Organic light emission diode and preparation method thereof

An electroluminescent device and luminescent technology, applied in the field of electric light sources, can solve problems such as short service life, poor OLED stability, and increased bandgap width, and achieve the effects of reducing production costs, high qualified rate of finished products, and improving production efficiency

Inactive Publication Date: 2014-09-10
OCEANS KING LIGHTING SCI&TECH CO LTD +2
3 Cites 1 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0005] However, in practical applications, it is found that the organic electroluminescent materials used in the organic functional layers of OLEDs are particularly sensitive to the intrusion of oxygen and water vapor, resulting in poor stability and short service life of OLEDs, which affects the popularization and application of OLEDs.
This is because oxygen is a triplet quencher, which significantly reduces the quantum efficiency of luminescence; on the other hand, the oxidation of oxygen to the luminescent layer will generate carbonyl compounds, which...
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Method used

A) ITO glass substrate pre-treatment: acetone cleaning→ethanol cleaning→deionized water cleaning→ethanol cleaning, all cleaned with an ultrasonic cleaner, single washing and cleaning for 5 minutes, then blowing dry with nitrogen, and drying in an oven for later use ;The cleaned ITO glass also needs surface activation treatment to increase the oxygen content of the conductive surface layer and improve the work function of the conductive layer surface; the thickness of ITO is 100nm;
As can be seen from the above, above-mentioned OLED device is by the organic matter barrier layer 5 and the inorganic matter barrier layer 6 that are alternately stacked and combined successively on the outer surface of cathode layer, through the synergistic effect of these two layers of barrier layers, effectively reduced water, Oxygen and other active substances can erode the organic electroluminescent device and effectively protect the organic functional materials and electrodes of the device, thereby significantly improving the stability of the OLED device and prolonging the service life of the OLED device. As shown in Table 1 below, the water vapor permeability of the OLED device is as high as 10-4g/m2·day, and its service life is as high as 6,500 hours or more. In addition, the barrier layer composed of the alternately stacked organic barrier layers 5 and inorganic barrier layers 6 has a high light transmittance.
Further, as a preferred embodiment of the present invention, an electron blocking layer 36 and a hole blocking layer 37 can also be set on the basis of the organic functional layer 3 as shown in Figure 1, wherein the electron blocking layer 36 is stacked and combined Between the hole transport layer 32 and the light emitting layer 33 , the hole blocking layer 37 is laminated and bonded between the light emitting layer 33 and the electron transport layer 34 , and its structure is shown in FIG. 2 . The arrangement of the electron blocking layer 36 and the hole blocking layer 37 can respectively trap electrons and holes in the light-emitting layer 33 as much as possible, so as to increase the probability of holes and electrons meeting in the light-emitting layer 33, so as to improve the recombination of the two. The amount of excitons formed, and the exciton energy is transferred to the luminescent material, thereby exciting the electrons of the luminescent material to transition from the ground state to the excited state, and the excited state energy is deactivated by radiation to generate photons and release light energy to achieve enhanced light-emitting layer 33 luminous intensity objects. For example, the electron blocking layer 36 can trap the electrons injected from the cathode layer 4 in the light emitting layer 33 as much as possible, and the hole blocking layer 37 can trap the holes injected from the anode layer 2 in the light emitting layer 33 as much as possible.
In this organic functional layer 3, the material selected for hole injection layer 31 can be MoO and N, N'-diphenyl-N, N'-two (1-naphthyl)-1,1' - Compounds of biphenyl-4,4'-diamine (NPB), wherein MoO3 preferably but not only accounts for 30 wt% of the total weight of the compound. Certainly, the material selected for the hole injection layer 31 may be other materials known in the art such as WO3, VOx or WOx. The thickness of the hole injection layer 31 can also be set according to the conventional thickness in the field. The arrangement of the hole injection layer 31 can effectively enhance the ohmic contact between it and the anode layer 2 , enhance the electrical conductivity, and improve the hole injection capability at the end of the anode layer 4 .
In this preferred embodiment, the hole-transport material in the organic blocking layer 5 material has a strong charge-giving property, and the electron-transport material has a strong charge-absorbing property, and is doped with each other by the hole-transport material and the electron-transport material, and both Combined with a high degree of amorphousness, a film with high density, good flatness and minimal stress is formed, which is beneficial to the film formation of the inorganic barrier layer 6, and at the same time makes the stress of the film layer extremely small, effectively preventing the inorganic barrier layer 6 from cracking , the strength of the laminated combination of the organic barrier layer 5 and the inorganic barrier layer 6 is enhanced, and the film-forming quality of the organic barrier layer 5 and the inorganic barrier layer 6 is guaranteed.
Known from above, the preparation method of above-mentioned organic electroluminescent device prepares alternately laminated organic blocking layer 5 and the inorganic substance blocking layer 6 respectively on cathode layer outer surface successively by vapor deposition and sputtering method, makes alternately stacked and combined The organic barrier layer 5 and the inorganic barrier layer 6 play a synergistic effect and effectively isolate th...
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Abstract

