CN104078574A - Organic light-emitting diode device and manufacturing method thereof - Google Patents
Organic light-emitting diode device and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to an organic light-emitting diode device and a manufacturing method thereof. The organic light-emitting diode device is of a layer structure, the layer structure is formed by sequentially stacking an anode conductive substrate, a hole injection layer, a hole transmission layer, a light-emitting layer, an electron transmission layer, an electron injection layer and a cathode layer, and the surface of the cathode layer is provided with a mixed barrier layer and an inorganic barrier layer which are alternatively stacked. The organic light-emitting diode device adopts mixed layers formed by co-evaporating alloy, a rhenium oxide and organic substance as barrier layers, the co-evaporating compactness of the rhenium oxide and the organic substance is good, and the barrier capacity of the alloy is good, so that erosion of water, oxygen and other active substrate in the outside to the organic light-emitting diode device can be effectively reduced, accordingly an organic function material and electrodes of the organic light-emitting diode device are effectively protected, the sealing performance requirement of package is met, and the service life of the OLED device can be remarkably prolonged.
Description
Technical Field
The invention relates to the field of photoelectronic devices, in particular to an organic electroluminescent device. The invention also relates to a preparation method of the organic electroluminescent device.
Background
Organic electroluminescent devices (OLEDs) are a class of current-mode semiconductor light-emitting devices based on organic materials. The typical structure is that a luminescent layer with the thickness of dozens of nanometers is made on ITO glass by organic luminescent materials, and a metal electrode with low work function is arranged above the luminescent layer. When a voltage is applied across the electrodes, the light-emitting layer generates light radiation.
The OLED device has the advantages of active light emission, high light emitting efficiency, low power consumption, lightness, thinness, no viewing angle limitation, and the like, and is considered by the industry as a new generation device which is most likely to occupy an dominating position in the future illumination and display device market. As a new lighting and display technology, OLED technology has developed rapidly over the last decade, with great success. As more and more illumination and display manufacturers are increasingly invested in research and development in the world, the industrialization process of the OLED is greatly promoted, so that the growth speed of the OLED industry is remarkable, and the day before large-scale mass production is reached.
Flexible products are the development trend of organic electroluminescent devices, but the problem of short service life generally exists at present, so the service life of the devices is directly influenced by the quality of the packaging technology. The invention mainly aims to provide an organic electroluminescent device and a preparation method thereof, and the packaging technology has the advantages of simple process, strong water and oxygen resistance (WVTR) and obviously prolonged service life of the flexible OLED device.
Disclosure of Invention
The invention aims to solve the problems and the defects of the prior art and provides an organic electroluminescent device and a preparation method thereof.
The technical scheme provided by the invention aiming at the technical problems is as follows: an organic electroluminescent device, the organic electroluminescent device is a laminated structure, the laminated structure is sequentially laminated as follows: an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer and a cathode layer; the surface of the cathode layer is provided with a mixed barrier layer and an inorganic barrier layer which are alternately stacked; wherein,
the mixed barrier layer is made of a mixture consisting of organic matters and oxides; the organic matter is one of N, N ' -diphenyl-N, N ' -di (1-naphthyl) -1,1 ' -biphenyl-4, 4 ' -diamine, 8-hydroxyquinoline aluminum, 4 ' -tri (N-3-methylphenyl-N-phenylamino) triphenylamine, 4, 7-diphenyl-1, 10-phenanthroline or 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene, and the oxide is Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The organic matter accounts for 50-70 mol% of the mixed barrier layer, and the oxide accounts for 30-50 mol% of the mixed barrier layer;
the inorganic barrier layer is made of a mixture of oxides, fluorides, alloys and sulfides, wherein the oxides are Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The fluoride is one of LiF and CeF2、MgF2、AlF3、CaF2Or BaF2The alloy is one of NiTi, AgCd, CuCd, CuAl, CuNi or AlZn, and the sulfide is CdS, PbS or FeS2One of CuS, ZnS or NiS;
the oxide accounts for 10-30 wt% of the inorganic barrier layer, the fluoride accounts for 20-70 wt% of the inorganic barrier layer, the alloy accounts for 10-30 wt% of the inorganic barrier layer, and the sulfide accounts for 10-20 wt% of the inorganic barrier layer.
The thickness of the mixed barrier layer is 200 nm-300 nm.
The thickness of the inorganic barrier layer is 200 nm-300 nm.
The number of the mixed barrier layers and the inorganic barrier layers which are alternately stacked is 4-6.
The hole injectionThe layer is made of MoO3Doping the mixed material into N, N '-diphenyl-N, N' -di (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine according to the doping concentration of 30 wt%;
the hole transport layer is made of 4, 4' -tri (carbazole-9-yl) triphenylamine;
the material of the luminescent layer is a doped mixed material formed by doping tris (2-phenylpyridine) iridium into 1,3, 5-tris (1-phenyl-1H-benzimidazole-2-yl) according to the doping concentration of 5 wt%;
the material of the electron transport layer is 4, 7-diphenyl-1, 10-phenanthroline;
the electron injection layer is made of CsN3A mixed material formed by doping 4, 7-diphenyl-1, 10-phenanthroline according to the doping concentration of 30 wt%;
the cathode layer is made of ZnS, Ag and ZnS which are sequentially laminated by adopting a vacuum evaporation method.
