CN107689428A - A kind of preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED - Google Patents
A kind of preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED Download PDFInfo
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- CN107689428A CN107689428A CN201710615393.0A CN201710615393A CN107689428A CN 107689428 A CN107689428 A CN 107689428A CN 201710615393 A CN201710615393 A CN 201710615393A CN 107689428 A CN107689428 A CN 107689428A
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- oled
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
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- H10K50/85—Arrangements for extracting light from the devices
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Abstract
The invention discloses a kind of preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, ito substrate is used into finite concentration laboratory ITO electro-conductive glass cleaning agent and ultraviolet rays cleaning machine cleaning treatment successively first;Reuse common process and prepare uniform PMMA/PS films, the ito substrate with PMMA/PS films is annealed to obtain free nanometer columnar arrays;The organic layer and electrode layer of OLED are finally deposited successively, encapsulation obtains OLED.Phase separation of the invention by regulating and controlling PMMA/PS films, free nanometer column array structure is prepared on an ito substrate, and be applied in OLED, manufacture craft is simple, and cost is low, membrane surface area is effectively lifted simultaneously, device efficient lighting area is increased, while changes the light angle of emergence, weakens loss at total reflection, light emission rate is improved, enhances the luminous of OLED.
Description
Technical field
Lighted the invention mainly relates to OLED and micro-nano structure production field, specifically one kind are used to strengthen OLED devices
The preparation method of the luminous free nanometer columnar arrays of part.
Background technology
The light extraction efficiency of OLED only has 30% or so at present, and people's generally use micro-nano structure goes out light efficiency to improve it
Rate.But present other kinds micro-nano structure, such as lenticule, preparation technology is complicated, it is necessary to strict contraposition, etching process, pair set
The requirement of standby condition and preparation technology is very high, costly.Therefore need to develop simple and quick inexpensive micro-nano structure preparation
Technique, it is luminous so as to strengthen it to improve the light extraction efficiency of OLED and efficient lighting area.
The content of the invention
For problem present in above-mentioned background technology, prepared the invention provides one kind based on PMMA and PS mixed solutions
Free nanometer columnar arrays preparation method.The structure fabrication processes are simple, available for the light extraction in OLED, lifting device
Rate, strengthen luminosity.
To reach above-mentioned purpose, the technical solution adopted in the present invention is:
A kind of preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, it is characterised in that first will be certain
The PMMA methyl methacrylates and PS granules of polystyrene of ratio dissolve in organic solvent, then common process makes PMMA/
PS films, most obtain free nanometer column array structure through vacuum annealing processing PMMA/PS films afterwards, you can.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:
1)Ito substrate cleans:Deionized water rinsing ito substrate is first used, substrate is then sequentially placed into certain density laboratory
It is cleaned by ultrasonic in ITO electro-conductive glass cleaning agent and deionized water, then the substrate taking-up after cleaning is dried up with nitrogen, finally
Thermal station drying is placed in, it is water stain to remove residual;
2)Treatment with ultraviolet light:By step 1)Ito substrate after cleaning is placed in ultraviolet rays cleaning machine and cleaned, and it is residual to remove substrate surface
The organic matter stayed;
3)The preparation of free nanometer columnar arrays, including:
(1)PMMA particles and PS particles are blended and dissolved in solvent with certain mass ratio, obtain PMMA/PS mixed solutions;
(2)Using PMMA/PS mixed solutions, uniform PMMA/PS films are made on an ito substrate using common process;
(3)The ito substrate with PMMA/PS films of gained is put into vacuum drying oven and annealed, is finally obtained thereon
Film with column micro-nano structure;
4)It is prepared by OLED:By step 3)After the substrate and attaching mask of gained, it is put into vacuum coating equipment chamber, true
The organic layer and electrode layer of OLED is deposited in Altitude successively;
5)Encapsulation:Will be through step 4)The OLED of preparation is moved in glove box from vacuum chamber, uses uv-curable glue and glass
Glass cover plate is packaged to device, is produced.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 3)In, the mass ratio of PMMA particles and the mixing of PS particles is 2-4 ﹕ 7,55-65 DEG C of vacuum drying oven annealing temperature,
Anneal duration 17-19h.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 3)In, the common process for making PMMA/PS films can be spin-coating method, ink-jet printing process, one in spraying process
Kind.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 3)In, free nanometer columnar arrays can also be prepared with other polymers material.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 1)In, certain density laboratory ITO electro-conductive glass cleaning agents wash away the organic substance residues on ito substrate surface,
Deionized water removes the laboratory ITO electro-conductive glass cleaning agent residual and particulate contaminant on ito substrate surface.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 2)In, ultraviolet rays cleaning machine, can be by oxygen molecule O by caused high intensity UV light2Change Viability smelly
Oxygen molecule O3, while the organic molecule on ito substrate surface is excited, make it easier to be absorbed and decomposed by ozone molecule.By
The ito substrate surface of UV ozone processing is more cleaned, and is improved the bonding force on ito substrate surface, is advantageous to the shape of subsequent film
Into.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 3)In, the mass ratio of PMMA particles and the mixing of PS particles is 3 ﹕ 7, and solvent for use is toluene, concentration 20mg/
ML, 60 DEG C of vacuum drying oven annealing temperature, anneal duration 18h.
