CN109473565A - A kind of high grade of transparency based on ultra-thin low workfunction metal is from encapsulation top emitting electrode and preparation method thereof - Google Patents
A kind of high grade of transparency based on ultra-thin low workfunction metal is from encapsulation top emitting electrode and preparation method thereof Download PDFInfo
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Abstract
A kind of high grade of transparency based on ultra-thin low workfunction metal belongs to field of display technology from encapsulation top emitting electrode and preparation method thereof.For three layer stacked structures: in transparent substrate, first layer is fine and close transport layer, and the second layer is the more smooth ultra-thin low work function metal grown by evaporation coating technique, and third layer is then one layer fine and close from encapsulated layer.It is still no using precedent as the transparent electrode of super thin metal main body due to the chemical characteristic of the low workfunction metals such as calcium, caesium.This patent uses laminated construction, by the way that in the transparent conductive film of ultra-thin low workfunction metal two sides deposition compact, (side is transport layer, one layer is from encapsulated layer), successfully prepared it is based on low workfunction metal, with the highly transparent top emitting electrode from encapsulation performance.The present invention greatly improves the transmitance of low workfunction metal electrode using almost undamaged technology of preparing prepares top emitting electrode to luminescent device surface.
Description
Technical field
The invention belongs to field of display technology, from encapsulation conductive electrode and its do not destroy more particularly to a kind of high grade of transparency
The preparation method of substrate grown semi-finished product device uses atom layer deposition process, or chemistry more particularly to a kind of
The height based on ultra-thin low workfunction metal of vapor deposition method, sputtering technology etc. and the laminated construction of hot evaporation process preparation
Transparency encapsulation top emitting electrode (i.e. transparent conductive cathode) and preparation method thereof certainly.
Background technique
Transparent conductive electrode (Transparent Conductive Electrode, TCE), i.e., have in visible-range
Good through performance, and the thin-film material with satisfactory electrical conductivity.It is produced in FPD, illumination, photovoltaic industry and intelligence
It is widely used in product.Wherein, Organic Light Emitting Diode (Organic Light-Emitting Diode, OLED) is used as one
The display illuminating device of kind rising in recent years is answered extensively due to the characteristics of its deflection, self-luminous, face shine, fast response time
With in FPD especially mobile phone screen.Meanwhile the above feature more for OLED to be prepared into and has multi-functional special type
Display device becomes possibility.Wherein, it due to the spontaneous light characteristic of OLED, does not need back lighting and it uses organic material
The transparent nature of material, therefore transparence display device can be prepared to.Transparence display is just to be known in recent years
A kind of display product.Compared with traditional display, transparence display device breaks through routine, more adds the interest of product,
Bring the unprecedented visual impact of user and completely new experience.Make it in retail advertising, company's displaying, Museum Exhibit, religion
Educate or the application scenarios such as the displaying of the prize in enterprise field, display and demonstration and the key areas such as military, medical on augmented reality
Functionally there is irreplaceable application value.
In order to realize the export of light, the electrode of OLED light emission side must be transparent.Traditional OLED is generally bottom
Emit OLED, TCE generally uses indium tin oxide (Indium Tin Oxide, ITO) to prepare.ITO is that one kind has both well
The transparent conductive material of translucency and electric conductivity has both good translucency and electric conductivity, therefore is widely used in all kinds of
It shows in illuminating product.However, traditional ITO can not meet its need as the cathode of device in preparing transparent OLED
Ask: ITO material during the preparation process, generally requires the preparation work for taking magnetron sputtering etc. to need high-energy bombardment substrate surface
Skill, and OLED organic material non-refractory, labile feature, therefore few selection ITO is as top emitting electrode material.
