CN104124372A - Organic light-emitting device and preparation method thereof - Google Patents

Organic light-emitting device and preparation method thereof Download PDF

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Publication number
CN104124372A
CN104124372A CN201310143977.4A CN201310143977A CN104124372A CN 104124372 A CN104124372 A CN 104124372A CN 201310143977 A CN201310143977 A CN 201310143977A CN 104124372 A CN104124372 A CN 104124372A
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layer
work function
metal
evaporation
organic electroluminescence
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周明杰
黄辉
张振华
王平
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/805—Electrodes
    • H10K50/82—Cathodes
    • H10K50/826—Multilayers, e.g. opaque multilayers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/85—Arrangements for extracting light from the devices
    • H10K50/854—Arrangements for extracting light from the devices comprising scattering means
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/85—Arrangements for extracting light from the devices
    • H10K50/856—Arrangements for extracting light from the devices comprising reflective means

Abstract

The invention discloses an organic light-emitting device and a preparation method thereof. The organic light-emitting device is composed of a conductive anode glass substrate, a hole injection layer, a hole transport layer, a luminescent layer, an electron transport layer, an electron injection layer and a composite cathode, wherein the layers are successively laminated. The composite anode includes a silicon compound layer, a conductive thin film layer, and a metal doping layer, wherein the layers are successively laminated. The silicon compounds are in a particle shape and form a well-ordered microsphere structure; and on the basis of the structure, light scattering can be carried out, so that the light can be centralized in the middle for outgoing; and because of the conductive thin film layer, the electron injection efficiency can be effectively improved. The metal doping layer is formed by mixing high-work function metal with the work function of 4.0 to 5.5eV and low-work function metal with the work function of 4.02.0eV to 3.5e; the low-work function metal is conductive to electron injection; and the high-work function metal enables the stability of the composite electrode to be improved. Meanwhile, the metal doping layer scatters the light, so that the light can be reflected to the bottom of the device.

Description

A kind of organic electroluminescence device and preparation method thereof
Technical field
The present invention relates to organic electroluminescent field, particularly a kind of organic electroluminescence device and preparation method thereof.
Background technology
1987, the C.W.Tang of Eastman Kodak company of the U.S. and VanSlyke reported the breakthrough in organic electroluminescent research.Utilize ultrathin film technology to prepare high brightness, high efficiency double-deck organic electroluminescence device (OLED).Under 10V, brightness reaches 1000cd/m 2, its luminous efficiency is 1.51lm/W, the life-span is greater than 100 hours.
The principle of luminosity of OLED is based under the effect of extra electric field, and electronics is injected into organic lowest unocccupied molecular orbital (LUMO) from negative electrode, and hole is injected into organic highest occupied molecular orbital (HOMO) from anode.Electronics and hole meet at luminescent layer, compound, form exciton, exciton moves under electric field action, and energy is passed to luminescent material, and excitation electron is from ground state transition to excitation state, excited energy, by Radiation-induced deactivation, produces photon, discharges luminous energy.
In traditional luminescent device, the light of device inside only has 18% left and right can be transmitted into outside to go, and other part can consume in device outside with other forms, (as the specific refractivity between glass and ITO, glass refraction is that 1.5, ITO is 1.8 between interface, refractive index poor, light arrives glass from ITO, will there is total reflection), caused the loss of total reflection, thereby it is lower to cause entirety to go out optical property.Therefore, be necessary to improve the luminous efficiency of OLED.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of organic electroluminescence device and preparation method thereof, described organic electroluminescence device, comprise the conductive anode substrate of glass, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the composite cathode that stack gradually, described composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer, and the present invention has improved conductive capability and the luminous efficiency of device.
First aspect, the invention provides a kind of organic electroluminescence device, comprise the conductive anode substrate of glass, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the composite cathode that stack gradually, described composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer, and the material of described silicon compound layer is silicon monoxide (SiO), silicon dioxide (SiO 2) and sodium metasilicate (Na 2siO 3) in one, the material of described conductive membrane layer is indium tin oxide (ITO), one in aluminium zinc oxide (AZO) and indium-zinc oxide (IZO), the material of described metal-doped layer is that work function is the composite material that the low work function metal of 2.0eV～3.5eV and high work function metal that work function is 4.0eV～5.5eV are mixed to form with mass ratio 5:1～20:1, described low work function metal is magnesium (Mg), strontium (Sr), one in calcium (Ca) and ytterbium (Yb), described high work function metal is silver (Ag), aluminium (Al), one in platinum (Pt) and gold (Au).
