CN102320752B - Patterning method for material - Google Patents
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- CN102320752B CN102320752B CN 201110154332 CN201110154332A CN102320752B CN 102320752 B CN102320752 B CN 102320752B CN 201110154332 CN201110154332 CN 201110154332 CN 201110154332 A CN201110154332 A CN 201110154332A CN 102320752 B CN102320752 B CN 102320752B
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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 inkjet printing methods that utilizes and material is carried out the method for patterning.
Background technology
The chemical reduction Graphene is considered to a kind of electro-conductive material of excellence because have good mechanical property and high specific conductivity, can substitute now widely used tin indium oxide (ITO), is applied to big area, and is transparent, flexible occasion.In addition, because the energy level of grapheme material is arranged with a lot of organic semiconductor material and can mutually be mated, thereby be expected to be applied in many organic electronics devices as outstanding electrode injection material.In fact, since Graphene was found, people had showed its good technical prospect (J.Wu, H.A.Becerril in a lot of organic electronics devices, 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 by 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 larger, directly prints and be difficult to realization.If adopt stripping technology to be prepared 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 be prepared with inkjet technology, can greatly be conducive to 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) in described step 1) gained macromolecule membrane surface utilizes the good solvent of the described macromolecule membrane of method coating of spray ink Printing, obtains the macromolecule membrane after patterning;
3) in described step 2) on macromolecule membrane after the gained patterning and after the described substrate surface that exposes prepares the film and one deck polystyrene film of one deck target material successively, peel described polystyrene film off after Yu Shuizhong soaks and except pattern film and the described macromolecule membrane of all target materials, complete the patterning of described material.
Described step 1) in, described substrate is quartz plate, silicon chip or surperficial silicon chip with silicon dioxide layer, and wherein, in described silicon chip with silicon dioxide layer, the thickness of described silicon dioxide layer is the 100-500 nanometer, preferred 300 nanometers; The material that consists of described macromolecule membrane is polyacrylonitrile, polystyrene 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 described macromolecule membrane is the 1-100 nanometer, preferred 2 nanometers; The described method for preparing macromolecule membrane is spin-coating method; In described spin-coating method, rotating speed is 2000-5000 rev/min, preferred 3500 rev/mins;
Described 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 described macromolecule membrane is selected from least a in DMF, toluene and chlorobenzene, preferred DMF; In this step, because spray ink Printing step solvent for use is step 1) good solvent of gained macromolecule membrane, when carrying out spray ink Printing, this solvent can dissolve macromolecule membrane according to predetermined pattern, expose the surface of substrate (as silicon-dioxide), thereby form the macromolecule membrane of patterning.In actually operating, can determine according to required pattern the number of required drop, as making electrode pair, the number of gained drop is 2.
Described step 3) in, the thickness of described target material film is the 1-10 nanometer, preferred 5 nanometers; The thickness of described polystyrene film is 700 nanometers to 10 micron, preferred 1 micron; The weight-average molecular weight of described polystyrene is 10000-1000000, preferred 200000; Described target material be can with step 1) the described substrate material of being combined, preferential oxidation Graphene or chromium; Institute is set forth in water in soaking step, and the time is 30 minutes to 3 hours, preferred 90 minutes; Prepare the film of described target material and the method for polystyrene film and be spin-coating method or hot vapour deposition method; In described spin-coating method, rotating speed is 3000-8000 rev/min, preferred 4000 rev/mins; In described hot evaporation coating method, vacuum tightness is less than 4 * 10
-4Pascal, evaporation rate was 1 dust/second.In this strip step, owing to having firmly binding ability between target material and substrate, thereby, when peeling off, step 2) the target material film that covers in the substrate that patterning exposes is not stripped from, all the other regional films are all peeled off, thereby have completed the patterning of target material.
The patterning method of described material also comprises the steps: in described step 1) before, described substrate is cleaned up with washing composition, water, deionized water, ethanol and acetone respectively.
The electrode for preparing according to the method described above, the electrode that especially is made of Graphene or chromium, and the application of the 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.
Due to graphene oxide as application of electrode the time, need to recover its Transition of Electrical Conductivity by the method for reduction is Graphene, therefore the above-mentioned electrode that is consisted of by Graphene, be will be according to the method described above graphene oxide after patterning, with the graphene oxide reduction and get, the method is ordinary method through annealing or the method that adds reductive agent, and the method for various redox graphenes commonly used all is suitable for, in method for annealing, vacuum tightness can be 8 * 10 as described
-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 being prepared with field effect transistors also belongs to protection scope of the present invention.
The present invention discloses first a kind of inkjet technology and stripping means of utilizing and directly prepared the method for graphene oxide in the silicon-dioxide substrate; The prepared Graphene electrodes thickness 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 can be directly used in the preparation of field-effect transistor in the silicon-dioxide substrate; The method not only is confined to the patterning of grapheme material, the material that other and silicon-dioxide substrate have the mortise ability, and as chromium, also available this method is carried out patterning.