In addition to conventional bottom emitting OLED, top emitting OLED product then generally uses super thin metal and metal composite electrode system
The translucent conductive electrode at standby top.The metals such as calcium, caesium have lower work function, with the electron-transport material at the top of OLED device
Material has good level-density parameter.Therefore, the materials such as calcium, caesium are widely used as the preparation of electron injecting layer or cathode layer, and
The metallic film transmitance of its good film-forming property, preparation is high.But unlike that the inert metals such as gold, silver, low workfunction metal
Matter is very active, easily reacts with water oxygen in air, and especially when thickness is less than or equal to 20 nanometers, oxidation deactivation is anti-
Answer more obvious, in order to overcome low workfunction metal, such as calcium, caesium have the problem of elevated chemical activity, usually utilize various
For the alloy of low workfunction metal and noncorroding metal as cathode material, common alloy electrode has magnesium silver alloy (volume ratio
For 10:1), lithium-aluminium alloy (lithium accounting about 1%) etc., the part of inert metal makes it have certain anti-corruption in alloy electrode
Corrosion, low workfunction metal part also effectively increases the efficiency of device, however there is also some problems for this alloy electrode.
The photopermeability of the alloy electrodes such as Mg-Ag (magnesium silver alloy) is very poor, only just has under the thickness of very thin (nanometer scale)
Certain light transmission properties, but when cathode layer is very thin, breaking or easy to oxidize metal problem is usually had, it cannot
Effective Ohmic contact is formed, defect is easily formed on interface causes the loss of charge injection process to increase；In preparation process, essence
Really by best proportion doped growing alloy electrode, there is also certain technical problems；Most importantly, alloy electrode penetrates
Rate is very low, can only be reluctantly as the semitransparent electrode of OLED device.
Summary of the invention
That present invention aim to address the low workfunction metal alloy cathode transmitances for being currently used in transparent OLED is low, goes out light
Performance is poor, stability difference problem, thus prepare the high grade of transparency, from encapsulation, high light-emitting efficiency and friendly transparent of substrate leading
Electric cathode, and further widen its application in all-transparent LED, solar-energy photo-voltaic cell.
To achieve the goals above, the present invention provides a kind of high grades of transparency based on ultra-thin low workfunction metal to encapsulate certainly
Top emitting electrode and preparation method thereof.The transparent top emitting electrode uses three layer stacked structures: in transparent substrate, first layer
For fine and close transport layer, the second layer is the more smooth ultra-thin low work function metal grown by evaporation coating technique, third layer
It is then one layer fine and close from encapsulated layer.Due to the chemical characteristic of the low workfunction metals such as calcium, caesium, as super thin metal main body
Transparent electrode still without apply precedent.This patent uses laminated construction, by ultra-thin low workfunction metal two sides deposition
Fine and close transparent conductive film (side is transport layer, and one layer is from encapsulated layer), has successfully prepared and is with low workfunction metal
Main body, with the highly transparent top emitting electrode from encapsulation performance.
Currently, the technique of deposited metal film is relatively simple, easy to implement, depositional mode of the present invention is vapor deposition
Technology, the ultra-thin low workfunction metal deposited are calcium.The film of the present invention for being deposited on metal two sides, should have
Bright, the conductive, characteristics such as stability is good, it is preferable that the protective layer using metal oxide as electrode two sides, depositional mode can
To be in a manner of sputtering, chemical vapor deposition, atomic layer deposition etc., since protective layer should have super thin and dense characteristic, so
It is also required to carry out special processing during the deposition process；In the case where using magnetron sputtering technique, need to control deposition velocity and
The size of deposited particles improves the temperature of sputtering zone and substrate deposition area under the growth conditions for keeping low power low temperature as far as possible
Difference, furthermore, it is necessary to which additional deposition CuPc is to protect the organic material in device；For another example apply inductively coupled plasma body enhancingization
It learns gas phase deposition technology (Inductively Coupled Plasma Chemical Vapor Deposition, ICP-CVD)
In the case where, need plasma module to carry out special designing, while needing to adjust plated film predecessor and technique；Atomic layer deposition
Product technology (Atomic Layer Deposition, ALD) is as a kind of reaction of monoatomic layer, the film preparation work of high shape-retaining ability
Skill has advantage in the thin-film material of deposition compact, however, wide using metal oxide band gap prepared by ALD, energy level is deep,
It is unfavorable for the cathode material as OLED.Therefore, it is necessary to by conjunction with its metal phase with low work function to obtain the saturating of practicability
Bright cathode.The mode of used depositing metal oxide is technique for atomic layer deposition in the present invention.