The invention also comprises a preparation method of the organic electroluminescent device, which comprises the following steps:
(a) preparing a hole injection layer, a hole transport layer, a luminescent layer, an electron transport layer, an electron injection layer and a cathode layer in sequence on an anode conducting layer of a cleaned anode conducting substrate by adopting a vacuum evaporation method;
(b) on the cathode layer, firstly, preparing a mixed barrier layer by adopting a vacuum evaporation method; preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation method; then, alternately laminating for a plurality of times in sequence to prepare a mixed barrier layer and an inorganic barrier layer; wherein,
the mixed barrier layer is made of a mixture consisting of organic matters and oxides; the organic matter is N, N ' -diphenyl-N, N ' -di (1-naphthyl) -1,1 ' -biphenyl-4, 4 ' -diamine, 8-hydroxyquinoline aluminum, 4 ' -tri (N-3-methylphenyl-N-phenylamino) triphenylamine, 4, 7-diphenyl-1, 10-phenanthroline or 1,3, 5-tri (1-One of phenyl-1H-benzimidazole-2-yl) benzene, wherein the oxide is Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The organic matter accounts for 50-70 mol% of the mixed barrier layer, and the oxide accounts for 30-50 mol% of the mixed barrier layer;
the inorganic barrier layer is made of a mixture of oxides, fluorides, alloys and sulfides, wherein the oxides are Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The fluoride is one of LiF and CeF2、MgF2、AlF3、CaF2Or BaF2The alloy is one of NiTi, AgCd, CuCd, CuAl, CuNi or AlZn, and the sulfide is CdS, PbS or FeS2One of CuS, ZnS or NiS;
the oxide accounts for 10-30 wt% of the inorganic barrier layer, the fluoride accounts for 20-70 wt% of the inorganic barrier layer, the alloy accounts for 10-30 wt% of the inorganic barrier layer, and the sulfide accounts for 10-20 wt% of the inorganic barrier layer.
The thickness of the inorganic barrier layer is 200 nm-300 nm; the thickness of the mixed barrier layer is 200 nm-300 nm.
In the step (a), the vacuum degree of the hole injection layer, the hole transport layer, the luminescent layer, the electron transport layer and the electron injection layer is 1 × 10-5Pa, the vacuum degree of the cathode layer is 3 multiplied by 10 during vacuum evaporation preparation-5Pa; the evaporation rate of the hole injection layer, the hole transport layer and the electron transport layer isThe evaporation rate of the luminescent layer and the electron injection layer isThe cathode layer has an evaporation rate of
In the step (b), the number of times of alternation of the mixed barrier layer and the inorganic barrier layer is 4-6 times.
In the step (b), when the vacuum evaporation is used for preparing the mixed barrier layer, the vacuum degree of the vacuum evaporation is 1 × 10-5Pa～1×10-3Pa, the evaporation rate of the vacuum evaporation isWhen the inorganic barrier layer is prepared by vacuum evaporation, the vacuum degree is 1 multiplied by 10-5Pa～1×10-3Pa。
Compared with the prior art, the organic electroluminescence device and the preparation method thereof have the following advantages: the mixed layer obtained by co-evaporating the alloy, the rhenium oxide and the organic matter is used as the barrier layer, the co-evaporating compactness of the rhenium oxide and the organic matter is good, and the alloy barrier capability is strong, so that the erosion of active substances such as external water, oxygen and the like to the organic electroluminescent device can be effectively reduced, the organic functional materials and the electrodes of the organic electroluminescent device are effectively protected, the requirement on the sealing performance of encapsulation is met, and the service life of the OLED device can be obviously prolonged.
Drawings
Fig. 1 is a schematic view of the structure of an organic electroluminescent device of the present invention.
Detailed Description
The present invention will be further described in detail with reference to the following examples.
The organic electroluminescent device of the present invention has a layered structure, and as shown in fig. 1, the layered structure includes an anode conductive substrate 101, a hole injection layer 102, a hole transport layer 103, a light emitting layer 104, an electron transport layer 105, an electron injection layer 106, a cathode layer 107, a mixed barrier layer 108, and an inorganic barrier layer 109, which are sequentially stacked.
In the organic electroluminescent device, a plurality of mixed barrier layers and inorganic barrier layers which are alternately laminated are arranged on the surface of the cathode layer. The number of the mixed barrier layers and the inorganic barrier layers which are alternately stacked is 4-6.
The mixed barrier layer is made of a mixture consisting of organic matters and oxides; the organic matter is one of N, N ' -diphenyl-N, N ' -di (1-naphthyl) -1,1 ' -biphenyl-4, 4 ' -diamine, 8-hydroxyquinoline aluminum, 4 ' -tri (N-3-methylphenyl-N-phenylamino) triphenylamine, 4, 7-diphenyl-1, 10-phenanthroline or 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene, and the oxide is Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The organic matter accounts for 50-70 mol% of the mixed barrier layer, and the oxide accounts for 30-50 mol% of the mixed barrier layer;
the inorganic barrier layer is made of a mixture of oxides, fluorides, alloys and sulfides, wherein the oxides are Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The fluoride is one of LiF and CeF2、MgF2、AlF3、CaF2Or BaF2The alloy is one of NiTi, AgCd, CuCd, CuAl, CuNi or AlZn, and the sulfide is CdS, PbS or FeS2One of CuS, ZnS or NiS;
the oxide accounts for 10-30 wt% of the inorganic barrier layer, the fluoride accounts for 20-70 wt% of the inorganic barrier layer, the alloy accounts for 10-30 wt% of the inorganic barrier layer, and the sulfide accounts for 10-20 wt% of the inorganic barrier layer.