Preferably, the thickness of described silicon compound layer is 10～50nm.
Preferably, the thickness of described conductive membrane layer is 50～150nm.
Preferably, the thickness of described metal-doped layer is 100～400nm.
Preferably, described conductive anode substrate of glass is the one in indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) and indium-zinc oxide glass (IZO), more preferably ITO.
Preferably, the material of described hole injection layer is molybdenum trioxide (MoO 3), tungstic acid (WO 3) and vanadic oxide (V 2o 5) in one, thickness is 20～80nm.More preferably, the material of described hole injection layer is MoO 3, thickness is 30nm.
Preferably, the material of described hole transmission layer is 1,1-, bis-[4-[N, N '-bis-(p-tolyl) amino] phenyl] cyclohexane (TAPC), 4,4', 4''-tri-(carbazole-9-yl) triphenylamine (TCTA) and N, N '-(1-naphthyl)-N, N '-diphenyl-4, one in 4 '-benzidine (NPB), the thickness of described hole transmission layer is 20～60nm, more preferably, the material of described hole transmission layer is TAPC, and thickness is 55nm.
Preferably, the material of described luminescent layer is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis--β-naphthylene anthracene (ADN), 4, two (the 9-ethyl-3-carbazole vinyl)-1 of 4'-, 1'-biphenyl (BCzVBi) and oxine aluminium (Alq 3) in one, thickness is 5～40nm, more preferably, the material of described luminescent layer is Alq 3, thickness is 25nm.
Preferably, the material of described electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen), 3-(biphenyl-4-yl)-5-(4-tert-butyl-phenyl)-4-phenyl-4H-1, the one in 2,4-triazole (TAZ) and N-aryl benzimidazole (TPBI), thickness is 40～300nm, more preferably, the material of described electron transfer layer is TAZ, and thickness is 150nm.
Preferably, the material of described electron injecting layer is cesium carbonate (Cs 2cO 3), cesium fluoride (CsF), nitrine caesium (CsN 3) and lithium fluoride (LiF) in one, thickness is 0.5～10nm, more preferably, the material of described electron injecting layer is LiF, thickness is 1nm.
Described composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer, silicon compound is microgranular, and particle is larger, and preparation forms and arranges orderly micro-sphere structure after getting on, this structure is carried out scattering to light again, improves effective emergent ray; Conductive film material work function is between the HOMO(of organic material HOMO highest occupied molecular orbital) and LUMO(lowest unoccupied molecular orbital) between energy level, can effectively improve the injection efficiency of electronics, simultaneously, mature preparation process, under specific thicknesses, conductive membrane layer light transmission rate in visible-range can reach 85%～90%, and most light can be seen through; Metal-doped layer material is that work function is the high work function metal doping composition that the low work function metal of 2.0eV～3.5eV and work function are 4.0eV～5.5eV, low work function metal is conducive to the injection of electronics, increase conductivity, high work function metal can improve the stability (work function is higher, and metal is more stable) of composite cathode.Meanwhile, metal-doped layer reflects light, makes light reflect back into the bottom of device, and this composite cathode can effectively improve the luminous efficiency of device.
