CN102320752A - Patterning method for material - Google Patents
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- CN102320752A CN102320752A CN201110154332A CN201110154332A CN102320752A CN 102320752 A CN102320752 A CN 102320752A CN 201110154332 A CN201110154332 A CN 201110154332A CN 201110154332 A CN201110154332 A CN 201110154332A CN 102320752 A CN102320752 A CN 102320752A
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Abstract
The invention discloses a patterning method for a material. The method comprises the following steps of: 1) preparing a layer of macromolecular film on a substrate; 2) coating a good solvent for the macromolecular film on the surface of the obtained macromolecular film by using an ink jet printing method, and obtaining a patterned macromolecular film; and 3) sequentially preparing a layer of target material film and a layer of polystyrene film on the patterned macromolecular film and the surface of the exposed substrate, soaking in water, peeling the polystyrene film, all the target material film except patterns and the macromolecular film, and thus completing patterning of the material. The shortest channel length of a graphene electrode can reach 2 microns, the graphene electrode obtained on the silicon dioxide substrate can be directly applied to an organic field effect transistor and used as an effective current carrier injection electrode, and other transfer or post treatment means is not needed.
Description
Technical field
The present invention relates to the patterning method of material, particularly relate to a kind of method of utilizing inkjet printing methods material to be carried out patterning.
Background technology
The chemical reduction Graphene is considered to a kind of electro-conductive material of excellence because have favorable mechanical performance and high specific conductivity, can substitute present widely used tin indium oxide (ITO), is applied to big area, and is transparent, flexible occasion.In addition, can mate each other because the energy level of grapheme material is arranged with a lot of organic semiconductor material, thereby be expected to, be applied to many organic electronics and learn in the device as outstanding electrode injecting material.In fact, since Graphene was found, people had learned in the device at a lot of organic electronics and have showed its good technical prospect (J.Wu, H.A.Becerril, Z.Bao, Z.Liu, Y.Chen, P.Peumans, Appl.Phys.Lett.2008,92,263302; G.Eda, Y.-Y.Lin, C.Mattevi, H.Yamaguchi, H.-A.Chen, I.S.Chen, C.-W.Chen, M.Chhowalla, Adv.Mater.2010,22,505; J.Wu, M.Agrawal, H.c.A.Becerril, Z.Bao, Z.Liu, Y.Chen, P.Peumans, ACS Nano 2009,4,43).In the application that these have been reported, the patterning of Graphene is mainly realized through photoetching and beamwriter lithography.
Stripping technology (lift-off technique) is used very extensive in photoetching, yet in spray ink Printing, does not also report.Because the grain graininess of Graphene is bigger, directly prints and be difficult to realization.If adopt stripping technology to prepare Graphene electrodes, just relate to the patterning problem of mask (mask) layer.How to utilize inkjet technology to prepare the mask layer of patterning, just become technological difficulties in the Graphene stripping technology.In case obtain good method, make that inexpensive chemical reduction grapheme material is convenient-to-running to prepare with inkjet technology, can greatly help the application of this material in electronics.
Summary of the invention
The patterning method that the purpose of this invention is to provide a kind of material.
The patterning method of material provided by the invention comprises the steps:
1) preparation one deck macromolecule membrane in substrate;
2) be coated with the good solvent of said macromolecule membrane in the method for said step 1) gained macromolecule membrane surface by utilizing spray ink Printing, obtain the macromolecule membrane behind the patterning;
3) in said step 2) on the macromolecule membrane behind the gained patterning and after the said substrate surface that exposes prepares the film and one deck polystyrene film of one deck target material successively; Peel said polystyrene film off after Yu Shuizhong soaks and except that pattern the film and the said macromolecule membrane of all target materials, accomplish the patterning of said material.