The thickness of the mixed barrier layer is 200 nm-300 nm, and the thickness of the inorganic barrier layer is 200 nm-300 nm.
In the organic electroluminescent device, the anode conductive substrate 101 includes an anode conductive layer and a substrate, the substrate may be a glass substrate or an organic thin film substrate, the anode conductive layer may be made of conductive oxides, such as Indium Tin Oxide (ITO), aluminum-doped zinc oxide (AZO), indium-doped zinc oxide (IZO) or fluorine-doped zinc oxide (FTO), and the conductive oxides are prepared on the glass substrate, which are abbreviated as ITO glass, AZO glass, IZO glass, and FTO glass. The anode conductive substrate may be made by itself or may be commercially available. In practical applications, other suitable materials can be selected as the anode conductive substrate 101 according to requirements. In practical applications, a desired anode pattern of the organic electroluminescent device can be prepared on the anode conductive substrate 101. The anode conductive substrate 101 is conventional and will not be described herein.
In the organic electroluminescent device, the materials and thicknesses of other functional layers are as follows:
the hole injection layer is made of MoO3Doping the mixed material into N, N '-diphenyl-N, N' -di (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine according to the doping concentration of 30 wt%; the thickness is 10 nm;
the hole transport layer is made of 4, 4' -tri (carbazole-9-yl) triphenylamine; thickness of 30nm
The material of the luminescent layer is a doped mixed material formed by doping tris (2-phenylpyridine) iridium into 1,3, 5-tris (1-phenyl-1H-benzimidazole-2-yl) according to the doping concentration of 5 wt%; the thickness is 20 nm;
the material of the electron transport layer is 4, 7-diphenyl-1, 10-phenanthroline; the thickness is 10 nm;
the electron injection layer is made of CsN3A mixed material formed by doping 4, 7-diphenyl-1, 10-phenanthroline according to the doping concentration of 30 wt%; the thickness is 20 nm.
The cathode layer is made of ZnS, Ag and ZnS which are sequentially laminated, and the thickness of the cathode layer is 30 nm.
The preparation method of the organic electroluminescent device comprises the following steps:
(a) preparing a hole injection layer, a hole transport layer, a luminescent layer, an electron transport layer, an electron injection layer and a cathode layer in sequence on an anode conducting layer of a cleaned anode conducting substrate by adopting a vacuum evaporation method;
the vacuum degree of the hole injection layer, the hole transport layer, the luminescent layer, the electron transport layer, the electron injection layer and the cathode layer is 1 multiplied by 10 when the hole injection layer, the hole transport layer, the luminescent layer, the electron transport layer, the electron injection layer and the cathode layer are prepared by vacuum evaporation-5Pa; the evaporation rates of the hole injection layer, the hole transport layer and the electron transport layer areThe light emitting layer and the electron injection layer have evaporation rates ofThe evaporation rate of the cathode layer is
(b) On the cathode layer, firstly, preparing a mixed barrier layer by adopting a vacuum evaporation method; preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation method; then, alternately laminating the prepared mixed barrier layer and the inorganic barrier layer for a plurality of times in sequence; the number of times of alternating the mixed barrier layer and the inorganic barrier layer is 4-6.
When the mixed barrier layer is prepared by vacuum evaporation, the vacuum degree of the vacuum evaporation is 1 multiplied by 10-5Pa～1×10-3Pa, the evaporation rate of the vacuum evaporation isWhen the inorganic barrier layer is prepared by vacuum evaporation, the vacuum degree is 1 multiplied by 10-5Pa～1×10-3Pa。
The mixed barrier layer is made of a mixture consisting of organic matters and oxides; the organic substance is N, N ' -diphenyl-N, N ' -di (1-naphthyl) -1,1 '-biphenyl-4, 4 '-diamine, 8-hydroxyquinoline aluminum, 4', 4 "-tris (N-3-methylphenyl-N-phenylamino) triphenylamine, 4, 7-diphenyl-1, 10-phenanthroline or 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene, the oxide being Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The organic matter accounts for 50-70 mol% of the mixed barrier layer, and the oxide accounts for 30-50 mol% of the mixed barrier layer;
the inorganic barrier layer is made of a mixture of oxides, fluorides, alloys and sulfides, wherein the oxides are Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The fluoride is one of LiF and CeF2、MgF2、AlF3、CaF2Or BaF2The alloy is one of NiTi, AgCd, CuCd, CuAl, CuNi or AlZn, and the sulfide is CdS, PbS or FeS2One of CuS, ZnS or NiS;
the oxide accounts for 10-30 wt% of the inorganic barrier layer, the fluoride accounts for 20-70 wt% of the inorganic barrier layer, the alloy accounts for 10-30 wt% of the inorganic barrier layer, and the sulfide accounts for 10-20 wt% of the inorganic barrier layer.
The thickness of the mixed barrier layer is 200 nm-300 nm, and the thickness of the inorganic barrier layer is 200 nm-300 nm.
The organic electroluminescent device and the production steps thereof of the present invention are specifically described in examples 1 to 6 below:
example 1
The organic electroluminescent device in this embodiment is a layered structure, and the layered structure sequentially includes:
the organic electroluminescent device comprises an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, a cathode layer, a mixed barrier layer and an inorganic barrier layer.