For more intuitive displaying, the top emitting electrode of now description preparation on a transparent substrate, the transparent top emitting electricity
Extremely three-decker is followed successively by transport layer, the ultra-thin low work content in the transport layer in transparent substrate from bottom to top
Number metal layers and above the ultra-thin low work function metal from encapsulated layer；Wherein transport layer is thin using high-compactness
Film both can be used as the electron transfer layer of electrode surface, can also be used as the buffering package layer of electrode Yu organic material interlayer；Thoroughly
Bright ultra-thin low work function metal provides a large amount of carrier, and with organic layer level-density parameter, ensure that carrier
Injection efficiency；Light extraction efficiency is improved from encapsulated layer, both can be used as electrode improves electrode isolation water oxygen energy from encapsulated layer
Power, and the antireflection layer for improving transparent electrode transmitance can be formed.
Further, the transparent substrates are glass, quartz, sapphire, polyethylene terephthalate (PET), polyamides
Any one of imines (PD), polyethylene naphthalate (PEN), surface undulation is preferably shorter than the thickness of ultra-thin metal layer
Then degree successively cleans the modes such as substrate surface and ultrasonic cleaning with acetone, alcohol and removes surface irregularities.
Further, the material of the transport layer is metal oxide, can be Zn0, Ti02、W03、AL2O3One of,
Its thickness is within the scope of 0.5-10nm, transport layer smooth surface.Deposition method selects technique for atomic layer deposition deposition.
Further, the material of the ultra-thin low work function metal is that lithium, calcium, potassium, rubidium, caesium etc. have compared with low work function
Alkaline-earth metal, or the alloy that wherein several alkaline-earth metal are mixed to form.The thickness of metal layer is within the scope of 5-40nm, deposition
Mode selects vacuum evaporation technology.
Further, the material from encapsulated layer is metal oxide, can be Zn0, Ti02、W03、AL2O3In one
Kind, it can be identical with the material that transport layer uses, thickness continuously fine and close can form a film in 0.5-30nm range from encapsulated layer,
And there is certain mechanical strength.Deposition method selects technique for atomic layer deposition.
A kind of preparation of the high grade of transparency based on ultra-thin low workfunction metal of the present invention from encapsulation top emitting electrode
Method, its step are as follows:
A. clean transparent substrate, drying；
B. transport layer is prepared on the organic function layer of the obtained substrate of step A or OLED device, transmission layer material is gold
Belong to oxide, can be Zn0, Ti02、W03、AL2O3One of, thickness is within the scope of 0.5-10nm；
C. prepare ultra-thin low work function metal in the transport layer that step B is obtained, metal layer material be lithium, calcium, potassium,
Rubidium, caesium etc. have the alkaline-earth metal compared with low work function, or the alloy that wherein several alkaline-earth metal are mixed to form, metal layer
Thickness is within the scope of 5-40nm；
D. preparation is metal oxygen from layer material is encapsulated from encapsulated layer on the ultra-thin low work function metal that step C is obtained
Compound can be Zn0, Ti02、W03、AL2O3One of, it can be identical with the material that transport layer uses, thickness is in 0.5-
30nm range；To obtain the high grade of transparency based on ultra-thin low workfunction metal from encapsulation top emitting electrode.
The present invention compared with prior art, has the characteristics that prominent and remarkable advantage as follows:
1) low workfunction metals such as calcium, caesium are utilized, improve the efficiency of transmission of carrier.
2) be prepared in low workfunction metal it is fine and close from encapsulated layer, so that packaging protection ultra-thin metal layer, ensure that
The service life of electrode.
3) using to luminescent device surface, almost undamaged technology of preparing prepares top emitting electrode.
4) transmitance of low workfunction metal electrode is greatly improved.
Detailed description of the invention
Fig. 1 is the top emitting electrode structure schematic diagram of laminated construction described in the embodiment of the present invention 1, wherein 11 be substrate,
12 is from encapsulated layer, 13 are ultra-thin calcium metal layer, be deposited growth ultra-thin calcium metal layer can according to demand with mask plate patterns,
14 be transport layer.
Fig. 2 is the top emitting electrode transmittance curve of laminated construction described in the embodiment of the present invention 1, and wherein abscissa is wave
Long, ordinate is transmitance；As shown, mean transmissivity has reached 80% or more.
