CN103700784A - Patterned electrode preparation method - Google Patents
Patterned electrode preparation method Download PDFInfo
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- CN103700784A CN103700784A CN201310498471.5A CN201310498471A CN103700784A CN 103700784 A CN103700784 A CN 103700784A CN 201310498471 A CN201310498471 A CN 201310498471A CN 103700784 A CN103700784 A CN 103700784A
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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
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
- H10K71/611—Forming conductive regions or layers, e.g. electrodes using printing deposition, e.g. ink jet printing
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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
- H10K71/621—Providing a shape to conductive layers, e.g. patterning or selective deposition
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the field of organic electronic devices and particularly relates to a patterned electrode preparation method. The invention adopts the technical scheme as follows: an electrode pattern protection film with oil ink is printed on the substrate of an electrode by a UV flat inkjet printer, the substrate is put into a corrosive liquid to corrode the electrode not protected by the oil ink on the substrate so as to form the patterned electrode on the substrate, the oil ink is removed through ultrasonic washing with the help of deionized water and an alkaline solution, then the patterned electrode is prepared, and the organic electronic device is further prepared on the patterned electrode. The patterned electrode prepared through the method provided by the invention has tidy edges, is not zigzag and simple in operation and does not need special process or equipment, and the patterned electrode preparation method is suitable for manufacturing a metal oxide electrode commonly used for a semiconductor device, and popularization and application are facilitated.
Description
Technical field
The invention belongs to organic electronic device field, be specifically related to a kind of preparation method of patterned electrodes.
Background technology
The graphical of organic electronic device transparency electrode adopts traditional wet etching method to prepare conventionally; traditional electrode pattern method is spin coating on conducting film (printing) photoresist; after the photo-mask processs such as front baking, exposure, development, post bake are processed; form the graphical of protective layer, then the semiconductor chip immersion to be corroded with protective layer figure is controlled in the corrosive liquid in certain temperature range and is corroded.Finally, the semiconductor chip of taking-up is rinsed well with deionized water, put into stripper and remove photoresist, and then process, obtain patterned electrode.
This traditional method completes conventionally in gold-tinted dust free room, and gluing is controlled the thickness of glued membrane by rotating speed, time, and the gluing electrode pattern that evenly guarantee is prepared is complete, can not occur dirty point, bubble, otherwise figure can lack in gluing process; Exposure need to be transferred to mask pattern on substrate, different electrode patterns needs different masks, exposure process need to be controlled the size of exposure, the sensitization degree that the time is adjusted photoresist, and sensitization is crossed the rear figure that develops at most and can be washed out, and sensitization is crossed figure at least and do not separated; Developer solution need to support the use with photoresist, and controls developing time well, otherwise there will be less aobvious, cross to manifest and resemble; Therefore, the existing method of preparing patterned electrodes not only needs more expensive gluing, exposure, developing apparatus, and needs corresponding technology controlling and process, and this preparation method's efficiency is low, cost is high, poor operability.
Summary of the invention
The object of the invention is to solve the deficiencies in the prior art and shortcoming, a kind of preparation method of patterned electrodes is provided.The technical program, without gluing, exposure, developing apparatus and technique, only need to be used a UV spray drawing machine can complete photolithography process, also without preparing mask, only need will in the electrode pattern input UV spray drawing machine designing, can print figure.
The preparation method of a kind of patterned electrodes provided by the invention, its step is as follows:
(1) substrate with different materials electrode is cleaned up, dried;
(2) UV etching resisting ink is packed in UV flat-plate ink jet printer, open UV flat-plate ink jet printer and set parameter, the electrode pattern designing in computer is inputted in UV flat-plate ink jet printer by data wire; The substrate cleaning up is inserted in UV flat-plate ink jet printer, and UV spray drawing machine prints the electrode pattern with ink on the substrate of electrode, on electrode, forms UV etching resisting ink diaphragm;
(3) baking oven of the substrate obtaining in step (2) being put into 80 ℃ ~ 200 ℃ toasts 20 ~ 60 min, takes out nature cooling; Then put into corrosive liquid, after corrosion 60 ~ 300s, do not have the electrode of ink figure protection to be corroded, thereby on substrate, obtain patterned electrode;
(4) step (3) is obtained to patterned electrode substrate and put into deionized water rinsing 5 ~ 60 min, then put into temperature and be 30 ~ 100 ℃ and 5% ~ 25% alkaline solution ultrasonic, remove after ink, use again rinsed with deionized water, take out and dry, then on patterned electrode, be prepared with organic electronic device.