In the said step 1), said substrate is the silicon chip that quartz plate, silicon chip or surface have silicon dioxide layer, and wherein, in the said silicon chip that has a silicon dioxide layer, the thickness of said silicon dioxide layer is the 100-500 nanometer, preferred 300 nanometers; The material that constitutes said macromolecule membrane is polyacrylonitrile, PS or polymethylmethacrylate, and preferable weight-average molecular weight is the polyacrylonitrile of 10000-1000000, and more preferably weight-average molecular weight is 200000 polyacrylonitrile; The thickness of said macromolecule membrane is the 1-100 nanometer, preferred 2 nanometers; The said method for preparing macromolecule membrane is a spin-coating method; In the said spin-coating method, rotating speed is 2000-5000 rev/min, preferred 3500 rev/mins;
Said step 2) in the method for spray ink Printing, the shower nozzle of ink-jet printer is 20 microns to 100 microns, preferred 30 microns; The adjacent drops spacing is the 120-70 micron, preferred 87 microns; Service temperature is 30-100 ℃, preferred 80 ℃; The good solvent of said macromolecule membrane is selected from N, at least a in dinethylformamide, toluene and the chlorobenzene, preferred N, dinethylformamide; In this step; Because spray ink Printing step solvent for use is the good solvent of step 1) gained macromolecule membrane, when carrying out spray ink Printing, this solvent can dissolve macromolecule membrane according to predetermined pattern; Expose the surface of substrate (like silicon-dioxide), thereby form the macromolecule membrane of patterning.In actually operating, can confirm the number of required drop according to required pattern, as making electrode pair, then the number of gained drop is 2.
In the said step 3), the thickness of said target material film is the 1-10 nanometer, preferred 5 nanometers; The thickness of said polystyrene film is 700 nanometers to 10 micron, preferred 1 micron; The weight-average molecular weight of said PS is 10000-1000000, preferred 200000; Said target material be can with the said substrate bonded of step 1) material, preferred graphene oxide or chromium; Institute is set forth in the water in the soaking step, and the time is 30 minutes to 3 hours, preferred 90 minutes; Prepare the film of said target material and the method for polystyrene film and be spin-coating method or hot vapour deposition method; In the said spin-coating method, rotating speed is 3000-8000 rev/min, preferred 4000 rev/mins; In the said hot evaporation coating method, vacuum tightness is less than 4 * 10
-4Pascal, evaporation rate was 1 dust/second.In this strip step, owing to have firm binding ability between target material and the substrate, thereby; When peeling off; Step 2) the target material film that covers in the substrate that patterning exposes is not stripped from, and all the other regional films are all peeled off, thereby has accomplished the patterning of target material.
The patterning method of said material also comprised the steps: before said step 1), used washing composition, water, deionized water, ethanol and acetone clean respectively said substrate.
The electrode for preparing according to the method described above, the electrode that especially is made up of Graphene or chromium, and the application of this method in the preparation electrode also belong to protection scope of the present invention.The thickness of this electrode is the 1-10 nanometer, and channel length is the 1-100 micron.
Because graphene oxide when using as electrode, need recover its electroconductibility through the reductive method and change Graphene into, so the above-mentioned electrode that is made up of Graphene; Be will be according to the method described above graphene oxide behind the patterning; With the graphene oxide reduction and get, this method is an ordinary method through annealing or the method that adds reductive agent, and the method for various redox graphenes commonly used is all suitable; In said method for annealing, vacuum tightness can be 8 * 10
-4-1 * 10
-5Pa is preferably less than 4 * 10
-4Pa, temperature can be 400-500 ℃, and preferred 450 ℃, the time can be 1-4 hour, preferred 2 hours.
In addition, the application of the electrode that the invention described above provides in the preparation organic field effect tube also belongs to protection scope of the present invention.
The present invention discloses a kind of method of utilizing inkjet technology and stripping means on silica-primed, directly to prepare graphene oxide first; Prepared graphene thickness of electrode of the present invention is controlled, and the channel length of electrode is controlled, and the channel length minimum can reach 2 microns; This Graphene electrodes does not need to shift, and on silica-primed, can directly be used for the preparation of field-effect transistor; This method not only is confined to the patterning of grapheme material, and other and silica-primed have the material of mortise ability, and like chromium, also available this method is carried out patterning.