In this embodiment, the following steps are specifically performed in sequence: ITO glass substrate and MoO3-NPB layer, TCTA layer, TPBI-Ir (ppy)3Layer, Bphen layer, CsN3-Bphen layer, ZnS/Ag/ZnS, TAPC-Re2O layer, Re2O-LiF-NiTi-CdS layer. (the diagonal "/" indicates a layered structure and the horizontal bar "-" indicates mutual doping.)
The organic electroluminescent device is prepared by adopting the following steps:
a) pretreatment of the ITO glass substrate: acetone cleaning → ethanol cleaning → deionized water cleaning → ethanol cleaning, wherein the cleaning is carried out by an ultrasonic cleaning machine, each time for 5 minutes, then blowing dry by nitrogen, and then baking by an oven for standby; the cleaned ITO glass needs to be subjected to surface activation treatment so as 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 the ITO glass substrate is 100 nm;
b) preparation of hole injection layer: adding MoO3Doping into NPB as hole injection material with doping concentration of 30wt%, thickness of 10nm, and vacuum degree of 1 × 10-5Pa, evaporation rate of
c) Preparation of hole transport layer: 4, 4' -tri (carbazole-9-yl) triphenylamine (TCTA) is adopted as a hole transport material, and the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 30 nm;
d) light-emitting layer: 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene (TPBI) is used as a host material, and tri (2-phenylpyridine) iridium (Ir (ppy) is used as a guest material3) Doping concentration 5% and vacuum degree 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
e) preparation of an electron transport layer: evaporating a layer of 4, 7-diphenyl-1, 10-phenanthroline (Bphen) as an electron transport layer on the luminescent layer, wherein the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 10 nm;
f) preparation of an electron injection layer: taking a Bphen electron injection layer as a host material of CsN3Doped into Bphen with doping concentration of 30wt% and vacuum degree of 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
g) preparing a cathode layer: the cathode adopts ZnS/Ag/ZnS, the thickness is 100nm, the vacuum degree is 1 multiplied by 10-5Pa, evaporation rate
h) Manufacturing a mixed barrier layer: preparing a mixed barrier layer on the cathode layer by vacuum evaporation, wherein the mixed barrier layer is prepared by doping and co-evaporating two substances, one is TAPC, and the other is Re2The proportion of O and TAPC is 40mol%, Re2The proportion of O is 60mol%, and the vacuum degree of the mixed barrier layer is 1 multiplied by 10-5Pa, evaporation rateThe thickness is 300 nm;
i) manufacturing an inorganic barrier layer: preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation mode, wherein the inorganic barrier layer is prepared by doping and co-evaporating four substances, and one is Re2O, another is LiF, the third is NiTi, the fourth is CdS, the oxide accounts for 20wt%, the fluoride accounts for 32wt%, and the alloy accounts for 32wt%The proportion is 30wt%, the proportion of sulfide is 18wt%, and the vacuum degree of the inorganic barrier layer is 1 multiplied by 10-5Pa, evaporation rateThe thickness is 250 nm;
j) repeating the steps h) and i)6 times alternately.
Example 2
The organic electroluminescent device in this embodiment is a layered structure, and the layered structure sequentially includes:
the organic electroluminescent device comprises an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, a cathode layer, a mixed barrier layer and an inorganic barrier layer.
In this embodiment, the following steps are specifically performed in sequence: ITO glass substrate and MoO3-NPB layer, TCTA layer, TPBI-Ir (ppy)3Layer, Bphen layer, CsN3-Bphen layer, ZnS/Ag/ZnS layer, ReO-CeF2Layer, ReO-CeF2-an AgCd-PbS layer. (the diagonal "/" indicates a layered structure and the horizontal bar "-" indicates mutual doping.)
The organic electroluminescent device is prepared by adopting the following steps:
a) pretreatment of the ITO glass substrate: acetone cleaning → ethanol cleaning → deionized water cleaning → ethanol cleaning, wherein the cleaning is carried out by an ultrasonic cleaning machine, each time for 5 minutes, then blowing dry by nitrogen, and then baking by an oven for standby; the cleaned ITO glass needs to be subjected to surface activation treatment so as 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 the ITO glass substrate is 100 nm;
b) preparation of hole injection layer: adding MoO3Doping into NPB as hole injection material with doping concentration of 30wt%, thickness of 10nm, and vacuum degree of 1 × 10-5Pa, evaporation rate of
c) Preparation of hole transport layer: 4, 4' -tri (carbazole-9-yl) triphenylamine (TCTA) is adopted as a hole transport material, and the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 30 nm;
d) light-emitting layer: 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene (TPBI) is used as a host material, and tri (2-phenylpyridine) iridium (Ir (ppy) is used as a guest material3) Doping concentration 5% and vacuum degree 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
e) preparation of an electron transport layer: evaporating a layer of 4, 7-diphenyl-1, 10-phenanthroline (Bphen) as an electron transport layer on the luminescent layer, wherein the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 10 nm;
f) preparation of an electron injection layer: taking a Bphen electron injection layer as a host material of CsN3Doped into Bphen with doping concentration of 30wt% and vacuum degree of 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
g) preparing a cathode layer: the cathode adopts ZnS/Ag/ZnS, the thickness is 100nm, the vacuum degree is 1 multiplied by 10-5Pa, evaporation rate
h) Manufacturing a mixed barrier layer: by vacuum evaporationPreparing a mixed barrier layer on the cathode layer, wherein the mixed barrier layer is prepared by doping and co-evaporating two substances, one is NPB, the other is ReO, the oxide accounts for 50mol%, the NPB accounts for 50mol%, and the vacuum degree of the mixed barrier layer is 5 multiplied by 10-5Pa, evaporation rate ofThe thickness is 250 nm;
i) manufacturing an inorganic barrier layer: preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation mode, wherein the inorganic barrier layer is prepared by doping and co-evaporating four substances, one is ReO, and the other is CeF2The third is AgCd, the fourth is PbS, the oxide accounts for 30wt%, the fluoride accounts for 40wt%, the alloy accounts for 10wt%, the sulfide accounts for 20wt%, and the vacuum degree of the mixed barrier layer is 5 multiplied by 10-5Pa, evaporation rateThe thickness is 300 nm;
j) repeating the steps h) and i)5 times alternately.