The described electrode with different materials of above-mentioned steps (1) is metal and metal oxide electrode thereof, silicon base compound electrode.Wherein metal is any one in gold, silver, copper, aluminium, chromium, zinc, magnesium; Alloy can be any one in molybdenum-aluminium, molybdenum-nickel, molybdenum-niobium, aluminium-neodymium, magnesium-aluminium; Metal oxide is any one or multiple mixture in ruthenium-oxide, cupric oxide, tin oxide, manganese oxide, cobalt oxide, nickel oxide, zinc oxide, silver oxide, gallium oxide, indium oxide, germanium oxide, aluminium oxide.
The described electrode substrate of above-mentioned steps (1) is flexibility or inflexibility substrate, and wherein inflexibility substrate is any one in glass, quartz plate, mica sheet, metal oxide sheet, timber, floor tile, ceiling and potsherd; Flexible substrate is any one in PETG, PEN, Merlon, polyether sulfone, polyimides, Polyetherimide.
The described UV flat-plate ink jet printer of above-mentioned steps (2) is the perfect adaptation of UV cured printing ink and digital spray printing technology.The operating efficiency of UV flat-plate ink jet printer and air brushing quality are very high, can carry out color painting in surfaces of various materials, not only can air brushing soft material, and can, to diversification future development, be also the development trend of digital spray printing technology.
The constituent of the UV etching resisting ink diaphragm that above-mentioned steps (2) is described at least comprises 2 kinds of acrylate, light trigger, organic carrier and additives.Wherein, 2 kinds of acrylate: a kind of is to contain carboxyl, another kind is epoxy acrylate monomer or dimer, and functional acrylic resin, if the acrylic resin that improves adhesive force is, the acrylic resin that reduces viscosity, cross-linking type acrylic resin, chemical resistant acrylic resin and can quick-setting acrylic resin; Described epoxy acrylate monomer or dimer should be selected low-viscosity, nonvolatile low-molecular-weight epoxy resin, as bisphenol type epoxy diacrylate; Described additive comprises conductive agent, surfactant, sensitising agent and light stabilizer.
The described corrosive liquid of above-mentioned steps (3) is any one or the multiple mixture in hydrochloric acid/nitric acid mixed liquor, chlorine/hydrochloric acid mixed solution, hydrogen peroxide/hydrochloric acid mixed solution, sodium chlorate/hydrochloric acid, hydrochloric acid/sulfuric acid mixture liquid.
The structure of the organic electronic device that above-mentioned steps (4) is described is comprised of substrate, anode, hole injection layer, hole transmission layer, organic luminous layer, electron transfer layer, electron injecting layer and metallic cathode layer successively.Described organic electronic device is mainly organic electroluminescent device OLED, OTFT OTFT, organic solar batteries OPV, electrochemical sensor or biology sensor.
The metallic cathode of above-mentioned organic electronic device can be the alloy materials such as the metal simple-substances such as gold (Au), silver (Ag), copper (Cu), aluminium (Al), titanium (Ti), nickel (Ni) or silver-colored magnesium (Ag-Mg), silver-colored titanium (Ag-Ti).
The patterned electrodes that adopts the inventive method to prepare, neat in edge, without zigzag, simple to operate, without special process and special installation, simplified the spin coating in conventional lithography process (printing) photoresist, through photo-mask processs such as front baking, exposure, development, post bakes, realized more fast, simpler, more effective patterned electrodes prepare approach.Be applicable to manufacture the metal oxide electrode that semiconductor device is conventional, be easy to promote the use of.
Accompanying drawing explanation
Fig. 1 is printed on by ink diaphragm the structural representation having in ITO electrode substrate in embodiment 1, and 1 is the ITO electrode in glass substrate, and 2 is ink diaphragm.