Second aspect, the invention provides a kind of preparation method of organic electroluminescence device, comprises following operating procedure:
(1) provide the conductive anode substrate of glass of required size, dry after cleaning; In conductive anode substrate of glass, adopt the method for thermal resistance evaporation to prepare successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
(2) on electron injecting layer, prepare composite cathode, described composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer;
On electron injecting layer, adopt the method for electron beam evaporation plating to prepare silicon compound layer, the material of described silicon compound layer is SiO, SiO 2and Na 2siO 3in one, the energy density of described electron beam evaporation plating is 10～l00W/cm 2;
On silicon compound layer, adopt the method for magnetron sputtering to prepare conductive membrane layer, the material of described conductive membrane layer is the one in ITO, AZO and IZO, and the accelerating voltage of magnetron sputtering is 300～800V, and magnetic field is 50～200G, and power density is 1～40W/cm 2;
On conductive membrane layer, adopt the method for thermal resistance evaporation to prepare metal-doped layer, the material of described metal-doped layer is that work function is the composite material that the low work function metal of 2.0eV～3.5eV and high work function metal that work function is 4.0～5.5eV are mixed to form with mass ratio 5:1～20:1, described low work function metal is the one in Mg, Sr, Ca and Yb, described high work function metal is the one in Ag, Al, Pt and Au, and evaporation pressure is 5 × 10 -5pa～2 × 10 -3pa, evaporation speed is 1～10nm/s; Obtain described organic electroluminescence device.
Preferably, the thickness of described silicon compound layer is 10～50nm.
Preferably, the thickness of described conductive membrane layer is 50～150nm.
Preferably, the thickness of described metal-doped layer is 100～400nm.
Preferably, the thermal resistance evaporation condition of described hole injection layer and electron injecting layer is: pressure is 5 × 10 -5pa～2 × 10 -3pa, evaporation speed is 1～10nm/s.
Preferably, the thermal resistance evaporation condition of described hole transmission layer, electron transfer layer and luminescent layer is: pressure is 5 × 10 -5pa～2 × 10 -3pa, evaporation speed is 0.1～1nm/s.
Preferably, described in the conductive anode substrate of glass of required size is provided, concrete operations are: conductive anode substrate of glass is carried out to photoetching treatment, be then cut into needed size.
Preferably, conductive anode substrate of glass is used successively liquid detergent by being operating as that described cleaning is dried afterwards, deionized water, and acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, the organic pollution of removal glass surface, cleans up rear air-dry.
Preferably, described conductive anode substrate of glass is the one in indium tin oxide glass (ITO), aluminium zinc oxide glass (AZO) and indium-zinc oxide glass (IZO), more preferably ITO.
Preferably, the material of described hole injection layer is MoO 3, WO 3and V 2o 5in one, thickness is 20～80nm.More preferably, the material of described hole injection layer is MoO 3, thickness is 30nm.
Preferably, the material of described hole transmission layer is the one in TAPC, TCTA and NPB, and described hole transmission layer material thickness is 20～60nm, and more preferably, the material of described hole transmission layer is TAPC, and thickness is 55nm.
Preferably, the material of described luminescent layer is DCJTB, ADN, BCzVBi and Alq 3in one, thickness is 5～40nm, more preferably, the material of described luminescent layer is Alq 3, thickness is preferably 25nm.
Preferably, the material of described electron transfer layer is the one in Bphen, TAZ and TPBI, and thickness is 40～300nm, and more preferably, the material of described electron transfer layer is TAZ, and thickness is 150nm.
Preferably, the material of described electron injecting layer is Cs 2cO 3, CsF, CsN 3with the one in LiF, thickness is 0.5～10nm, and more preferably, the material of described electron injecting layer is LiF, and thickness is 1nm.
Described composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer, silicon compound is microgranular, and particle is larger, and preparation forms and arranges orderly micro-sphere structure after getting on, this structure is carried out scattering to light again, improves effective emergent ray; Conductive film material work function is between the HOMO(of organic material HOMO highest occupied molecular orbital) and LUMO(lowest unoccupied molecular orbital) between energy level, can effectively improve the injection efficiency of electronics, simultaneously, mature preparation process, under specific thicknesses, conductive membrane layer light transmission rate in visible-range can reach 85%～90%, and most light can be seen through; Low work function metal and work function that metal-doped layer is 2.0eV～3.5eV by work function are that the high work function metal of 4.0eV～5.5eV is adulterated, low workfunction metal is conducive to the injection of electronics, increase conductivity, high-work-function metal can improve the stability (work function is higher, and metal is more stable) of composite cathode.Meanwhile, metal-doped layer reflects light, makes light reflect back into the bottom of device, and this composite cathode can effectively improve the luminous efficiency of device.