Fig. 3 is the structural schematic diagram of electroluminescent device described in the embodiment of the present invention 2.In figure, 31 be transparent substrates,
32 be the laminated construction top emitting electrode layer, 33 be electrically conducting transparent ito anode, 34 be organic function layer, from bottom to up according to
Secondary is HAT-CN (hole injection layer, 10nm)/TAPC (hole transmission layer, 50nm)/Alq3: C545T (luminescent layer, 20nm,
Alq3The quality doping concentration of middle C545T is 1%)/Alq3(electron transfer layer, 30nm)/Liq (electron injecting layer, 0.5nm).
Fig. 4 is double for the electroluminescent device of cathode by anode, laminate electrode of ITO described in the embodiment of the present invention 2
Side goes out the brightness-voltage curve of light, and abscissa is voltage, and ordinate is that brightness, wherein ITOside and ACAside respectively indicate
The side ITO and ACA electrode side；As shown, the laminate electrode of design and the two sides ITO have reached photo-equilibrium out.
Specific embodiment
In order to make the features of the present invention it is more obvious, it can be readily appreciated that below with reference to the specific embodiment of the invention, to the present invention
It is further described.
A kind of high emission structure at top laminate electrode of transparency of the invention, structure are ultra-thin transport layer, heat steaming
Plate the ultra-thin calcium metal layer of growth, and fine and close from encapsulated layer.Apply it to the cathode of organic electroluminescence device, device
Concrete composition be: transparent substrates, conductive anode ITO, hot evaporation growth hole injection layer, hole transmission layer, doping shine
Layer, electron transfer layer, electronic barrier layer and laminated construction top emitting electrode layer.
Embodiment 1: in the present embodiment, a kind of Al2O3/Ca/Al2O3 top emitting electrode layer of laminated construction is prepared
1. being gone forward side by side with the burnishing surface that ethanol solution, acetone soln and deionized water successively clean the substrate of glass of single-sided polishing
Row ultrasonic cleaning, is dried up after cleaning with drying nitrogen.
2. substrate of glass is transferred in atomic layer deposition apparatus, it is former by Ying Zuo nanosecond science and technology company ALD-200 heat type
Sublayer depositing device grows aluminium oxide (Al on the glass substrate2O3), chamber pressure, that is, vacuum degree is evacuated to 1.6 × 10-3Torr,
Adjusting growth temperature is 60 DEG C, and adjustings carrier gas nitrogen flow is 25sccm, and by following instruction input machine: (1) the three of 0.02s
Aluminium methyl pulse (2) waits the aquapulse (4) of 35s emptying time (3) 0.02s to wait the above step of 120s emptying time (5) circulation
Rapid 50 times.Wherein pulse is passed through reaction chamber with carrier gas nitrogen, and only carrier gas nitrogen circulates reaction chamber when emptying time.Obtained biography
Defeated layer with a thickness of 5nm.
3. being packed into calcium metal simple-substance in Shenyang Li Ning Co., Ltd hot evaporation equipment, 2. substrate that step obtains is taken out,
It is transferred into the hot evaporation equipment in glove box, then successively uses mechanical pump and molecular pump by the vacuum of evaporated device vacuum chamber
Degree is evacuated to 9 × 10-4Pa, heats calcium metal later, and heated current exists in 70A or so, rate stabilization to be grownWhen start to give birth to
Long, growth rate obtains calcium metal layer (13) by film thickness gauge real-time monitoring, by controlling mask plate in substrate, with a thickness of
16nm。
4. substrate is transferred in atomic layer deposition apparatus in glove box, 2. with step, obtain from encapsulated layer (12),
Its thickness is 5nm.
5. using the transmitance of Shimadzu Co., Ltd UV3600 test electrode, electrode transmittance curve is as shown in Figure 2.
Embodiment 2
Prepare complete electroluminescent device, the structure of device are as follows: substrate of glass/ITO/HAT-CN (10nm)/TAPC
(50nm)/Alq3: C545T (20nm, 1%)/Alq3(30nm)/Liq(0.5nm)/Al2O3(5nm)/Ca(20nm)/Al2O3
(5nm), the device are the organic electroluminescent green devices that two sides goes out light.The preparation method is as follows:
1. cleaning electrically conducting transparent substrate I TO glass using ethanol solution, acetone soln and deionized water and carrying out ultrasonic clear
It washes, is dried up after cleaning with drying nitrogen.Wherein anode layer of the ITO above substrate of glass as device, square resistance are about
30 Ω/mouth.