Fig. 2 is that in embodiment 1 diaphragm region, ITO electrode is through the resistance variations curve chart of different time corrosion, and wherein resistance change rate adopts the four probe method of FOUR-POINT PROBE METER to measure, and ITO electrode square resistance in corrosion process increases.
Fig. 3 is the microstructure figure that the graphical ITO electrode of embodiment 1 after corrosion and glass substrate are amplified 500 times under the microscope, and 1 is glass substrate, and 2 is ITO electrode after corrosion, and pattern edge is neat as seen from the figure.
Fig. 4 is the testing current curve chart that embodiment 2 utilizes organic electronic light emitting device prepared by ITO electrode that distinct methods corrosion obtains.Curve 1 is the I-V curve of the organic electronic light emitting device prepared of ITO electrode that the corrosion of general photoetching method obtains; Curve 2 is I-V curves of the organic electronic light emitting device prepared of ITO electrode that the method for utilizing UV spray drawing machine to print diaphragm corrosion obtains.
Fig. 5 is the luminance test curve chart that embodiment 2 utilizes organic electronic light emitting device prepared by ITO electrode that distinct methods corrosion obtains.Curve 1 is the brightness curve of the organic electronic light emitting device prepared of ITO electrode that the corrosion of general photoetching method obtains; Curve 2 is brightness curves of the organic electronic light emitting device prepared of ITO electrode that the method for utilizing UV spray drawing machine to print diaphragm corrosion obtains.
Embodiment
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is described in detail.
Embodiment 1:
Utilize UV spray drawing machine to print the method for diaphragm corrosion, erode away electrode respectively in the ITO of 25 * 25mm conductive substrates, be of a size of 10 * 25mm, as shown in Fig. 1, wherein black region is ITO electrode.The time of corrosion is respectively 50 s, 100 s, 150 s, 200 s, etchant solution is by volume for the ratio mixed preparing of 10:0.8:10 forms by the hydrochloric acid that is 36% by mass fraction and 98% nitric acid and deionized water, utilize FOUR-POINT PROBE METER to survey the square resistance of different etching time bottom electrodes, as shown in Fig. 2, square resistance is trend over time, and between 50 s ~ 200 s, just can obtain patterned ITO electrode, pattern edge is neat, as shown in Fig. 3, this figure is the microstructure figure of 500 times.From scheming: in the interface of ITO electrode corrosion, amplify 500 times through microscope, edge is still very clear, without zigzag, free of pinholes, residual without adhesive.
Embodiment 2:
By photoresist mask and UV spray drawing machine, print the method for diaphragm corrosion and prepared respectively the substrate (25 * 25mm) with ITO conductive electrode (10 * 25mm); and having prepared on this basis structure is: glass/ITO(180nm)/NPB (50nm)/DCM:(Alq3 0.5% 20nm) the OLED device of/Alq3 (30nm)/Ca (10nm)/Ag; wherein ITO is anode; NPB is hole transmission layer; DCM is luminescent layer; Alq3 is electron transfer layer; Ca is resilient coating, and Ag is negative electrode.Wherein, A group device ITO electrode prepares by photoetching corrosion, and B group device ITO electrode is printed diaphragm caustic solution by UV spray drawing machine and prepared, and detailed process is as follows:
(1) A, B group device substrate is the glass with ITO electrode, and first, by substrate scrub clean, glass substrate is of a size of 25 * 25mm; Corrosion preparation rectangle ITO electrode centered by the center of glass substrate, it is of a size of 10 * 25mm;
(2) A handling well, B group device substrate is placed in to multi-source organic molecule gas-phase deposition system.The vacuum degree of system can reach 10-5Pa, and in the process of film growth, the vacuum degree of system maintains 4 * 10-4Pa left and right.Centered by the center of glass substrate, utilization is of a size of organic mask plate of 20 * 20mm and prepares successively each layer (comprising NPB (50nm)/DCM:(Alq3 0.5% 20nm)/Alq3 (30nm)/Ca (10nm) that area is the organic electronic device of 20 * 20mm), the metal mask version evaporation that the last zone line utilization at substrate is of a size of 10 * 23mm is of a size of 10 * 23mm metal A g negative electrode, thereby obtains OLED device;
(3) carry out the contrast of A, bis-groups of device current tests of B, luminance test.As shown in Fig. 4; from electric current, with the change curve of voltage, can find out that the performance of B group device increases, the device of ITO electrode prepared by this explanation employing UV spray drawing machine printing diaphragm etch increases than the performance of the device of the ITO electrode that adopts photoetching method to prepare.As shown in Fig. 5, from brightness, with the change curve of voltage, can find out that the brightness of B group device increases, this explanation UV spray drawing machine is printed diaphragm and has effectively been intercepted the erosion of etchant solution to ITO electrode.