The invention discloses an organic light emission diode (OLED) and a preparation method thereof. The organic light emission diode is composed of a transparent substrate layer, an anode layer, an organic functional layer, a cathode layer, an organic barrier layer and an inorganic barrier layer, wherein the transparent substrate layer, the anode layer, the organic functional layer, and the cathode layer are successively laminated and combined and the organic barrier layer and the inorganic barrier layer are successively and alternately laminated and combined. Materials used by the inorganic barrier layer include tellurides, selenides, and oxides, wherein the components are mutually doped; the tellurides account for 10% to 30%, by weight, of the total weight of the inorganic barrier layer materials; and the selenides account for 10% to 30%, by weight, of the total weight of the inorganic barrier layer materials. According to the organic light emission diode provided by the invention, corrosion of active materials like water and oxygen and the like on the organic light emission diode can be effectively reduced, thereby obviously improving the stable performance of the OLED and prolonging the service life of the OLED. Besides, the preparation method has advantages of simple process, easily-controlled condition, and easily-large area preparation.

Application Domain

Solid-state devicesSemiconductor/solid-state device manufacturing +1

Technology Topic

Organic electroluminescenceAmount of substance +9

Image

  • Organic light emission diode and preparation method thereof
  • Organic light emission diode and preparation method thereof
  • Organic light emission diode and preparation method thereof

Examples

  • Experimental program(8)
  • Effect test(1)