2. successively using mechanical pump and molecular pump by vacuum degree in vacuum chamber in Shenyang Li Ning Co., Ltd hot evaporation equipment
It is evacuated to 5 × 10-4Pa, then in ito glass substrate after the drying with being sequentially depositing hole injection layer, hole transmission layer, doping
Luminescent layer, electron transfer layer, electronic barrier layer, i.e. HAT-CN (10nm)/TAPC (50nm)/Alq3: C545T (20nm, 1%)/
Alq3(30nm)/Liq (0.5nm), growth rate is by film thickness gauge real-time monitoring, not more than
3. the substrate for obtaining above-mentioned steps is transferred in atomic layer deposition apparatus in glove box, in embodiment 1
2., 3., 4. step, obtains Al2O3/Ca/Al2O3Top emitting electrode layer.
4. providing voltage with the KEYSIGHT digital sourcemeter B2902A of U.S.'s Agilent Agilent, photoresearch is used
PR680 test brightness, obtain the voltage-luminance characteristics of device, as shown in Figure 4.
Claims (9)
1. a kind of high grade of transparency based on ultra-thin low workfunction metal is from the preparation method for encapsulating top emitting electrode, step is such as
Under:
A. clean transparent substrate, drying；
B. transport layer is prepared on the organic function layer of the obtained substrate of step A or OLED device, transmission layer material is metal oxygen
Compound, thickness is within the scope of 0.5-10nm；
C. ultra-thin low work function metal is prepared in the transport layer that step B is obtained, metal layer material is with compared with low work function
Alkaline-earth metal, or the alloy that wherein several alkaline-earth metal are mixed to form, the thickness of metal layer is within the scope of 5-40nm；
D. preparation is metal oxide from layer material is encapsulated from encapsulated layer on the ultra-thin low work function metal that step C is obtained,
Its thickness is within the scope of 0.5-30nm；To obtain the high grade of transparency based on ultra-thin low workfunction metal from encapsulation top emitting electricity
Pole.
2. the system that a kind of high grade of transparency based on ultra-thin low workfunction metal as described in claim 1 encapsulates top emitting electrode certainly
Preparation Method, it is characterised in that: transmission layer material is Zn0, Ti02、W03、AL2O3One of.
3. the system that a kind of high grade of transparency based on ultra-thin low workfunction metal as described in claim 1 encapsulates top emitting electrode certainly
Preparation Method, it is characterised in that: technique for atomic layer deposition is selected to deposit transport layer.
4. the system that a kind of high grade of transparency based on ultra-thin low workfunction metal as described in claim 1 encapsulates top emitting electrode certainly
Preparation Method, it is characterised in that: alkaline-earth metal is lithium, calcium, potassium, rubidium or caesium.
5. the system that a kind of high grade of transparency based on ultra-thin low workfunction metal as described in claim 1 encapsulates top emitting electrode certainly
Preparation Method, it is characterised in that: select vacuum evaporation technology depositing ultrathin low work function metal.
6. the system that a kind of high grade of transparency based on ultra-thin low workfunction metal as described in claim 1 encapsulates top emitting electrode certainly
Preparation Method, it is characterised in that: from layer material is encapsulated for Zn0, Ti02、W03、AL2O3One of.
7. the system that a kind of high grade of transparency based on ultra-thin low workfunction metal as described in claim 1 encapsulates top emitting electrode certainly
Preparation Method, it is characterised in that: select technique for atomic layer deposition deposition from encapsulated layer.
8. the system that a kind of high grade of transparency based on ultra-thin low workfunction metal as described in claim 1 encapsulates top emitting electrode certainly
Preparation Method, it is characterised in that: transparent substrates be glass, quartz, sapphire, polyethylene terephthalate, polyimides or
One of polyethylene naphthalate, surface undulation are lower than the thickness of ultra-thin low work function metal.
9. a kind of high grade of transparency based on ultra-thin low workfunction metal encapsulates top emitting electrode certainly, it is characterised in that: be by right
It is required that 1~8 any one the method is prepared.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113161503A (en) * | 2020-12-30 | 2021-07-23 | 吉林大学 | Transparent electrode |
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Application publication date: 20190315 |