Description of drawings
Fig. 1 is a step 2), 3), 5), 6) finish after the optical microscope photograph of substrate;
Fig. 2 is the AFM photo of the Graphene electrodes of embodiment 1 preparation;
Fig. 3 is the flying-spot microscope photo of the Graphene electrodes of the present invention's preparation;
Fig. 4 is applied to the device curve in the organic field effect tube for the Graphene electrodes among the embodiment 1;
Fig. 5 is the electron scanning micrograph of the chromium metal electrode among the embodiment 2.
Embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration, but the present invention is not limited to following examples.Said method is ordinary method if no special instructions.Said material all can get from open commercial sources if no special instructions.
Embodiment 1, in preparation Graphene electrodes and show its application in organic field effect tube on the silica-primed.
1) clean silica-primed:
The silicon chip that the surface is had thickness 300 nano silicons uses each ultrasonic cleaning of washing composition, water, deionized water, acetone and ethanol after 5 minutes successively, oven dry;
2) silicon slice placed that step 1) is disposed places in the desk-top sol evenning machine rotary head; Dripping a weight-average molecular weight and be 200000 polyacrylonitrile concentration is the N of 1.5mg/mL; The solution of dinethylformamide; Regulate the sol evenning machine rotating speed at 3500 rpms, on silicon chip, form uniform polyacrylonitrile macromolecule membrane, thickness is 2 nanometers;
3) spray ink Printing patterning polyacrylonitrile mask layer:
With step 2) in make; The silicon chip that the surface has mask layer places on ink-jet printer (the jetlab II inkjet printing equipment) operator's console, and 80 ℃ of red-tape operati platform temperature drip N at silicon chip surface with ink-jet printer; The dinethylformamide solvent; The printer head of selecting for use is 30 microns, 87 microns of adjacent drops spacings, and pattern is made up of two adjacent drops.
Fig. 1 a is the pattern that the dry back of drop forms on the polyacrylonitrile surface; Can know by figure, the ring that forms at the solvent droplets edge, its width is far smaller than the diameter of drop itself, and this makes the resolving power of stamping machine counter electrode channel region have greatly improved.
4) the silicon chip surface that obtains in step 3) with pattern, spin coating (rotating speed is 4000 rev/mins) graphite oxide aqueous solution three times, preparing a layer thickness is the graphene oxide film of 5 nanometers.
Fig. 1 b has prepared graphene oxide film optical microscope photograph afterwards; Can know that by figure because graphene oxide and silicon dioxide substrates have stronger bonding force, graphene oxide is deposited on the position that exposes silica-primed more easily.
5) polystyrene film of 1 micron of spin coating on step 4) gained graphene oxide film (rotating speed is 4000 a rev/mins) layer thickness; Then substrate was put into water 90 minutes; With tweezers peel polystyrene film off and except that circle pattern the film and the macromolecule membrane of all target materials, accomplish the patterning of graphene oxide.
Fig. 1 c peels the graphene oxide pattern that the PS macromolecule membrane obtains later on off; Can know that by figure the pattern of graphene oxide and the pattern of polyacrylonitrile have good complementary relationship, having proved has good transfer efficiency between the pattern.
6) for the graphene oxide that makes the gained patterning recovers electroconductibility, so that use as electrode, the substrate that will have the graphene oxide pattern places vacuum, when vacuum tightness is lower than 4 * 10
-4Pascal is heated to 450 ℃, keeps promptly obtaining in 2 hours the Graphene of patterning.
Fig. 1 d is the optical microscope photograph through the reduction Graphene electrodes after the reduction of step 6) thermal annealing.
Fig. 2 is the AFM photo through the reduction Graphene electrodes after the step 6).
Fig. 3 is the electron scanning micrograph through the reduction Graphene electrodes after the step 6).