Example Embodiment

[0050] Correspondingly, the embodiments of the present invention also provide a method for preparing the organic electroluminescent device described above. The process flow diagram of the method is as follows image 3 Therefore, see also Figures 1 to 2 , the method includes the following steps:
[0051] S01. Provide a light-transmitting substrate layer 1;
[0052] S02. Preparation of anode layer 2: plating anode layer 2 on one surface of light-transmitting substrate layer 1 in step S01;
[0053] S03. Preparation of organic functional layer 3: in step S02, the surface of anode layer 2 opposite to the bonding surface of light-transmitting substrate layer 1 is sequentially plated with hole injection layer 31, hole transport layer 32, light-emitting layer 33, and electron transport layer 34 , an electron injection layer 35 to form an organic functional layer 3;
[0054] S04. Preparation of cathode layer 4: plating cathode layer 4 on the outer surface of organic functional layer 3 in step S03;
[0055] S05. Prepare an organic barrier layer 5 and an inorganic barrier layer 6 that are alternately stacked and combined with the outer surface of the cathode layer 4:
[0056] In the vacuum coating system, the organic material functional layer 5 is formed by doping and co-evaporating the organic material barrier layer material on the outer surface of the cathode layer 4;
[0057] In a vacuum system, the inorganic barrier layer 6 is formed by magnetron sputtering the inorganic barrier layer material on the outer surface of the organic functional layer 5;
[0058] The steps of preparing the organic functional layer 5 and the inorganic barrier layer 6 are sequentially repeated on the outer surface of the inorganic barrier layer 6 .
[0059] Specifically, in the above step S01, the structure, material and specifications of the light-transmitting substrate layer 1 are as described above, and for the sake of space, they will not be repeated here. In addition, in the S01 step, the pre-processing steps of the light-transmitting substrate layer 21, such as cleaning and decontamination steps, are also included.
[0060] In the above step S02 , the substrate is placed in a magnetron sputtering system to form a film by sputtering on the surface of the substrate to form the anode layer 2 . The sputtering conditions can adopt the conventional process conditions in the art.
[0061] Preferably, before performing the following step S03, the method further includes performing plasma treatment on the anode layer 2 in step S02: placing the substrate plated with the anode layer 2 in a plasma treatment chamber for plasma treatment. The plasma treatment conditions may adopt conventional process conditions in the art. After plasma treatment, the anode layer 2 can effectively improve the anode work function and reduce the injection barrier of holes.
[0062] Of course, a transparent substrate plated with an anode such as ITO can also be directly selected, and the transparent substrate plated with an anode is subjected to preliminary pretreatment, such as cleaning, plasma treatment, and the like, and then the following step S03 is performed.
[0063] In the above step S03, after the hole transport layer 31 is plated on the outer surface of the anode layer 2, the hole transport layer 32, the light-emitting layer 33, the electron transport layer 34, and the electron injection layer 35 are sequentially evaporated on the outer surface of the hole transport layer 31. , the materials selected for plating the layers and the uniform thickness are as described above. The process conditions involved in evaporating each layer may be in accordance with the conventional conditions in the art.
[0064] Further, when the organic functional layer 3 further contains an electron blocking layer 36 and a hole blocking layer 37, such as figure 2 shown. Therefore, in this step S03, the step of plating the electron blocking layer 36 after the hole transport layer 32 and the plating of the light emitting layer 33 also includes the step of plating the electron blocking layer 36, and after the step of plating the light emitting layer 33 and the plating of the electron transport layer 34, it also includes plating the hole blocking layer 37 A step of. The materials and thicknesses selected for the plating of the electron blocking layer 36 and the hole blocking layer 37 are as described above, respectively. The process conditions involved in evaporating the two layers can be in accordance with the conventional conditions in the art.
[0065] In the above step S04 , the substrate coated with the organic functional layer 3 is placed in a coating system, and the cathode material described above is used as the coating source to coat the outer surface of the organic functional layer 3 to form the cathode layer 4 . The vapor deposition conditions can adopt the conventional process conditions in the art.