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 4)In, the vacuum in vacuum coating equipment chamber<2×10-7Torr。
A kind of described preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, its feature exist
In:The step 5)In, glove box water oxygen content is strict controlled in extremely low scope, avoids water and oxygen to prepared OLED devices
The influence of part film layer.
The present invention principle be:
Ito substrate with PMMA/PS films is put into vacuum drying oven and annealed.In annealing process, with solvent not
Disconnected volatilization, PMMA/PS films are separated, i.e., the PMMA materials and PS materials as solute occur respectively in annealing process
Separate out, reunite, deposition process.Above-mentioned phase separation can be controlled by conditions such as PMMA and PS mass ratio and temperature
Journey, regulation and control form the shape and volume of micro-nano structure, finally give the required film with column micro-nano structure.
As shown in figure 1, in conventional OLED device, exciton is propagated through in organic layer recombination luminescence, light device inside
Loss at total reflection is easily produced in journey, light emission rate is relatively low;After columnar arrays structure, beam projecting angle is changed, is reduced
Loss at total reflection, improve light emission rate.As shown in Fig. 2 columnar arrays increase organic surface product, so as to increase effective hair
Light area.
Compared with the prior art, beneficial effects of the present invention are embodied in:
Phase separation of the invention by regulating and controlling PMMA/PS films, free nanometer column battle array is prepared on an ito substrate
Array structure, and be applied in OLED.The array structure causes the outgoing condition of OLED transmitting light to change,
Light loss can effectively be suppressed, improve light extraction efficiency;The efficient lighting area of device is also increased simultaneously, improves luminance
Degree.It is used for the micro-nano structure manufacturing process of OLED compared to other, this method technique is simple, and cost is low, is adapted to extensive raw
Production uses.
Brief description of the drawings
Fig. 1 is the schematic diagram that array structure improves OLED light extraction efficiency, wherein preceding figure is conventional device, rear figure is to adopt
With the device of array structure;
Fig. 2 is the schematic diagram that array structure increases OLED efficient lighting area;
Fig. 3 is the free nanometer column array structure schematic diagrames of PMMA/PS;
Fig. 4 is the atomic force surface topography X-Y scheme of the free nanometer columnar arrays of PMMA/PS(It is left)And graphics(It is right);
Fig. 5 is brightness-voltage curve figure of OLED, and wherein A is conventional device, and B is to have own nanometer columnar arrays
Device.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is given based on technical solution of the present invention
Detailed embodiment and specific operation process, but protection scope of the present invention is not limited to following embodiments.
As shown in Figure 1,2,3, 4, a kind of preparation method for being used to increase the free nanometer columnar arrays of efficient lighting area,
Comprise the following steps:
1)Ito substrate cleans:Deionized water rinsing ito substrate is first used, substrate is then sequentially placed into the reality that volumetric concentration is 5%
Test in room ITO electro-conductive glass cleaning agent and deionized water and be cleaned by ultrasonic, the substrate after cleaning is dried up with nitrogen, then is placed in
100 DEG C of drying 10min of thermal station, it is water stain to remove residual;
2)UV ozone processing:By step 1)Ito substrate after cleaning is placed in ultraviolet rays cleaning machine and cleaned, and removes substrate surface
The organic matter of residual, wherein high intensity UV light wave a length of 185nm and 254nm, processing time are caused by ultraviolet rays cleaning machine
20min;
3)The preparation of free nanometer columnar arrays, including:
(1)PMMA particles and PS particles are blended and dissolved in toluene solvant with the ﹕ 7 of mass ratio 3, concentration 20mg/mL, then
3h is shaken in thermal station and fully dissolves hybrid particles, obtains PMMA/PS mixed solutions.Thermal station temperature 60 C, vibration rotating speed 600r/
min;
(2)PMMA/PS mixed solutions are dropped in and are placed in spin coating instrument through step 2)On ito substrate after processing, spin coating obtains
Even PMMA/PS films.Spin coating instrument rotating speed is 2000r/min, spin coating duration 30s;
(3)Ito substrate with PMMA/PS films is put into vacuum drying oven, it is annealed to obtain with column micro-nano structure
Film, wherein annealing temperature are 60 DEG C, annealing time 18h.The free nanometer column array structure schematic diagram of gained as shown in figure 3,
Atomic force surface topography X-Y scheme(It is left)And graphics(It is right)As shown in Fig. 4.
4)It is prepared by OLED:Will be through step 3)The ito substrate of processing is put into vacuum coating equipment chamber, is evacuated to 2
×10-7The organic layer and electrode layer of OLED is deposited after Tor successively;
5)Encapsulation:Will be through step 4)The OLED of preparation moves to glove box from vacuum chamber(Glove box parameter is oxygen content<
0.1ppm, water content<0.01ppm)In, device is packaged using uv-curable glue and glass cover-plate, extraneous with isolation
Water and oxygen.