Example 3
The organic electroluminescent device in this embodiment is a layered structure, and the layered structure sequentially includes:
the organic electroluminescent device comprises an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, a cathode layer, a mixed barrier layer and an inorganic barrier layer.
In this embodiment, the following steps are specifically performed in sequence: ITO glass substrate and MoO3-NPB layer, TCTA layer, TPBI-Ir (ppy)3Layer, Bphen layer, CsN3-Bphen layer, ZnS/Ag/ZnS, Alq3-Re2O3Layer of Re2O3-MgF2-CuCd-FeS2And (3) a layer. (the diagonal "/" indicates a layered structure and the horizontal bar "-" indicates mutual doping.)
The organic electroluminescent device is prepared by adopting the following steps:
a) pretreatment of the ITO glass substrate: acetone cleaning → ethanol cleaning → deionized water cleaning → ethanol cleaning, wherein the cleaning is carried out by an ultrasonic cleaning machine, each time for 5 minutes, then blowing dry by nitrogen, and then baking by an oven for standby; the cleaned ITO glass needs to be subjected to surface activation treatment so as 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 the ITO glass substrate is 100 nm;
b) preparation of hole injection layer: adding MoO3Doping into NPB as hole injection material with doping concentration of 30wt%, thickness of 10nm, and vacuum degree of 1 × 10-5Pa, evaporation rate of
c) Preparation of hole transport layer: 4, 4' -tri (carbazole-9-yl) triphenylamine (TCTA) is adopted as a hole transport material, and the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 30 nm;
d) light-emitting layer: 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene (TPBI) is used as a host material, and tri (2-phenylpyridine) iridium (Ir (ppy) is used as a guest material3) Doping concentration 5% and vacuum degree 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
e) preparation of an electron transport layer: evaporating a layer of 4, 7-diphenyl-1, 10-phenanthroline (Bphen) as an electron transport layer on the luminescent layer, wherein the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 10 nm;
f) preparation of an electron injection layer: taking a Bphen electron injection layer as a host material of CsN3Doped into Bphen with doping concentration of 30wt% and vacuum degree of 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
g) preparing a cathode layer: the cathode adopts ZnS/Ag/ZnS, the thickness is 100nm, the vacuum degree is 1 multiplied by 10-5Pa, evaporation rate
h) Manufacturing a mixed barrier layer: preparing a mixed barrier layer on the cathode layer by adopting a vacuum evaporation mode, wherein the mixed barrier layer is prepared by doping and co-evaporating two substances, namely Alq3The other is Re2O3The proportion of oxide is 30mol%, Alq370mol% of the mixed barrier layer, and the vacuum degree of the mixed barrier layer is 5 multiplied by 10-5Pa, evaporation rate of the Mixed Barrier layerThe thickness is 200 nm;
i) manufacturing an inorganic barrier layer: preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation mode, wherein the inorganic barrier layer is prepared by doping and co-evaporating four substances, and one is Re2O3The other is MgF2The third is CuCd, the fourth is FeS2The oxide accounts for 10wt%, the fluoride accounts for 65wt%, the alloy accounts for 15wt%, the sulfide accounts for 10wt%, and the vacuum degree of the inorganic barrier layer is 5 multiplied by 10-5Pa, evaporation rateThe thickness is 200 nm;
j) repeating the steps h) and i)6 times alternately.
Example 4
The organic electroluminescent device in this embodiment is a layered structure, and the layered structure sequentially includes:
the organic electroluminescent device comprises an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, a cathode layer, a mixed barrier layer and an inorganic barrier layer.
In this embodiment, the following steps are specifically performed in sequence: ITO glass substrate and MoO3-NPB layer, TCTA layer, TPBI-Ir (ppy)3Layer, Bphen layer, CsN3-Bphen layer, ZnS/Ag/ZnS, ReO2-AlF3Layer, ReO2-AlF3-a layer of CuAl-CuS. (the diagonal "/" indicates a layered structure and the horizontal bar "-" indicates mutual doping.)