Can know that by figure the channel length of this Graphene electrodes is the 1-2 micron.
Utilize this embodiment to prepare the gained Graphene and prepare organic field effect tube:
This embodiment is prepared gained Graphene electrodes surface adopt the method for hot vapor deposition to prepare one deck pentacene semiconductor film, vacuum tightness is lower than 4 * 10 in the evaporate process
-4Pascal, evaporation rate 1 dust per second obtains the organic field effect tube based on pentacene.
In air, test with Keithley 4200 semi-conductor test instruments.Fig. 4 a is the transition curve of the organic field effect tube that obtains, and Fig. 4 b is the curve of output of the organic field effect tube that obtains.
Can know under the very short situation of electrode raceway groove, still to have good transfer and curve of output by figure.
Embodiment 2, on silica-primed, utilize spray ink Printing and stripping technology that chromium is carried out patterning
1) clean silica-primed:
The silicon chip that the surface is had thickness 300 nano silicons uses each ultrasonic cleaning of washing composition, water, deionized water, acetone and ethanol after 5 minutes successively, oven dry;
2) silicon slice placed that step 1) is disposed places in the desk-top sol evenning machine rotary head; Dripping a weight-average molecular weight and be 200000 polyacrylonitrile concentration is the N of 1.5mg/mL; The solution of dinethylformamide; Regulate the sol evenning machine rotating speed at 3500 rpms, on silicon chip, form uniform polyacrylonitrile macromolecule membrane, thickness 1 nanometer;
3) spray ink Printing patterning polyacrylonitrile mask layer:
With step 2) gained surface places on the ink-jet printer operator's console for the silicon chip of polyacrylonitrile macromolecule membrane; 80 ℃ of red-tape operati platform temperature; Drip N at silicon chip surface with ink-jet printer, dinethylformamide solvent, the printer head of selecting for use are 30 microns; 87 microns of adjacent drops spacings, drop are 2.
4) in vacuum tightness less than 4 * 10
-4Pascal, evaporation rate are under the condition of 1 dust/second, and utilizing hot evaporation coating method vapor deposition one layer thickness on the polyacrylonitrile mask layer is the chromium layer of 5 nanometers.
5) the PS macromolecule membrane of 1 micron of spin coating one deck (rotating speed is 4000 rev/mins) thickness on step 4) gained chromium layer; Then substrate was put into water 90 minutes; With tweezers peel polystyrene film off and except that circle pattern the film and the macromolecule membrane of all target materials, accomplish the patterning of chromium material.
Fig. 5 is the electron scanning micrograph that has patterning chromium electrode on the silicon chip of silicon-dioxide on the surface.It is thus clear that the chromium electrode channel length that obtains is 2 microns, has favorable uniformity.
Claims (9)
1. the patterning method of a material comprises the steps:
1) preparation one deck macromolecule membrane in substrate;
2) be coated with the good solvent of said macromolecule membrane in the method for said step 1) gained macromolecule membrane surface by utilizing spray ink Printing, obtain the macromolecule membrane behind the patterning;
3) in said step 2) on the macromolecule membrane behind the gained patterning and after the said substrate surface that exposes prepares the film and one deck polystyrene film of one deck target material successively; Peel said polystyrene film off after Yu Shuizhong soaks and except that pattern the film and the said macromolecule membrane of all target materials, accomplish the patterning of said material.