[0066] In the above step S05, in the step of plating the organic functional layer 5, the organic functional layer 5 is formed by vapor deposition on the outside of the cathode layer 4 prepared in the above step S04 using the material selected for the organic functional layer 5 as a plating source.
[0067] Wherein, the material selected for the organic functional layer 5 is as described above, and the material preferably includes a hole transport material and an electron transport material doped with each other, wherein the hole transport material accounts for 40% of the total mole percent of the organic blocking layer material. %~60%. The hole transport material and the electron transport material are as described above, and in order to save space, they will not be repeated here. The organic materials doped with each other are co-evaporated to form the organic functional layer 5 . Of course, the organic material selected for the organic functional layer 5 can also be formed by vapor deposition using other organic materials commonly used in the art.
[0068] In a preferred embodiment, the process conditions for forming the organic functional layer 5 by evaporation are as follows:
[0069] The vacuum degree during co-evaporation of the materials selected for the organic functional layer 5 is 1×10 -5 Pa~1×10 -3 Pa, the evaporation rate of the material is The preferred vapor deposition process conditions can make the formed organic functional layer 5 more flat and dense. The evaporation time under the evaporation process conditions can be flexibly adjusted and controlled according to the thickness of the organic functional layer 5 .
[0070] In the above step S05, in the step of plating the inorganic barrier layer 6, the material selected for the inorganic barrier layer 6 plating is the inorganic material described above, and its materials include telluride, selenide and oxide; wherein, the selenide is The weight percentage of the total weight of the inorganic barrier material is 10% to 30%, the weight percentage of the telluride to the total weight of the inorganic barrier material is 10% to 30%, and the types of telluride, selenide and oxide are respectively As mentioned above, in order to save space, details are not repeated here.
[0071] In a preferred embodiment, the process conditions for forming the inorganic barrier layer 6 by magnetron sputtering are as follows:
[0072] The background vacuum in magnetron sputtering is 1×10 -5 Pa~1×10 -3 Pa. Wherein, the inert gas introduced in the magnetron sputtering can be an inert gas commonly used in the art, such as Ar. The preferred process conditions of magnetron sputtering can make the formed inorganic barrier layer 6 more dense, and the lamination and bonding with the above-mentioned organic functional layer 5 are more tightly and firmly. Under the process conditions of the magnetron sputtering, the magnetron sputtering time can be flexibly adjusted and controlled according to the thickness of the inorganic barrier layer 6 .
[0073] In the above-mentioned step S05, when the steps of repeatedly preparing the organic functional layer 5 and the inorganic barrier layer 6 are sequentially performed on the outer surface of the inorganic barrier layer 6, the number of times of repeating the preparation of the organic functional layer 5 and the inorganic barrier layer 6 is preferably 4 to 6. Of course, as mentioned above, the number of times of repeating the preparation of the organic functional layer 5 and the inorganic barrier layer 6 may be more than 1 time, less than 3 times or more than 7 times, and the specific number of stacking can be based on the organic electroluminescent device The light-emitting wavelength can be adjusted flexibly, so that the organic electroluminescent device can achieve the best light-emitting effect.
[0074] As can be seen from the above, the above-mentioned preparation method of the organic electroluminescent device prepares alternately stacked organic barrier layers 5 and inorganic barrier layers 6 on the outer surface of the cathode layer by evaporation and sputtering, respectively, so that the alternately stacked organic barrier layers are combined. 5 and the inorganic barrier layer 6 play a synergistic effect, effectively blocking the erosion of the organic electroluminescent device by active substances such as water and oxygen. In addition, by adjusting the process conditions of the coating, the organic barrier layer 5 and the inorganic barrier layer 6 are closely combined, flat and dense, thereby significantly prolonging the service life of the OLED device. The preparation method of the organic electroluminescent device has simple and mature procedures, easily controllable conditions, high yield of finished products, effectively improves production efficiency, reduces production cost, and is suitable for industrial production.
[0075] The organic electroluminescent device and the preparation method thereof according to the embodiments of the present invention will now be further described in detail with reference to specific examples.