The organic electroluminescent device is prepared by adopting the following steps:
a) pretreatment of the ITO glass substrate: acetone cleaning → ethanol cleaning → deionized water cleaning → ethanol cleaning, wherein the cleaning is carried out by an ultrasonic cleaning machine, each time for 5 minutes, then blowing dry by nitrogen, and then baking by an oven for standby; the cleaned ITO glass needs to be subjected to surface activation treatment so as 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 the ITO glass substrate is 100 nm;
b) preparation of hole injection layer: adding MoO3Doping into NPB as hole injection material with doping concentration of 30wt%, thickness of 10nm, and vacuum degree of 1 × 10-5Pa, evaporation rate of
c) Preparation of hole transport layer: 4, 4' -tri (carbazole-9-yl) triphenylamine (TCTA) is adopted as a hole transport material, and the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 30 nm;
d) light-emitting layer: 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene (TPBI) is used as a host material, and tri (2-phenylpyridine) iridium (Ir (ppy) is used as a guest material3) Doping concentration 5% and vacuum degree 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
e) preparation of an electron transport layer: evaporating a layer of 4, 7-diphenyl-1, 10-phenanthroline (Bphen) as an electron transport layer on the luminescent layer, wherein the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 10 nm;
f) preparation of an electron injection layer: taking a Bphen electron injection layer as a host material of CsN3Doped into Bphen with doping concentration of 30wt% and vacuum degree of 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
g) preparing a cathode layer: the cathode adopts ZnS/Ag/ZnS, the thickness is 100nm, the vacuum degree is 1 multiplied by 10-5Pa, evaporation rate
h) Manufacturing a mixed barrier layer: preparing a mixed barrier layer on the cathode layer by adopting a vacuum evaporation mode, wherein the mixed barrier layer is prepared by doping and co-evaporating two substances, namely m-MTDATA and ReO2The oxide accounts for 35mol%, the m-MTDATA accounts for 65mol%, and the vacuum degree of the mixed barrier layer is 5 multiplied by 10-5Pa, evaporation rateThe thickness is 250 nm;
i) manufacturing an inorganic barrier layer: preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation mode, wherein the inorganic barrier layer is prepared by doping and co-evaporating four substances, namely ReO2The other is AlF3The third is CuAl, the fourth is CuS, the oxide accounts for 15wt%, the fluoride accounts for 54wt%, the alloy accounts for 20wt%, the sulfide accounts for 11wt%, and the vacuum degree of the inorganic barrier layer is 5 multiplied by 10-5Pa, evaporation rateThe thickness is 240 nm;
j) repeating the steps h) and i) for 4 times alternately.
Example 5
The organic electroluminescent device in this embodiment is a layered structure, and the layered structure sequentially includes:
the organic electroluminescent device comprises an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, a cathode layer, a mixed barrier layer and an inorganic barrier layer.
In this embodiment, the following steps are specifically performed in sequence: ITO glass substrate and MoO3-NPB layer, TCTA layer, TPBI-Ir (ppy)3Layer, Bphen layer, CsN3-Bphen layer, ZnS/Ag/ZnS, BCP-Re2O5Layer of Re2O5-CaF2-a layer of CuNi-ZnS. (the diagonal "/" indicates a layered structure and the horizontal bar "-" indicates mutual doping.)
The organic electroluminescent device is prepared by adopting the following steps:
a) pretreatment of the ITO glass substrate: acetone cleaning → ethanol cleaning → deionized water cleaning → ethanol cleaning, wherein the cleaning is carried out by an ultrasonic cleaning machine, each time for 5 minutes, then blowing dry by nitrogen, and then baking by an oven for standby; the cleaned ITO glass needs to be subjected to surface activation treatment so as 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 the ITO glass substrate is 100 nm;
b) preparation of hole injection layer: adding MoO3Doping into NPB as hole injection material with doping concentration of 30wt%, thickness of 10nm, and vacuum degree of 1 × 10-5Pa, evaporation rate of
c) Preparation of hole transport layer: 4, 4' -tri (carbazole-9-yl) triphenylamine (TCTA) is adopted as a hole transport material, and the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 30 nm;
d) light-emitting layer: 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene (TPBI) is used as a host material, and tri (2-phenylpyridine) iridium (Ir (ppy) is used as a guest material3) Doping concentration 5% and vacuum degree 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
e) preparation of an electron transport layer: evaporating a layer of 4, 7-diphenyl-1, 10-phenanthroline (Bphen) as an electron transport layer on the luminescent layer, wherein the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 10 nm;
f) preparation of an electron injection layer: taking a Bphen electron injection layer as a host material of CsN3Doped into Bphen with doping concentration of 30wt% and vacuum degree of 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
g) preparing a cathode layer: the cathode adopts ZnS/Ag/ZnS, the thickness is 100nm, the vacuum degree is 1 multiplied by 10-5Pa, evaporation rate
h) Manufacturing a mixed barrier layer: preparing a mixed barrier layer on the cathode layer by adopting a vacuum evaporation mode, wherein the mixed barrier layer is prepared by doping and co-evaporating two substances, one is BCP, and the other is Re2O5The proportion of the oxide is 45mol%, the proportion of the BCP is 55mol%, and the vacuum degree of the mixed barrier layer is 5 multiplied by 10-5Pa, evaporation rateThe thickness is 250 nm;
i) manufacturing an inorganic barrier layer: preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation mode, wherein the inorganic barrier layer is prepared by doping and co-evaporating four substances, and one is Re2O5The other is CaF2The third is CuNi, the fourth is ZnS, the oxide accounts for 25wt%, the fluoride accounts for 43wt%, the alloy accounts for 18wt%, the sulfide accounts for 14wt%, and the vacuum degree of the inorganic barrier layer is 5X 10-5Pa, evaporation rateThe thickness is 270 nm;
j) repeating the steps h) and i)6 times alternately.
Example 6
The organic electroluminescent device in this embodiment is a layered structure, and the layered structure sequentially includes:
the organic electroluminescent device comprises an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, a cathode layer, a mixed barrier layer and an inorganic barrier layer.