Implement the embodiment of the present invention, there is following beneficial effect:
(1) composite cathode provided by the invention is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer, has improved electric conductivity and the luminous efficiency of device;
(2) preparation method of composite cathode provided by the invention, technique is simple, and cost is low.
Brief description of the drawings
In order to be illustrated more clearly in technical scheme of the present invention, to the accompanying drawing of required use in execution mode be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of the organic electroluminescence device that provides of the embodiment of the present invention 1;
Fig. 2 is brightness and the luminous efficiency graph of a relation of the embodiment of the present invention 1 and comparative example's organic electroluminescence device.
Embodiment
Below in conjunction with the accompanying drawing in embodiment of the present invention, the technical scheme in embodiment of the present invention is clearly and completely described.
Embodiment 1
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) first ito glass substrate is carried out to photoetching treatment, be then cut into 2 × 2cm 2square dimensions, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry; Then on anode, adopt the condition of thermal resistance evaporation to prepare successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Wherein,
The material of hole injection layer is MoO 3, the pressure 8 × 10 adopting when evaporation -5pa, evaporation speed is 3nm/s, evaporation thickness is 30nm;
The material of hole transmission layer is TAPC, and the pressure adopting when evaporation is 8 × 10 -5pa, evaporation speed is 0.2nm/s, evaporation thickness is 55nm;
The material of luminescent layer is Alq 3, the pressure adopting when evaporation is 8 × 10 -5pa, evaporation speed is 0.2nm/s, evaporation thickness is 25nm;
The material of electron transfer layer is TAZ, and the pressure adopting when evaporation is 8 × 10 -5pa, evaporation speed is 0.2nm/s, evaporation thickness is 150nm;
The material of electron injecting layer is LiF, and the pressure adopting when evaporation is 8 × 10 -5pa, evaporation speed is 3nm/s, evaporation thickness is 1nm;
(2) prepare composite cathode;
On electron injecting layer, electron beam evaporation plating is prepared SiO 2, obtaining the silicon compound layer that thickness is 25nm, the energy density of electron beam evaporation plating is 25W/cm 2;
On silicon compound layer, adopt the method for magnetron sputtering to prepare ITO, obtain the conductive membrane layer that thickness is 80nm, the accelerating voltage of magnetron sputtering is 500V, and magnetic field is 150G, and power density is 20W/cm 2;
Thermal resistance evaporation Mg and the Ag composite material that 10:1 is mixed to form in mass ratio on conductive membrane layer, obtaining thickness is the metal-doped layer of 200nm, the pressure adopting when evaporation is 8 × 10 -5pa, evaporation speed is 3nm/s, obtains organic electroluminescence device.
Fig. 1 is the structural representation of the organic electroluminescence device prepared of the present embodiment, as shown in Figure 1, organic electroluminescence device prepared by the present embodiment, comprise the conductive anode substrate of glass 1, hole injection layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5, electron injecting layer 6 and the composite cathode 7 that stack gradually, composite cathode 7 is made up of the silicon compound layer 71 stacking gradually, conductive membrane layer 72 and metal-doped layer 73.Concrete structure is expressed as:
Ito glass/MoO 3/ TAPC/Alq 3/ TAZ/LiF/SiO 2/ ITO/Mg:Ag(10:1), wherein, slash "/" represents to stack gradually, colon ": " in Mg:Ag represents to mix, 10:1 represents the former and the latter's mass ratio, after each symbol represents in embodiment meaning identical.