Description of drawings
Fig. 1 is step 2), 3), 5), 6) finish after the optical microscope photograph of substrate;
Fig. 2 is the atomic force microscopy of the Graphene electrodes of embodiment 1 preparation;
Fig. 3 is the flying-spot microscope photo of the Graphene electrodes for preparing of the present invention;
Fig. 4 is that the Graphene electrodes in embodiment 1 is applied to the device curve in organic field effect tube;
Fig. 5 is the electron scanning micrograph of the chromium metal electrode in embodiment 2.
Embodiment
The present invention is further elaborated below in conjunction with specific embodiment, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described material all can get from open commercial sources if no special instructions.
Embodiment 1, in the silicon-dioxide substrate preparation Graphene electrodes and show its application in organic field effect tube.
1) clean the silicon-dioxide substrate:
Use successively each ultrasonic cleaning of washing composition, water, deionized water, acetone and ethanol after 5 minutes with the silicon chip of thickness 300 nano silicons on the surface, oven dry;
2) with step 1) silicon chip that is disposed is positioned in 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, form uniform polyacrylonitrile macromolecule membrane on silicon chip, thickness is 2 nanometers;
3) spray ink Printing patterning polyacrylonitrile mask layer:
With step 2) in make, the surface is placed on ink-jet printer (jetlab II inkjet printing equipment) operator's console with the silicon chip of mask layer, 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 is 30 microns, 87 microns of adjacent drops spacings, and pattern is comprised of two adjacent drops.
Fig. 1 a is the dry rear pattern in polyacrylonitrile surface formation of drop; As seen from the figure, at the ring of solvent droplets edge formation, its width is far smaller than the diameter of drop itself, and this makes printer have greatly improved to the resolving power of electrode channel region.
4) in step 3) the figuratum silicon chip surface of tool that obtains, spin coating (rotating speed is 4000 rev/mins) graphite oxide aqueous solution three times, preparation a layer thickness is the graphene oxide film of 5 nanometers.
Fig. 1 b has prepared graphene oxide film optical microscope photograph afterwards; As seen from the figure, because graphene oxide and silicon dioxide substrates have stronger bonding force, graphene oxide more easily is deposited on the position that exposes the silicon-dioxide substrate.
5) in step 4) polystyrene film of 1 micron of spin coating (rotating speed is 4000 rev/mins) a layer thickness on gained graphene oxide film, then substrate was put into water 90 minutes, with tweezers peel polystyrene film off and except circle pattern film and the macromolecule membrane of all target materials, complete the patterning of graphene oxide.
Fig. 1 c peels the graphene oxide pattern that the polystyrene macromolecule membrane obtains later on off; As seen from the figure, the pattern of graphene oxide and the pattern of polyacrylonitrile have good complementary relationship, and having proved has good transfer efficiency between pattern.
6) for the graphene oxide that makes the gained patterning recovers electroconductibility, in order to use as electrode, will be placed in vacuum with the substrate of graphene oxide pattern, when vacuum tightness lower than 4 * 10
-4Pascal is heated to 450 ℃, keeps namely obtaining in 2 hours the Graphene of patterning.
Fig. 1 d is for through step 6) optical microscope photograph of reduced graphene electrode after the thermal annealing reduction.
Fig. 2 is for through step 6) atomic force microscopy of afterwards reduced graphene electrode.
Fig. 3 is for through step 6) electron scanning micrograph of afterwards reduced graphene electrode.
As seen from the figure, the channel length of this Graphene electrodes is the 1-2 micron.
Utilize this embodiment to prepare the gained Graphene and be prepared with field effect transistors:
The method that this embodiment is prepared the hot evaporation of gained Graphene electrodes surface employing prepares one deck pentacene semiconductor film, and in evaporate process, low vacuum is in 4 * 10
-4Pascal, evaporation rate 1 dust per second obtains the organic field effect tube based on pentacene.
Test with Keithley 4200 semi-conductor test instruments in air.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.
As seen from the figure, in the situation that the electrode raceway groove is very short, still have good transfer and curve of output.
Embodiment 2, utilize spray ink Printing and stripping technology to carry out patterning to chromium in the silicon-dioxide substrate
1) clean the silicon-dioxide substrate:
Use successively each ultrasonic cleaning of washing composition, water, deionized water, acetone and ethanol after 5 minutes with the silicon chip of thickness 300 nano silicons on the surface, oven dry;
2) with step 1) silicon chip that is disposed is positioned in 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, form uniform polyacrylonitrile macromolecule membrane, thickness 1 nanometer on silicon chip;
3) spray ink Printing patterning polyacrylonitrile mask layer:
With step 2) gained surface is placed 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, the dinethylformamide solvent, the printer head of selecting is 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 evaporation a layer thickness on the polyacrylonitrile mask layer is the chromium layer of 5 nanometers.