In this embodiment, the following steps are specifically performed in sequence: ITO glass substrate and MoO3-NPB layer, TCTA layer, TPBI-Ir (ppy)3Layer, Bphen layer, CsN3-Bphen layer, ZnS/Ag/ZnS, ReO2-AlF3Layer, ReO2-AlF3-a layer of CuA-CuS. (the diagonal "/" indicates a layered structure and the horizontal bar "-" indicates mutual doping.)
The organic electroluminescent device is prepared by adopting the following steps:
a) pretreatment of the ITO glass substrate: acetone cleaning → ethanol cleaning → deionized water cleaning → ethanol cleaning, wherein the cleaning is carried out by an ultrasonic cleaning machine, each time for 5 minutes, then blowing dry by nitrogen, and then baking by an oven for standby; the cleaned ITO glass needs to be subjected to surface activation treatment so as 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 the ITO glass substrate is 100 nm;
b) preparation of hole injection layer: adding MoO3Doping into NPB as hole injection material with doping concentration of 30wt%, thickness of 10nm, and vacuum degree of 1 × 10-5Pa, evaporation rate of
c) Preparation of hole transport layer: 4, 4' -tri (carbazole-9-yl) triphenylamine (TCTA) is adopted as a hole transport material, and the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 30 nm;
d) light-emitting layer: 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene (TPBI) is used as a host material, and tri (2-phenylpyridine) iridium (Ir (ppy) is used as a guest material3) Doping concentration 5% and vacuum degree 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
e) preparation of an electron transport layer: evaporating a layer of 4, 7-diphenyl-1, 10-phenanthroline (Bphen) as an electron transport layer on the luminescent layer, wherein the vacuum degree is 1 multiplied by 10-5Pa, evaporation rateThe evaporation thickness is 10 nm;
f) preparation of an electron injection layer: taking a Bphen electron injection layer as a host material of CsN3Doped into Bphen with doping concentration of 30wt% and vacuum degree of 1X 10-5Pa, evaporation rateEvaporation thickness 20 nm;
g) preparing a cathode layer: the cathode adopts ZnS/Ag/ZnS, the thickness is 100nm, the vacuum degree is 1 multiplied by 10-5Pa, evaporation rate
h) Manufacturing a mixed barrier layer: preparing a mixed barrier layer on the cathode layer by adopting a vacuum evaporation mode, wherein the mixed barrier layer is prepared by doping and co-evaporating two substances, namely TPBi and ReO3The proportion of oxide is 40mol%, the proportion of TPBi is 60mol%, and the vacuum degree is 1 multiplied by 10-3Pa, evaporation rateThe thickness is 250 nm;
i) manufacturing an inorganic barrier layer: preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation mode, wherein the inorganic barrier layer is prepared by doping and co-evaporating four substances, namely ReO2The other is AlF3The third is CuAl, the fourth is CuS, the oxide accounts for 20wt%, the fluoride accounts for 53wt%, the alloy accounts for 12wt%, the sulfide accounts for 15wt%, and the vacuum degree of the inorganic barrier layer is 5 multiplied by 10-5Pa, evaporation rateThe thickness is 240 nm;
j) repeating the steps h) and i)6 times alternately.
Performance testing
The organic electroluminescent devices according to the present invention of examples 1 to 6 above were subjected to the water oxygen resistance (WVTR) and transmittance test, and as can be seen from table 1 below, the water oxygen resistance reached 10-4g/m2The performance of the OLED is more than day, and the service life of the OLED light-emitting device manufactured by the OLED light-emitting device is more than 3790 hours on average.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| WVTR(g/m2/day) | 6.3E-4 | 6.7E-4 | 7.2E-4 | 7.6E-4 | 8.0E-4 | 8.5E-4 |
| Life (hours) | 3912 | 3869 | 3854 | 3825 | 3821 | 3790 |
Therefore, the organic electroluminescent device and the preparation method thereof have the following advantages:
1. the mixed layer obtained by co-evaporation of the alloy, the rhenium oxide and the organic matter is used as the barrier layer, the co-evaporation compactness of the rhenium oxide and the organic matter is good, and the alloy barrier capability is strong, so that the erosion of active substances such as external water, oxygen and the like to the organic electroluminescent device can be effectively reduced, the organic functional materials and the electrodes of the organic electroluminescent device are effectively protected, the requirement on the sealing performance of encapsulation is met, and the service life of the OLED device can be obviously prolonged. The water and oxygen resistance of the paint reaches 10-4g/m2The service life of the OLED light-emitting device manufactured by the method is more than 4800 hours on average.
2. The preparation method of the organic electroluminescent device is simple in preparation process and easy for large-area preparation, is particularly suitable for application of the flexible OLED device, solves the packaging problem of the flexible OLED, and promotes the development of flexible OLED products.