Example Embodiment

[0076] Example 1
[0077] An organic electroluminescent device whose structure is: glass substrate/ITO/MoO 3 :NPB/TCTA/TPBI:Ir(ppy) 3 /Bphen/CsN 3 :Bphen/Al/(TPD:Bphen/Sb 2 Se 3 :MgO:Sb 2 Te 3 ) 6.
[0078] The preparation method of the organic electroluminescent device comprises the following steps:
[0079] a) Pre-treatment of ITO glass substrate: acetone cleaning → ethanol cleaning → deionized water cleaning → ethanol cleaning, all of which are cleaned with an ultrasonic cleaner, single cleaning for 5 minutes, then blown dry with nitrogen, and dried in an oven for use; The cleaned ITO glass also needs to be subjected to surface activation treatment to increase the oxygen content of the conductive surface layer and improve the work function of the surface of the conductive layer; the thickness of ITO is 100nm;
[0080]b) Preparation of organic functional layer: plating hole injection layer, hole transport layer, light emitting layer, electron transport layer and electron injection layer on the outer surface of the ITO layer in step a) in sequence; specifically,
[0081] Preparation of hole injection layer: MoO 3 Doped into N,N'-diphenyl-N,N'-bis(1-naphthyl)-1,1'-biphenyl-4,4'-diamine (NPB), the doping amount is 30wt %, thickness 10nm, vacuum degree 3×10 -5 Pa, evaporation rate
[0082] Preparation of hole transport layer: 4,4',4''-tris(carbazol-9-yl)triphenylamine (TCTA) was used as hole transport material, vacuum degree 3×10 -5 Pa, evaporation rate Evaporation thickness 30nm;
[0083] Preparation of light-emitting layer: the host material is 1,3,5-tris(1-phenyl-1H-benzimidazol-2-yl)benzene (TPBI), and the guest material is tris(2-phenylpyridine)iridium ( Ir(ppy) 3 ), the doping amount is 5wt%, the vacuum degree is 3×10 -5 Pa, evaporation rate Evaporation thickness 20nm;
[0084] Preparation of electron transport layer: A layer of 4,7-diphenyl-1,10-phenanthroline (Bphen) was evaporated as electron transport material, vacuum degree 3×10 -5 Pa, evaporation rate Evaporation thickness 10nm;
[0085] Preparation of the electron injection layer: the CsN 3 Doping into Bphen, the doping amount is 30wt%, the vacuum degree is 3×10 -5 Pa, evaporation rate Evaporation thickness 20nm;
[0086] c) Preparation of cathode layer: The cathode is made of Al, the thickness is 100 nm, and the vacuum degree is 3 × 10 -5 Pa, evaporation rate
[0087] d) Fabrication of organic blocking layer: The organic blocking layer is made of TPD as the hole transport material, and Bphen as the electron transport material. Prepared by vapor deposition, vacuum degree 1×10 -5 Pa, evaporation rate Thickness 300nm;
[0088] e) Fabrication of inorganic barrier layer: the inorganic barrier layer is made of telluride, selenide and oxide doped magnetron sputtering, and the selenide is Sb 2 Se 3 , the telluride is Sb 2 Te 3 , the oxide is MgO, where Sb 2 Se 3 The weight percentage of the total weight of the inorganic barrier material is 20%, Sb 2 Te 3 The weight percentage of the total weight of the inorganic barrier material is 30%, and the background vacuum degree of magnetron sputtering is 1×10 -5 Pa, thickness 200nm;
[0089] f) Alternately repeat d) and e) 6 times.

Example Embodiment

[0090] Example 2
[0091] An organic electroluminescent device whose structure is: glass substrate/ITO/MoO 3 :NPB/TCTA/TPBI:Ir(ppy) 3 /Bphen/CsN 3 :Bphen/Al/(BCP:NPB/MoSe 2 :Bi 2 Te:Al 2 O 3 ) 6.
[0092] The preparation method of the organic electroluminescent device comprises the following steps:
[0093] a), b), and c) are the same as in Example 1;
[0094] d) Fabrication of the organic blocking layer: The organic blocking layer is made of NPB as the hole transport material and BCP doping and co-evaporation as the electron transport material, wherein the hole transport material accounts for 50% of the total mole percentage of the organic blocking layer material. Vacuum Prepared by vapor deposition, vacuum degree 5×10 -5 Pa, evaporation rate Thickness 250nm;
[0095] e) Fabrication of inorganic barrier layer: the inorganic barrier layer is made of telluride, selenide and oxide doped magnetron sputtering, and the selenide is MoSe 2 , the telluride is Bi 2 Te, oxide is Al 2 O 3 , where MoSe 2 The weight percentage of the total weight of the inorganic barrier material is 15%, Bi 2 The weight percentage of Te in the total weight of the inorganic barrier material is 10%, and the background vacuum degree of magnetron sputtering is 1×10 -5 Pa, thickness 100nm;
[0096] f) Alternately repeat d) and e) 6 times.

PUM

PropertyMeasurementUnit
Thickness200.0 ~ 300.0nm
Thickness100.0 ~ 200.0nm
Thickness100.0nm

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