Embodiment 2
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) first AZO substrate of glass is carried out to photoetching treatment, be then cut into 2 × 2cm 2square dimensions, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry; Then on anode, adopt the method for thermal resistance evaporation to prepare successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Wherein,
The material of hole injection layer is WO 3, the pressure adopting when evaporation is 2 × 10 -3pa, evaporation speed is 10nm/s, evaporation thickness is 80nm;
The material of hole transmission layer is NPB, and the pressure adopting when evaporation is 2 × 10 -3pa, evaporation speed is 0.1nm/s, evaporation thickness is 60nm;
The material of luminescent layer is ADN, and the pressure adopting when evaporation is 2 × 10 -3pa, evaporation speed is 0.1nm/s, evaporation thickness is 5nm;
The material of electron transfer layer is Bphen, and the pressure adopting when evaporation is 2 × 10 -3pa, evaporation speed is 10nm/s, evaporation thickness is 300nm;
The material of electron injecting layer is CsF, and the pressure adopting when evaporation is 2 × 10 -3pa, evaporation speed is 0.1nm/s, evaporation thickness is 10nm;
(2) prepare composite cathode;
On electron injecting layer, electron beam evaporation plating is prepared SiO, obtains the silicon compound layer that thickness is 10nm, and the energy density of electron beam evaporation plating is 10W/cm 2;
On silicon compound layer, adopt the method for magnetron sputtering to prepare AZO, obtain the conductive membrane layer that thickness is 150nm, the accelerating voltage of magnetron sputtering is 300V, and magnetic field is 200G, and power density is 1W/cm 2;
Thermal resistance evaporation Sr and the Al composite material that 20:1 is mixed to form in mass ratio on conductive membrane layer, obtaining thickness is the metal-doped layer of 400nm, the pressure adopting when evaporation is 2 × 10 -3pa, evaporation speed is 10nm/s, obtains organic electroluminescence device.
Organic electroluminescence device prepared by the present embodiment, comprise the conductive anode substrate of glass, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the composite cathode that stack gradually, composite cathode is made up of stacked silicon compound layer, conductive membrane layer and metal-doped layer.Concrete structure is expressed as:
AZO glass/WO 3/ NPB/ADN/Bphen/CsF/SiO/AZO/Sr:Al(20:1).
Embodiment 3
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) first IZO substrate of glass is carried out to photoetching treatment, be then cut into 2 × 2cm 2square dimensions, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry; Then on anode, adopt the method for thermal resistance evaporation to prepare successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Wherein,
The material of hole injection layer is V 2o 5, the pressure adopting when evaporation is 5 × 10 -5pa, evaporation speed is 1nm/s, evaporation thickness is 20nm;
The material of hole transmission layer is NPB, and the pressure adopting when evaporation is 5 × 10 -5pa, evaporation speed is 1nm/s, evaporation thickness is 20nm;
The material of luminescent layer is BCzVBi, and the pressure adopting when evaporation is 5 × 10 -5pa, evaporation speed is 1nm/s, evaporation thickness is 40nm;
The material of electron transfer layer is TAZ, and the pressure adopting when evaporation is 5 × 10 -5pa, evaporation speed is that 1nm/s evaporation thickness is 60nm;
The material of electron injecting layer is Cs 2cO 3, the pressure adopting when evaporation is 5 × 10 -5pa, evaporation speed is 1nm/s, evaporation thickness is 0.5nm;
(2) prepare composite cathode;
On electron injecting layer, electron beam evaporation plating is prepared Na 2siO 3, obtaining the silicon compound layer that thickness is 50nm, the energy density of electron beam evaporation plating is 100W/cm 2;
On silicon compound layer, adopt the method for magnetron sputtering to prepare IZO, obtain the conductive membrane layer that thickness is 50nm, the accelerating voltage of magnetron sputtering is 800V, and magnetic field is 50G, and power density is 40W/cm 2;
Thermal resistance evaporation Ca and the Pt composite material that 5:1 is mixed to form in mass ratio on conductive membrane layer, obtaining thickness is the metal-doped layer of 100nm, the pressure adopting when evaporation is 5 × 10 -5pa, evaporation speed is 1nm/s, obtains organic electroluminescence device.
Organic electroluminescence device prepared by the present embodiment, comprise the conductive anode substrate of glass, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the composite cathode that stack gradually, composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer.Concrete structure is expressed as:
IZO glass/V 2o 5/ NPB/BCzVBi/TAZ/Cs 2cO 3/ Na 2siO 3/ IZO/Ca:Pt(5:1).