Described in summary; utilize the resulting ITO electrode edge of method of UV spray drawing machine printing diaphragm corrosion clear; without zigzag; free of pinholes; residual without adhesive, the electric conductivity of ITO electrode is had no significant effect, can prevent cabling short circuit or broken string when preparing microdevice simultaneously; the device performance of the ITO electrode of therefore, preparing by the method is good.
Claims (8)
1. a preparation method for patterned electrodes, its step is as follows:
(1) substrate with different materials electrode is cleaned up, dried;
(2) UV etching resisting ink is packed in UV flat-plate ink jet printer, open UV flat-plate ink jet printer and set parameter, the electrode pattern designing in computer is inputted in UV flat-plate ink jet printer by data wire; The substrate cleaning up is inserted in UV flat-plate ink jet printer, and UV spray drawing machine prints the electrode pattern with ink on the substrate of electrode, on electrode, forms UV etching resisting ink diaphragm;
(3) substrate obtaining in step (2) is put into baking oven and toast, take out nature cooling; Then put into corrosive liquid, after corrosion a period of time, do not have the electrode of ink figure protection to be corroded, thereby on substrate, obtain patterned electrode;
(4) substrate step (3) being obtained is put into deionized water rinsing, then puts into alkaline solution, ultrasonic at a certain temperature, after removal ink, by rinsed with deionized water, takes out and dries, and finally on patterned electrode, is prepared with organic electronic device.
2. according to the preparation method of a kind of patterned electrodes described in claim 1, it is characterized in that: the described electrode with different materials is metal and metal oxide electrode thereof, silicon base compound electrode, and wherein metal is any one in gold, silver, copper, aluminium, chromium, zinc, magnesium; Alloy can be any one in molybdenum-aluminium, molybdenum-nickel, molybdenum-niobium, aluminium-neodymium, magnesium-aluminium; Metal oxide is any one or multiple mixture in ruthenium-oxide, cupric oxide, tin oxide, manganese oxide, cobalt oxide, nickel oxide, zinc oxide, silver oxide, gallium oxide, indium oxide, germanium oxide, aluminium oxide.
3. according to the preparation method of a kind of patterned electrodes described in claim 1, it is characterized in that: the substrate of described electrode is flexibility or inflexibility substrate, wherein inflexibility substrate is any one in glass, quartz plate, mica sheet, metal oxide sheet, timber, floor tile, ceiling, potsherd; Flexible substrate is any one in PETG, PEN, Merlon, polyether sulfone, polyimides, Polyetherimide.
4. according to the preparation method of a kind of patterned electrodes described in claim 1, it is characterized in that: the constituent of described UV etching resisting ink diaphragm at least comprises 2 kinds of acrylate, light trigger, organic carrier and additives.
5. according to the preparation method of a kind of patterned electrodes described in claim 1 or 4, it is characterized in that: 2 kinds of described acrylate: a kind of is to contain carboxyl, another kind is epoxy acrylate monomer or dimer, and functional acrylic resin, if the acrylic resin that improves adhesive force is, the acrylic resin that reduces viscosity, cross-linking type acrylic resin, chemical resistant acrylic resin and can quick-setting acrylic resin; Described epoxy acrylate monomer or dimer should be selected low-viscosity, nonvolatile low-molecular-weight epoxy resin, as bisphenol type epoxy diacrylate; Described additive comprises conductive agent, surfactant, sensitising agent and light stabilizer.
