-10 nm, and the material of the electron injection layer comprises at least one of LiF, NaF and Liq;
the first electrode is an anode and is made of indium tin oxide;
the second electrode is a cathode, the thickness of the second electrode is 100 nm-200 nm, and the second electrode is made of at least one of aluminum, silver, magnesium-silver alloy and indium zinc oxide.
7. A method for preparing an OLED device is characterized in that,
preparing a layer of first electrode;
preparing a first light-emitting structure layer on the first electrode in an ink jet printing mode;
preparing a charge generation layer on the first light emitting structure layer;
preparing a second light emitting structure layer on the charge generation layer by an ink jet printing mode;
forming an electron injection layer on the second light emitting structure layer by a vacuum evaporation method;
and forming a cathode layer on the electron injection layer by vacuum evaporation.
8. The method of manufacturing an OLED device according to claim 7,
the first light-emitting structure layer is prepared by the following steps
Printing organic small molecular material ink or inorganic oxide semiconductor material ink on the anode layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a hole injection layer;
printing a polymer material ink on the hole injection layer. After vacuum drying and film forming, removing residual solution by adopting a thermal annealing process to form a hole transport layer;
printing organic light-emitting layer material ink on the hole transport layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a light-emitting layer;
and printing small-molecule cross-linking material ink on the luminous layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form an electron transmission layer.
9. The method for preparing the OLED device according to claim 8, wherein the charge generation layer is prepared by the following steps:
printing inorganic oxide nano particle ink on the electronic transmission layer of the first light-emitting structure layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form an inorganic oxide semiconductor layer;
and printing neutral polymer ink on the inorganic oxide semiconductor layer, drying in vacuum to form a film, and removing residual solution by adopting a thermal annealing process to form a neutral layer.
10. The method of claim 9, wherein the step of preparing the neutral polymer ink comprises
Mixing an acidic polymer material with a sodium hydroxide solution to form a mixed solution until the pH value of the mixed solution is greater than or equal to 7.
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Application publication date: 20200619 |