The above-mentioned embodiments are merely preferred examples of the present invention, and not intended to limit the present invention, and those skilled in the art can easily make various changes and modifications according to the main concept and spirit of the present invention, so that the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An organic electroluminescent device, the organic electroluminescent device is a laminated structure, the laminated structure is sequentially laminated as follows: an anode conductive substrate, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer and a cathode layer; the cathode layer is characterized in that mixed barrier layers and inorganic barrier layers which are alternately stacked are arranged on the surface of the cathode layer; wherein,
the mixed barrier layer is made of a mixture consisting of organic matters and oxides; the organic matter is N, N '-diphenyl-N, N' -di (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine8-hydroxyquinoline aluminum, 4' -tri (N-3-methylphenyl-N-phenylamino) triphenylamine, 4, 7-diphenyl-1, 10-phenanthroline or 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene, wherein the oxide is Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The organic matter accounts for 50-70 mol% of the mixed barrier layer, and the oxide accounts for 30-50 mol% of the mixed barrier layer;
the inorganic barrier layer is made of a mixture of oxides, fluorides, alloys and sulfides, wherein the oxides are Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The fluoride is one of LiF and CeF2、MgF2、AlF3、CaF2Or BaF2The alloy is one of NiTi, AgCd, CuCd, CuAl, CuNi or AlZn, and the sulfide is CdS, PbS or FeS2One of CuS, ZnS or NiS;
the oxide accounts for 10-30 wt% of the inorganic barrier layer, the fluoride accounts for 20-70 wt% of the inorganic barrier layer, the alloy accounts for 10-30 wt% of the inorganic barrier layer, and the sulfide accounts for 10-20 wt% of the inorganic barrier layer.
2. The organic electroluminescent device according to claim 1, wherein the thickness of the hybrid barrier layer is 200nm to 300 nm.
3. The organic electroluminescent device according to claim 1, wherein the inorganic barrier layer has a thickness of 200nm to 300 nm.
4. The organic electroluminescent device according to claim 1, wherein: the number of the mixed barrier layers and the inorganic barrier layers which are alternately stacked is 4-6.
5. The organic electroluminescent device according to claim 1, wherein:
the hole injection layer is made of MoO3Doping the mixed material into N, N '-diphenyl-N, N' -di (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine according to the doping concentration of 30 wt%;
the hole transport layer is made of 4, 4' -tri (carbazole-9-yl) triphenylamine;
the material of the luminescent layer is a doped mixed material formed by doping tris (2-phenylpyridine) iridium into 1,3, 5-tris (1-phenyl-1H-benzimidazole-2-yl) according to the doping concentration of 5 wt%;
the material of the electron transport layer is 4, 7-diphenyl-1, 10-phenanthroline;
the electron injection layer is made of CsN3A mixed material formed by doping 4, 7-diphenyl-1, 10-phenanthroline according to the doping concentration of 30 wt%;
the cathode layer is made of ZnS, Ag and ZnS which are sequentially laminated by adopting a vacuum evaporation method.
6. A preparation method of an organic electroluminescent device comprises the following steps:
(a) preparing a hole injection layer, a hole transport layer, a luminescent layer, an electron transport layer, an electron injection layer and a cathode layer in sequence on an anode conducting layer of a cleaned anode conducting substrate by adopting a vacuum evaporation method;
(b) on the cathode layer, firstly, preparing a mixed barrier layer by adopting a vacuum evaporation method; preparing an inorganic barrier layer on the mixed barrier layer by adopting a vacuum evaporation method; then, alternately laminating for a plurality of times in sequence to prepare a mixed barrier layer and an inorganic barrier layer; wherein,
the mixed barrier layer is made of a mixture consisting of organic matters and oxides; the organic matter is one of N, N ' -diphenyl-N, N ' -di (1-naphthyl) -1,1 ' -biphenyl-4, 4 ' -diamine, 8-hydroxyquinoline aluminum, 4 ' -tri (N-3-methylphenyl-N-phenylamino) triphenylamine, 4, 7-diphenyl-1, 10-phenanthroline or 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene, and the oxide is Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The organic matter accounts for 50-70 mol% of the mixed barrier layer, and the oxide accounts for 30-50 mol% of the mixed barrier layer;
the inorganic barrier layer is made of a mixture of oxides, fluorides, alloys and sulfides, wherein the oxides are Re2O、ReO、Re2O3、ReO2、Re2O5Or ReO3The fluoride is one of LiF and CeF2、MgF2、AlF3、CaF2Or BaF2The alloy is one of NiTi, AgCd, CuCd, CuAl, CuNi or AlZn, and the sulfide is CdS, PbS or FeS2One of CuS, ZnS or NiS;
the oxide accounts for 10-30 wt% of the inorganic barrier layer, the fluoride accounts for 20-70 wt% of the inorganic barrier layer, the alloy accounts for 10-30 wt% of the inorganic barrier layer, and the sulfide accounts for 10-20 wt% of the inorganic barrier layer.
7. The production method according to claim 6, wherein the thickness of the mixed barrier layer is 200nm to 300 nm; the thickness of the inorganic barrier layer is 200 nm-300 nm.
8. The production method according to claim 6, wherein in the step (a), the degree of vacuum of the hole injection layer, the hole transport layer, the light-emitting layer, the electron transport layer, the electron injection layer and the cathode layer is 1X 10 when the layers are prepared by vacuum evaporation-5Pa; the evaporation rate of the hole injection layer, the hole transport layer and the electron transport layer isThe evaporation rate of the luminescent layer and the electron injection layer isThe cathode layer has an evaporation rate of
9. The method according to claim 6, wherein in the step (b), the number of times of alternation of the mixed barrier layer and the inorganic barrier layer is 4 to 6.
10. The method according to claim 6, wherein in the step (b), the vacuum degree of the vacuum evaporation is 1 x 10 when the vacuum evaporation is used for preparing the mixed barrier layer-5Pa～1×10-3Pa, the evaporation rate of the vacuum evaporation isWhen the inorganic barrier layer is prepared by vacuum evaporation, the vacuum degree is 1 multiplied by 10-5Pa～1×10-3Pa。
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