Embodiment 4
A preparation method for organic electroluminescence device, comprises following operating procedure:
(1) first IZO substrate of glass is carried out to photoetching treatment, be then cut into 2 × 2cm 2square dimensions, then use successively liquid detergent, deionized water, acetone, ethanol, the each ultrasonic 15min of isopropyl alcohol, removes the organic pollution of glass surface, cleans up rear air-dry; Then on anode, adopt the method for thermal resistance evaporation to prepare successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer; Wherein,
The material of hole injection layer is WO 3, the pressure adopting when evaporation is 5 × 10 -4pa, evaporation speed is 5nm/s, evaporation thickness is 30nm;
The material of hole transmission layer is TCTA, and the pressure adopting when evaporation is 5 × 10 -4pa, evaporation speed is 0.2nm/s, evaporation thickness is 50nm;
The material of luminescent layer is DCJTB, and the pressure adopting when evaporation is 5 × 10 -4pa, evaporation speed is 0.2nm/s, evaporation thickness is 5nm;
The material of electron transfer layer is TPBi, and the pressure adopting when evaporation is 5 × 10 -4pa, evaporation speed is 0.2nm/s, evaporation thickness is 40nm;
The material of electron injecting layer is CsN 3, the pressure adopting when evaporation is 5 × 10 -4pa, evaporation speed is 5nm/s, evaporation thickness is 1nm;
(2) prepare composite cathode;
On electron injecting layer, electron beam evaporation plating is prepared SiO 2, obtaining the silicon compound layer that thickness is 35nm, the energy density of electron beam evaporation plating is 50W/cm 2;
On silicon compound layer, adopt the method for magnetron sputtering to prepare IZO, obtain the conductive membrane layer that thickness is 100nm, the accelerating voltage of magnetron sputtering is 350V, and magnetic field is 100G, and power density is 25W/cm 2;
Thermal resistance evaporation Yb and the Au composite material that 7:1 is mixed to form in mass ratio on conductive membrane layer, obtaining thickness is the metal-doped layer of 180nm, the pressure adopting when evaporation is 5 × 10 -4pa, evaporation speed is 5nm/s, obtains organic electroluminescence device.
Organic electroluminescence device prepared by the present embodiment, comprise the conductive anode substrate of glass, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and the composite cathode that stack gradually, composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer.Concrete structure is expressed as:
IZO glass/WO 3/ TCTA/DCJTB/TPBi/CsN 3/ SiO 2/ IZO/Yb:Au(7:1).
Comparative example
For being presented as creativeness of the present invention, the present invention is also provided with comparative example, the difference of comparative example and embodiment 1 is that the negative electrode in comparative example is metal simple-substance silver (Ag), and thickness is 120nm, and the concrete structure of comparative example's organic electroluminescence device is ito glass/MoO 3/ TAPC/Alq 3/ TAZ/LiF/Ag, respectively corresponding conductive anode substrate of glass, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and negative electrode.
Effect embodiment
Adopt the USB4000 fiber spectrometer testing electroluminescent spectrum of U.S. marine optics Ocean Optics, the current-voltage tester Keithley2400 test electric property of Keithley company of the U.S., CS-100A colorimeter test brightness and the colourity of Konica Minolta company of Japan, obtain the luminous efficiency of organic electroluminescence device with brightness change curve, to investigate the luminous efficiency of device, tested object is organic electroluminescence device prepared by embodiment 1 and comparative example.Test result as shown in Figure 2.
Fig. 2 is the embodiment of the present invention 1 and the luminous efficiency of comparative example's organic electroluminescence device and the graph of a relation of brightness.From Fig. 2, can find out, under different brightness, all large than comparative example of the luminous efficiency of embodiment 1, the maximum luminous efficiency of embodiment 1 is 9.65lm/W, and that comparative example is only 5.96lm/W, this explanation, silicon compound in composite cathode in embodiment 1 carries out scattering to light, improve effective emergent ray, conductive membrane layer can effectively improve the injection efficiency of electronics, most light can be seen through, metal-doped layer is conducive to the injection of electronics, increase conductivity, the stability that improves composite cathode makes light reflect back into the bottom of device, this composite cathode can effectively improve the luminous efficiency of device.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.