Shown in Fig. 4, for the atomic force surface topography two for the free nanometer columnar arrays being prepared using this patent method
Dimension figure(It is left)And graphics(It is right), more uniform intensive irregular columnar arrays are prepared through this patent method as can be seen from Figure
Structure, wherein columnar arrays diameter about 100nm, height about 100nm.
OLED prepared by the above method is tested, it is as shown in Figure 5 to obtain brightness-voltage curve.Figure
In as can be seen that identical voltage under, the OLED B for having free nanometer columnar arrays compares conventional OLED device A, and brightness has
Greatly improve.During wherein 14V, there is the device brightness of free nanometer columnar arrays up to 1174.4cd/m2, than conventional OLED devices
The brightness of part(350.23cd/m2)235% is improved, illustrates that free nanometer columnar arrays are used for OLED, OLED can be increased
The efficient lighting area of device, change the angle of emergence of its light, improve light extraction efficiency, the bright of OLED can be greatly improved
Degree.
Claims (5)
1. a kind of preparation method for being used to strengthen the luminous free nanometer columnar arrays of OLED, it is characterised in that first by one
The PMMA methyl methacrylates and PS granules of polystyrene of certainty ratio dissolve in organic solvent, then common process makes
PMMA/PS films, most obtain free nanometer column array structure through vacuum annealing processing PMMA/PS films afterwards, you can.
2. specifically include following steps:A kind of according to claims 1 is used to strengthening that OLED is luminous freely to be received
The preparation method of rice columnar arrays, it is characterised in that:
1)Ito substrate cleans:Deionized water rinsing ito substrate is first used, substrate is then sequentially placed into certain density laboratory
It is cleaned by ultrasonic in ITO electro-conductive glass cleaning agent and deionized water, then the substrate taking-up after cleaning is dried up with nitrogen, finally
Thermal station drying is placed in, it is water stain to remove residual;
2)Treatment with ultraviolet light:By step 1)Ito substrate after cleaning is placed in ultraviolet rays cleaning machine and cleaned, and it is residual to remove substrate surface
The organic matter stayed;
3)The preparation of free nanometer columnar arrays, including:
(1)PMMA particles and PS particles are blended and dissolved in solvent with certain mass ratio, obtain PMMA/PS mixed solutions;
(2)Using PMMA/PS mixed solutions, uniform PMMA/PS films are made on an ito substrate using common process;
(3)The ito substrate with PMMA/PS films of gained is put into vacuum drying oven and annealed, is finally obtained thereon
Film with column micro-nano structure;
4)It is prepared by OLED:By step 3)After the substrate and attaching mask of gained, it is put into vacuum coating equipment chamber, true
The organic layer and electrode layer of OLED is deposited in Altitude successively;
5)Encapsulation:Will be through step 4)The OLED of preparation is moved in glove box from vacuum chamber, uses uv-curable glue and glass
Glass cover plate is packaged to device, is produced.
A kind of 3. making side for being used to strengthen the luminous free nanometer columnar arrays of OLED according to claims 1
Method, it is characterised in that:The step 3)In, the mass ratio of PMMA particles and the mixing of PS particles is 2-4 ﹕ 7, and vacuum drying oven annealing is warm
55-65 DEG C of degree, anneal duration 17-19h.
A kind of 4. making side for being used to strengthen the luminous free nanometer columnar arrays of OLED according to claims 1
Method, it is characterised in that:The step 3)In, the common process for making PMMA/PS films can be spin-coating method, ink-jet printing process,
One kind in spraying process.
A kind of 5. making side for being used to strengthen the luminous free nanometer columnar arrays of OLED according to claims 1
Method, it is characterised in that:The step 3)In, free nanometer columnar arrays can also be prepared with other polymers material.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109270604A (en) * | 2018-09-01 | 2019-01-25 | 哈尔滨工程大学 | A kind of preparation method of microlens array |
CN109448564A (en) * | 2019-01-04 | 2019-03-08 | 京东方科技集团股份有限公司 | A kind of display panel and preparation method thereof, display device |
CN111384287A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
-
2017
- 2017-07-26 CN CN201710615393.0A patent/CN107689428B/en active Active
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109270604A (en) * | 2018-09-01 | 2019-01-25 | 哈尔滨工程大学 | A kind of preparation method of microlens array |
CN111384287A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
CN111384287B (en) * | 2018-12-29 | 2021-06-22 | Tcl科技集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
CN109448564A (en) * | 2019-01-04 | 2019-03-08 | 京东方科技集团股份有限公司 | A kind of display panel and preparation method thereof, display device |
US11150401B2 (en) | 2019-01-04 | 2021-10-19 | Chengdu Boe Optoelectronics Technology Co., Ltd. | Display panel, method for fabricating the same, and display device |
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