6. the preparation method of a kind of patterned electrodes according to claim 1, is characterized in that: described corrosive liquid comprises any one or the multiple mixture in hydrochloric acid/nitric acid mixed liquor, chlorine/hydrochloric acid mixed solution, hydrogen peroxide/hydrochloric acid mixed solution, sodium chlorate/hydrochloric acid mixed solution, hydrochloric acid/sulfuric acid mixture liquid, iron chloride/hydrochloric acid mixed solution, sulfuric acid/chromic acid mixture, sulfuric acid/hydrogen peroxide mixed liquor.
7. the preparation method of a kind of patterned electrodes according to claim 1, is characterized in that: organic electronic device is comprised of substrate, anode, hole injection layer, hole transmission layer, organic luminous layer, electron transfer layer, electron injecting layer and metallic cathode layer successively.
8. according to the preparation method of a kind of patterned electrodes described in claim 1, it is characterized in that: organic electronic device is organic electroluminescent device OLED, OTFT OTFT, organic solar batteries OPV, electrochemical sensor or biology sensor.
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| CN201310498471.5A CN103700784A (en) | 2013-10-22 | 2013-10-22 | Patterned electrode preparation method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462343A (en) * | 2017-08-10 | 2017-12-12 | 上海幂方电子科技有限公司 | A kind of full printing flexible sensor and its preparation technology |
| CN107672333A (en) * | 2017-09-29 | 2018-02-09 | 华南理工大学 | A kind of method that UV pretreatments improve solution-type silver inks water inkjet printing quality of forming film |
| CN108374173A (en) * | 2018-04-19 | 2018-08-07 | 东北大学 | The environmental-friendly chemical milling solution and chemical milling method of single crystal super alloy precision castings |
| CN110739267A (en) * | 2019-09-12 | 2020-01-31 | 西北工业大学 | High-precision flexible microcircuit processing method based on printing and photoetching combined mode |
| US10676809B2 (en) | 2018-06-20 | 2020-06-09 | Lockheed Martin Corporation | Methods and systems for generating patterns on flexible substrates |
| CN112289965A (en) * | 2020-12-16 | 2021-01-29 | 浙江宏禧科技有限公司 | Method for preparing silicon-based OLED anode by wet etching |
| CN114280869A (en) * | 2021-12-29 | 2022-04-05 | 湖南鼎一致远科技发展有限公司 | Inorganic electroluminescent device and UV (ultraviolet) spray printing preparation method thereof |
-
2013
- 2013-10-22 CN CN201310498471.5A patent/CN103700784A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462343A (en) * | 2017-08-10 | 2017-12-12 | 上海幂方电子科技有限公司 | A kind of full printing flexible sensor and its preparation technology |
| CN107672333A (en) * | 2017-09-29 | 2018-02-09 | 华南理工大学 | A kind of method that UV pretreatments improve solution-type silver inks water inkjet printing quality of forming film |
| CN108374173A (en) * | 2018-04-19 | 2018-08-07 | 东北大学 | The environmental-friendly chemical milling solution and chemical milling method of single crystal super alloy precision castings |
| CN108374173B (en) * | 2018-04-19 | 2019-06-11 | 东北大学 | The environmental-friendly chemical milling solution and chemical milling method of single crystal super alloy precision castings |
| US10676809B2 (en) | 2018-06-20 | 2020-06-09 | Lockheed Martin Corporation | Methods and systems for generating patterns on flexible substrates |
| CN110739267A (en) * | 2019-09-12 | 2020-01-31 | 西北工业大学 | High-precision flexible microcircuit processing method based on printing and photoetching combined mode |
| CN112289965A (en) * | 2020-12-16 | 2021-01-29 | 浙江宏禧科技有限公司 | Method for preparing silicon-based OLED anode by wet etching |
| CN114280869A (en) * | 2021-12-29 | 2022-04-05 | 湖南鼎一致远科技发展有限公司 | Inorganic electroluminescent device and UV (ultraviolet) spray printing preparation method thereof |
| CN114280869B (en) * | 2021-12-29 | 2024-04-02 | 湖南鼎一致远科技发展有限公司 | Inorganic electroluminescent device and UV (ultraviolet) inkjet printing preparation method thereof |
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Application publication date: 20140402 |