Claims (10)

1. an organic electroluminescence device, comprise the conductive anode substrate of glass stacking gradually, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer and composite cathode, it is characterized in that, described composite cathode is by the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer composition, the material of described silicon compound layer is silicon monoxide, one in silicon dioxide and sodium metasilicate, the material of described conductive membrane layer is indium tin oxide, one in aluminium zinc oxide and indium-zinc oxide, the material of described metal-doped layer is that work function is the composite material that the low work function metal of 2.0eV～3.5eV and high work function metal that work function is 4.0eV～5.5eV are mixed to form with mass ratio 5:1～20:1, described low work function metal is magnesium, strontium, one in calcium and ytterbium, described high work function metal is silver, aluminium, one in platinum and gold.
2. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of described silicon compound layer is 10～50nm.
3. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of described conductive membrane layer is 50～150nm.
4. organic electroluminescence device as claimed in claim 1, is characterized in that, the thickness of described metal-doped layer is 100～400nm.
5. a preparation method for organic electroluminescence device, is characterized in that, comprises following operating procedure:
(1) provide the conductive anode substrate of glass of required size, dry after cleaning; In conductive anode substrate of glass, adopt the method for thermal resistance evaporation to prepare successively hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and electron injecting layer;
(2) on electron injecting layer, prepare composite cathode, described composite cathode is made up of the silicon compound layer stacking gradually, conductive membrane layer and metal-doped layer;
On electron injecting layer, adopt the method for electron beam evaporation plating to prepare silicon compound layer, the material of described silicon compound layer is the one in silicon monoxide, silicon dioxide and sodium metasilicate, and the energy density of described electron beam evaporation plating is 10～l00W/cm 2;
On silicon compound layer, adopt the method for magnetron sputtering to prepare conductive membrane layer, the material of described conductive membrane layer is the one in indium tin oxide, aluminium zinc oxide and indium-zinc oxide, the accelerating voltage of described magnetron sputtering is 300～800V, magnetic field is 50～200G, and power density is 1～40W/cm 2;
On conductive membrane layer, adopt the method for thermal resistance evaporation to prepare metal-doped layer, the material of described metal-doped layer is that work function is the composite material that the low work function metal of 2.0eV～3.5eV and high work function metal that work function is 4.0eV～5.5eV are mixed to form with mass ratio 5:1～20:1, described low work function metal is the one in magnesium, strontium, calcium and ytterbium, described high work function metal is the one in silver, aluminium, platinum and gold, and evaporation pressure is 5 × 10 -5pa～2 × 10 -3pa, evaporation speed is 1～10nm/s; Obtain described organic electroluminescence device.
6. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the thickness of described silicon compound layer is 10～50nm.
7. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the thickness of described conductive membrane layer is 50～150nm.
8. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the thickness of described metal-doped layer is 100～400nm.
9. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the thermal resistance evaporation condition of described hole injection layer and electron injecting layer is: pressure is 5 × 10 -5pa～2 × 10 -3pa, evaporation speed is 1～10nm/s.
10. the preparation method of organic electroluminescence device as claimed in claim 5, is characterized in that, the thermal resistance evaporation condition of described hole transmission layer, electron transfer layer and luminescent layer is: pressure is 5 × 10 -5pa～2 × 10 -3pa, evaporation speed is 0.1～1nm/s.
CN201310143977.4A 2013-04-24 2013-04-24 Organic light-emitting device and preparation method thereof Pending CN104124372A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4720432A (en) * 1987-02-11 1988-01-19 Eastman Kodak Company Electroluminescent device with organic luminescent medium
US20030151356A1 (en) * 1996-05-03 2003-08-14 Karl Pichler Organic light-emitting device and method of fabricating the same
CN1792120A (en) * 2003-05-20 2006-06-21 出光兴产株式会社 Organic electroluminescent element and display device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4720432A (en) * 1987-02-11 1988-01-19 Eastman Kodak Company Electroluminescent device with organic luminescent medium
US20030151356A1 (en) * 1996-05-03 2003-08-14 Karl Pichler Organic light-emitting device and method of fabricating the same
CN1792120A (en) * 2003-05-20 2006-06-21 出光兴产株式会社 Organic electroluminescent element and display device

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Application publication date: 20141029