5) in step 4) the polystyrene macromolecule membrane of 1 micron of spin coating one deck (rotating speed is 4000 rev/mins) thickness on gained chromium layer, then substrate was put into water 90 minutes, with tweezers peel polystyrene film off and except circle pattern film and the macromolecule membrane of all target materials, complete the patterning of chromium material.
Fig. 5 be the surface with the silicon chip of silicon-dioxide on the electron scanning micrograph of patterning chromium electrode.As seen the chromium electrode channel length that obtains is 2 microns, has good homogeneity.
Claims (12)
1. the patterning method of a material, comprise the steps:
1) preparation one deck macromolecule membrane in substrate;
2) in described step 1) gained macromolecule membrane surface utilizes the good solvent of the described macromolecule membrane of method coating of spray ink Printing, obtains the macromolecule membrane after patterning;
3) in described step 2) on macromolecule membrane after the gained patterning and after the described substrate surface that exposes prepares the film and one deck polystyrene film of one deck target material successively, peel described polystyrene film off after Yu Shuizhong soaks and except pattern film and the described macromolecule membrane of all target materials, complete the patterning of described material.
2. method according to claim 1 is characterized in that: described step 1), described substrate is that quartz plate, silicon chip or surface are with the silicon chip of silicon dioxide layer; The material that consists of described macromolecule membrane is polyacrylonitrile, polystyrene or polymethylmethacrylate; The thickness of described macromolecule membrane is the 1-100 nanometer;
Described step 2) in the method for spray ink Printing, the shower nozzle of ink-jet printer is 20 microns to 100 microns; The adjacent drops spacing is the 120-70 micron; Service temperature is 30-100 ℃; The good solvent of described macromolecule membrane is selected from least a in DMF, toluene and chlorobenzene;
Described step 3) in, the thickness of described target material film is the 1-10 nanometer; The thickness of described polystyrene film is 700 nanometers to 10 micron; The weight-average molecular weight of described polystyrene is 10000-1000000; Described target material be can with step 1) the described substrate material of being combined; Institute is set forth in water in soaking step, and the time is 30 minutes to 3 hours.
3. method according to claim 1 and 2 is characterized in that: the method for preparing macromolecule membrane described step 1) is spin-coating method;
Described step 3) in, the film of the described target material of preparation and the method for polystyrene film are spin-coating method or hot vapour deposition method.
4. method according to claim 3 is characterized in that: described step 1) in described spin-coating method, rotating speed is 2000-5000 rev/min;
Described step 3) in described spin-coating method, rotating speed is 3000-8000 rev/min; In described hot evaporation coating method, vacuum tightness is less than 4 * 10
-4Pascal, evaporation rate was 1 dust/second.
5. method according to claim 4, it is characterized in that: the patterning method of described material also comprises the steps: in described step 1) before, described substrate is cleaned up with washing composition, water, deionized water, ethanol and acetone respectively.
6. method according to claim 5, it is characterized in that: described step 1), in described silicon chip with silicon dioxide layer, the thickness of described silicon dioxide layer is the 100-500 nanometer; The material that consists of described macromolecule membrane is the polyacrylonitrile of 10000-1000000; The thickness of described macromolecule membrane is 2 nanometers;
Described step 2) in the method for spray ink Printing, the shower nozzle of ink-jet printer is 30 microns; The adjacent drops spacing is 87 microns; Service temperature is 80 ℃; The good solvent of described macromolecule membrane is DMF;
Described step 3) in, the thickness of described target material film is 5 nanometers; The thickness of described polystyrene film is 1 micron; The weight-average molecular weight of described polystyrene is 200000; Described target material is graphene oxide or chromium; Institute is set forth in water in soaking step, and the time is 90 minutes;
Described step 1) in described spin-coating method, rotating speed is 3500 rev/mins;
Described step 3) in described spin-coating method, rotating speed is 4000 rev/mins; In described hot evaporation coating method, vacuum tightness is less than 4 * 10
-4Pascal, evaporation rate was 1 dust/second.
7. method according to claim 6, it is characterized in that: described step 1), in described silicon chip with silicon dioxide layer, the thickness of described silicon dioxide layer is 300 nanometers; The material that consists of described macromolecule membrane is 200000 polyacrylonitrile.
8. the application of the arbitrary described method of claim 1-7 in the preparation electrode.
9. the arbitrary described method of claim 1-7 prepares the electrode of gained.
10. electrode according to claim 9 is characterized in that: the material that consists of described electrode is Graphene or chromium; The thickness of described electrode is the 1-10 nanometer, and channel length is the 1-100 micron.
11. the application of the described electrode of claim 9 in being prepared with field effect transistors.
12. the application of the described electrode of claim 10 in being prepared with field effect transistors.
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| TW201504363A (en) * | 2013-07-16 | 2015-02-01 | Enerage Inc | Graphene printing ink and preparation method of graphene circuit |
| CN103606634B (en) * | 2013-11-14 | 2016-02-10 | 中国科学院化学研究所 | A kind of pattern metal electrodes and preparation method thereof |
| 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 |
| 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 |
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