2. method according to claim 1 is characterized in that: in the said step 1), said substrate is the silicon chip that quartz plate, silicon chip or surface have silicon dioxide layer; Wherein, In the said silicon chip that has a silicon dioxide layer, the thickness of said silicon dioxide layer is the 100-500 nanometer, preferred 300 nanometers; The material that constitutes said macromolecule membrane is polyacrylonitrile, PS or polymethylmethacrylate, and preferable weight-average molecular weight is the polyacrylonitrile of 10000-1000000, and more preferably weight-average molecular weight is 200000 polyacrylonitrile; The thickness of said macromolecule membrane is the 1-100 nanometer, preferred 2 nanometers;
Said step 2) in the method for spray ink Printing, the shower nozzle of ink-jet printer is 20 microns to 100 microns, preferred 30 microns; The adjacent drops spacing is the 120-70 micron, preferred 87 microns; Service temperature is 30-100 ℃, preferred 80 ℃; The good solvent of said macromolecule membrane is selected from N, at least a in dinethylformamide, toluene and the chlorobenzene, preferred N, dinethylformamide;
In the said step 3), the thickness of said target material film is the 1-10 nanometer, preferred 5 nanometers; The thickness of said polystyrene film is 700 nanometers to 10 micron, preferred 1 micron; The weight-average molecular weight of said PS is 10000-1000000, preferred 200000; Said target material be can with the said substrate bonded of step 1) material, preferred graphene oxide or chromium; Institute is set forth in the water in the soaking step, and the time is 30 minutes to 3 hours, preferred 90 minutes.
3. method according to claim 1 and 2 is characterized in that: the method for preparing macromolecule membrane in the said step 1) is a spin-coating method;
In the said step 3), prepare the film of said target material and the method for polystyrene film and be spin-coating method or hot vapour deposition method.
4. method according to claim 3 is characterized in that: in the said spin-coating method of said step 1), rotating speed is 2000-5000 rev/min, preferred 3500 rev/mins;
In the said spin-coating method of said step 3), rotating speed is 3000-8000 rev/min, preferred 4000 rev/mins; In the said hot evaporation coating method, vacuum tightness is less than 4 * 10
-4Pascal, evaporation rate was 1 dust/second.
5. according to the arbitrary described method of claim 1-4, it is characterized in that: the patterning method of said material, also comprised the steps: before said step 1), use washing composition, water, deionized water, ethanol and acetone clean respectively said substrate.
6. the application of the arbitrary said method of claim 1-5 in the preparation electrode.
7. the arbitrary said method of claim 1-5 prepares the electrode of gained.
8. electrode according to claim 7 is characterized in that: the material that constitutes said electrode is Graphene or chromium; The thickness of said electrode is the 1-10 nanometer, and channel length is the 1-100 micron.
9. claim 7 or the 8 said electrodes application in the preparation organic field effect tube.
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| CN104292984A (en) * | 2013-07-16 | 2015-01-21 | 安炬科技股份有限公司 | Graphene ink and method for manufacturing graphene circuit |
| CN106531878A (en) * | 2016-10-25 | 2017-03-22 | 中国科学院化学研究所 | Preparation method of patterned polyethylene 4-thiol nickel thin film and device |
| CN107478320A (en) * | 2017-08-23 | 2017-12-15 | 京东方科技集团股份有限公司 | Transistor sound sensing element and preparation method thereof, sonic transducer and portable equipment |
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| CN104292984A (en) * | 2013-07-16 | 2015-01-21 | 安炬科技股份有限公司 | Graphene ink and method for manufacturing graphene circuit |
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| CN106531878A (en) * | 2016-10-25 | 2017-03-22 | 中国科学院化学研究所 | Preparation method of patterned polyethylene 4-thiol nickel thin film and device |
| CN106531878B (en) * | 2016-10-25 | 2019-02-05 | 中国科学院化学研究所 | Pattern the preparation method of four mercaptan nickel film of polyethylene and device |
| CN107478320A (en) * | 2017-08-23 | 2017-12-15 | 京东方科技集团股份有限公司 | Transistor sound sensing element and preparation method thereof, sonic transducer and portable equipment |
| CN107478320B (en) * | 2017-08-23 | 2019-11-05 | 京东方科技集团股份有限公司 | Transistor sound sensing element and preparation method thereof, sonic transducer and portable equipment |
| US11043644B2 (en) | 2017-08-23 | 2021-06-22 | Boe Technology Group Co., Ltd. | Transistor acoustic sensor element and method for manufacturing the same, acoustic sensor and portable device |
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